~31~t~6~
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1 TITLE OF THE INVENTION
Light-receiving ~ember for Electrophotography
BACKGROUND OF THE INVENTION
Field of the Invention
This invention relates to a light-receiving
member for electrophotography having sensitivity to
electromagnetic waves such as light [herein used in a
broad sense, including ultraviolet rays, visible light,
infrared rays, X-rays, and ~-rays].
Related Background Art
In the field of image formation, photo-
conductive materials which form light-receiving layers
in light-receiving members for electrophotography are
required to have a high sensitivity, a high SN ratio
[Photocurrent (Ip)/Dark current (Id)], absorption
spectral charaeteristics matching to those of electro-
magnetic waves to be irradiated, a rapid response to
light, a desired dark resistance value as well as no
~o harm to human bodies during usage. Particularly, in
the case of a light-receiving member for electrophoto-
graphy to be assembled in an electrophotographic device
to be used in an office as office apparatus, the afore-
said harmless eharaeteristie is very important.
From the standpoint as mentioned above,
amorphous silicon ~hereinafter represented as A-Si]
has recently attracted attention as a photoconductive
~L304~
material. For example, German OLS Nos. 2746967 and
2855718 disclose applications of A-Si for use in light-
receiving members for electrophotography.
Under the present situation, although the
light-receiving members for electropho~ography having
light-receiving layers constituted of A-Si of the prior
art have been attempted to be improved respectively and
individually with respect to electrical, optical,
photoconductive characteristics such as dark resistance
0 value, photosensitivity, response to light and en-
vironmental characteristics in use and further with
respect to stability with lapse of time and durability,
there still remains room to be further improved in
overall characteristics.
For instance, when improvements to higher
photosensitivity and higher dark resistance were
scheduled to be effected at the same time in light-
receiving members, residual potential was frequently
observed to remain during use thereof. When such a
light-receiving member was repeatedly used for a long
time, various inconveniences were caused such as
accumulation of fatiques by repeated uses or the so-
called ghost phenomenon wherein residual images were
~ormed.
Also, when constituting the light-receiving
layer of A-Si material, the photoconductive member may
contain as constituent atoms hydrogen atoms or halogen
1 atoms such as fluorine atoms, chlorine atoms, etc.,
for improving their electrical, photoconductive
characteristics, boron atoms, phosphorus atoms, etc.,
for controlling the electroconduction type as wel as
other atoms for improving other characteristics~
Depending on the manner in which these constituent
atoms are contained, there may sometimes be caused
problems with respect to electrical, photoconductive
charactexistics or dielectric strength and further
stability of the characteristics with lapse of time of
the layer formed.
That is, the following inconveniences have
frequently occurred. For example, the life of the
photocarriers generated by light irradiation in the
1~ photoconductive layer constituting the light-receiving
layer is not so long, or the image defect which is
generally called "blank area" and may be considered
to be due to the local discharging breaking phenomenon
or the image defect which is generally called "white
line" and may be considered to be formed by friction
with a cleaning blade are occurred in the image
transferred onto a transfer paper. Also, when the
li~ht-xeceiving layer has, for example, a surface
layer with a certain film thickness as constituent
layer on the surface thereof and the surface layer is
substantially transparent to the light used, changes
will occur on the reflected spectrum of the surface
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1 layer by abrasion with friction for a long time,
whereby undesirable changes occurred with lapse of time
in many cases particularly with respect to sensitivity,
etc. Further, when used in a highly humid atmosphere
or used immediately after being left to stand in a
highly humid atmosphere for a long time, the so-called
faint image was frequently formed.
Thus, it is required in designing of a light-
receiving member to make elaborations about layer
constitutions, chemical compositions of the respective
layers, preparation methods, etc., so as to solve all
of the problems as mentioned above along with the im-
provement of A Si materials per se.
1~ SUMMARY OF THE INVENTION
An object of the present invention is to solve
the various problems in the light-receiving member for
electrophotography having a light-receiving layer of
the prior art constituted of A-Si as described above.
Another object of the present invention is to
provide a light-receiving member for electrophoto-
~raphy having a light-receiving layer having a
photoconductive layer constituted of A-Si as o~e of
constituent layers having electrlcal, optical and
photoconductive characteristics which are sub-
stantially constantly stable almost without dependence
on the use environment, having excellent light fatigue
1 resistance as well as excellent durability and humidity
resistance without causing any deterioration phenomenon
after repeated uses and being free entirely or sub-
stantially from residual potential observed.
Still another object of the present invention
is to provide a light-receiving member for electro-
photography having a light-receiving layer having a
photoconductive layer constituted of A-Si as one of
constituent layers having excellent adhesion between
l~ the substrate and the layer provided on the substrate
or between the respective layers laminated, which is
dense and stable in structural arrangement and also
high in layer quality.
Yet another object of the present invention is
to provide a light-receiving member for electrophoto-
graphy exhibiting excellent electrophotographic
characteristics, which is sufficiently capable of
retaining charges at the time of charging treatment for
formation of an electrostatic image to the extent such
that conventional electrophotographic methods can be
very effectively applied when it is provided for use
as a light-receiving member for electrophotography.
Again, another object of the present invention
is to provide a light-receiving member for electro-
?5 photography capable of providing easily a high qualityimage which is high in density, clear in half tone and
high in resolution, without any image defect or faint
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1 image during prolonged use.
Yet still another object of the present in-
vention is to provide a light-receiving member for
electrophotography having high photosensitivity, high
SN ratio characteristic and high dielectric strength,
and which can be maintained under constant state
throughout the whole period during prolonged use.
According to the present invention, there is
provided a light-receiving member for electrophoto-
~raphy comprising a substrate and a light-receiving
layer on the substrate comprising photoconductive layer
exhibiting photoconductivity comprising an amorphous
material containing at least one of hydrogen atoms and
halogen atoms as the constituent in a matrix of silicon
atoms (hereinafter abbreviated as "A-Si(H,X)") and a
surface layer comprising an amorphous material con-
taining silicon atoms, carbon atoms and hydrogen atoms
as the constituents, said surface layer being changed
in the distribution concentration in the layer thick-
~0 ness direction of the carbon atoms such that matchingin optical band gap is obtained at the interface with
said photoconductive layer, and the maximum distri-
bution concentration of the hydrogen atoms within said
surface layer being 41 to 70 atomic percent.
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BRIEF DESCRIPTION OF THE DRAWINGS
Figs. lA to lH and 28 to 32 are schematic
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1 illustrations of the layer constitutions of the prefer-
red embodiments of the light-receiving member for
electrophotography of the present inventioni
Figs. 2A to 2C and 3 to 5 are schematic illus-
trations of unevenness shapes of the substrate surfaceand the method for preparing the uneveness shapes;
Figs. 6 to 9 are illustrations showing examples
of the distribution states in the layer thickness
direction of carbon atoms and hydrogen atoms in the
surface layer;
Figs. 10 to 14 are illustrations showing
axamples of the distribution states in the layer
thickness direction of the group II atoms and the group
V atoms of the periodic table in the charge injection
preventive layer;
Figs. 15 to 21 are illustrations showing
examples of the distribution states in the layer
thickness direction of oxygen atoms and/or nitrogen
atoms and/or carbon atoms in the charge injection
preventive layer;
Figs. 22-27 are illustrations showing examples
o~ the distribution states in the layer thickness
direction of germanium atoms in the longer wavelength
absorbing layer;
Fi~. 33 is a schematic illustration of the
preparation device according to the glow discharge
method which is an example of the device for forming
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1 the light-receiving layer of the light-receiving member
for eleetrophotography of the present invention;
Fig. 34 and 37-42 are illustrations sh~wing
the aistribution states of the respective atoms.
Fig. 35 and 36 are each illustration showing
the erossseetional shape of the substra~e used in
Examples of the present invention.
DESCRIPTION OF THE PREFERRED EMBODIME~TS
~ _ _ . . . ..
In the following, the light-receiving member of
the present invention is deseribed in detail referring
to the drawings.
Fig. lA illustrates schematically the layer
eonstitution of a first preferred embodiment of the
light-reeeiving member for electrophotography of the
present invention.
The light-receiving member l00 for electro-
photography shown in Fig. lA has a light-receiving
layer 102 provided on a substrate l0l for light-
receiving member, the light-reeeiving layer 102 having
a layer eonstitution eomprising a photoconductive layer
103 consisting of A-Si(H,X) and having photoeonductivi-
ty and a surface layer 104 constituted of an amorphous
material eontaining silicon atoms, carbon atoms, and
hydrogen atoms as the constitutent elements, with the
distribu~ion eoneentrations of the eonstituent elements
being determined sueh that matching in optical band gap
1 can be obtained at the interface with the photocon-
ductive layer, and the maximum distribution concen-
tration of hydrogen atoms within the surface layer
being 41 to 70 atomic %.
The light-receiving member for electrophoto-
graphy of the present invention designed so as to have
the layer constitution as specified above can solve
all of the various problems as mentioned above and
exhibits extremely excellent electrical, optical,
photoconductive characteristics, dielectric strength
and use environmental characteristic.
Particularly, there is no influence of the
residual potential on image formation at all, with its
electrical characteristic beiny stable and having high
sensitivity and high SN ratio, as well as excellent
light fatigue resistance, repeated use characteristic,
humidity resistance, dielactric strength, whereby the
density is high, the half tone appears clearly, and an
image of high resolving power and high quality can be
obtained stably throughout the whole period during use
of over a long term.
Substrate
.
The substrate to be used in the present in-
vention may be either electroconductive or insulating.
As the electroconductive substrate, there may be
mentionèd metals such as NiCr, stainless steel, Al, Cr,
Mo, Au, Nb, Ta, V, Ti, Pt, Pd, etc. or alloys thereof.
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As insulating substrates, there may con-
ventionally be used films or sheets of synthetic resins,
including polyester, polyethylene, polycarbonate,
cellulose acetate, polypropylene, polyvinyl chloride,
polyvinylidene chloride, polystyrene, polyamide, etc.,
glasses, ceramics, papers and so on. These insulating
substrates should preferably have at least one surface
subjected to electroconductive treatment, and it is
desirahle to provide other layers on the side at which
said electroconductive treatment has been applied.
For example, electroconductive treatment of a
glass can be effected by providing a thin film of NiCr,
Al, Cr, Mo, Au, Ir, Nb, Ta, V, Ti, Pt, Pd, In203, SnO2,
ITO (In203 ~ SnO2) thereon. Alternatively, a synthetic
resin film such as polyester film can be subjected to
the electroconductive treatment on its surface by
vacuum vapor deposition, electron-beam deposition or
sputtering of a metal such as NiCr, Al, Ag, Pb, Zn,
Ni, Au, Cr, Mo, Ir, Nb, Ta, V, Ti, Pt, etc. or by
laminating treatment with the metal, thereby imparting
electroconductivity to the surface The substrate may
be shaped in any form such as cylinders, belts, plates
or others, and its form may be determined as desired.
For example, it may desirably be formed into an endless
belt or a cylinder for use in continuous high speed
copying. The substrate may have a thickness, which is
conveniently determined so that a light-receiving
~0~
1 member as desired may be formed. When the light-
receiving member is required to have a flexibility, the
substrate is made as thin as possible, so far as the
function of a support can be exhibited. ~owever, in
such a case, the thickness is generally 10 ~ or more
from the points of fabrication and handling of the
substrate as well as its mechanical strength~
Particularly, in the case of performing image
recording by use of coherent light such as laser beam,
unevenness may be provided on the substrate surface in
order to cancel the image badness by the so-called
interference fringe pattern which appears in the
visible image.
The unevenness to be provided on the substrate
surface can be formed by fixing a bit having a V-shaped
cutting blade at a predetermined position on a cutting
working machine such as milling machine, lathe, etc.,
and cut working accurately the substrate surface by,
for example, moving regularly in a certain direction
while rotating a cylindrical substrate according to a
program previously designed as desired, thereby forming
to a desired uneveness shape, pitch and depth. The
inverse V-shaped linear projection produced by the
unevenness formed by such a cutting working has a
spiral structure with a center axis of the cylindrical
substrate as its center. The spiral structure of the
inverse V-shaped projection may be made into a multiple
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1 spiral structure such as double or triple structure or
a crossed spiral structure.
Alternatively, a parallel line structure along
the center axis may also be introduced in addition to
the spiral structure.
The longitudinal s~ctional shape of the con-
vexity of the unevenness provided on the substrate
surface is made an inverse V-shape for a managed non-
uniformization of the layer thickness within minute
columns of each layer formed and ensuring the good
adhesion and desired electrical contact between the
substrate and the layer directly provided on the
substrate, but it should desirably be made substantial-
ly isosceles triangle, right triangle or scalene
triangle, as shown in Fig. 2. Among these shapes,
isosceles triangle and right triangle are preferred.
In the present invention, the respective
dimensions of unevenness provided on the substxate
surface under managed state should be set so as to
accomplish consequently the objects of the present
invention in view of the points as described below.
That is, in the first place, the A-Si(H,X)
layer constituting the light receiving layer is
sensitive to the state of the surface of the layer
formed, and the layer quality will vary greatly
depending on the surface state.
Therefore, it is necessary to set the
~36tl g~
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dimensions of unevenness provided on the substrate
surface so that lowering in layer quality of the
A-Si(H,X) layer may not be brought about~
Secondly, if there is an extreme unevenness on
the ~ree surface of the light-receiving layer, it
becomes impossible to perform completely cleaning in
the cleaning operation after image formation. Also,
when blade cleaning is practiced, there is the problem
that the blade will be damaged sooner.
1~ As the result of investigations of the problems
in layer deposition as described above, problems in
process of electrophotography and the conditions for
prevention of intererence fringe pattern, it has been
found that the pitch at the concavity on the substrate
1~ surface should preferably be 500 ~m to 0.3 ~m, more
preferably 200 ~m to 1 ~m, optimally 50 ~m to 5 ~m~
It is also desirable that the maximum depth of
the concavity should preferably be made 0.1 ~m to 5 ~m,
more preferably 0.3 ~m to 3 ~m, optimally 0.6 ~m to 2
~m. When the pitch and the maximum depth of the con-
cavity of the substrate surface are within the ranges
as specified above, the gradient of the slanted plane
of the concavity (or the linearly projected portion)
may preferably be 1 to 20, more preferably 3 to
15, most preferably 4 to 10.
On the other hand, the maximum difference in
layer thickness based on the nonuniformness in layer
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1 thickness of the respective layers deposited on such
a substrate should preferably be made ~ m to 2 ~m
within the same pitch, more preferably o.l ~m to 1.5
~m, optimally 0.2 ~m to 1 ~m.
Also, as an alternative method for cancelling
image badness by interference fringe pattern in the
case of using coherent light such as laser beam, un-
evenness shape with a plural number of spherical mark
recesses may be also provided on the substrate surface.
That is, the surface of the substrate has more
minute unevenness than resolving power required for
the light-receiving member for electrophotography, and
yet the unevenness is formed of a plural number of
spherical mark recesses.
Referring now to Fig. 4 and Fig. 5, the shape
of the surface of the substrate in the light-receiving
member for electrophotography and a preferable pre-
paration example thereof are explained below, but the
shape of the substrate in the light-receiving member
of the present invention and its preparation method are
not limited by these.
Fig. 4 illustrates schematically a partially
enlarged view of a part of the unevenness shape
according to a typical example of the shape of the
surface of the substrate in the light-receiving member
for electrophotography of the present inventionO
In Fig. 4, 1601 represents a substrate, 1602
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1 the surface of substrate, 1603 a rigid body true sphere
and 1604 a spherical mark recess.
Further~ Fig. 4 also shows an example of prefer-
able preparation method for obtaining the surface shape
of the substrate. More specifically, by permitting a
rigid body true sphere 1603 to fall naturally from a
position at a predetermined height from the substrate
surface 1602 and be collided against the substrate
surface 1602, whereby a spherical recess 1604 can be
In formed. And, by use of a plural number of rigid body
true spheres 1603 with substantially the same radius
R', and permitting them to fall simultaneously or
successively from the same height h, a plural number
of spherical mark recesses 1604 having the same radius
of curvature R and the width D can be formed on the
substrate surface 1602.
A typical example of the substrate having un-
evenness shape with a plural number of spherical mark
recesses formed on the surface as described above is
shown in Fig. 5. In Fig. 5, 1701 represents a
substrate, 1702 the convexity of the unevenness, 1703
a rigid body true sphere and 1704 the concavity of
the unevenness.
In this connection, the radius of curvature R
and the width D of the unevenness shape with the
spherical mark recesses on the substrate surface of
the light receiving member for electrophotography of
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the present invention are important factors for ac-
complishing efficiently the effect of preventiny
generation of interference fringe in the light~
receiving member of the present invention. The
present inventors have made various experiments and
consequently found the following facts. That is,
when the radius of curvature R and the width D
satisfy the following formula:
D > 0 035,
0~5 or more Newton ring by shearing interference
exists within each mark recess. Further, when they
satisfy the following formula:
R > 0 055'
one or more Newton ring by shearing interference
exists within each mark recess.
From these facts, in order to disperse the
interference fringe generated as a whole in the light-
receiving member, within the respective mark recessesthereby preventing generation of interference fringe
in the light-receiving member, it is desirable that
the above D/R should be made 0.035 or more, preferably
0.055 or more.
Also, the width D of the unevenness with mark
recess should be at most about 500 ~m, preferably 200
~m or less, more preferably 100 ~m or less.
~3~149~19
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1 Fig. 3 shows an example of the case having a
light-receiving layer 1500 comprising a photocon-
ductive layer 1502 and a surface layer 1503 formed on
the substrate 1501 prepared according to the above
method. The surface layer 1503 has a free surface
1504~
In the present invention, in order to achieve
its objects effectively, the photoconductive layer
103, 1502 constituting a part of the light-receiving
layer 102, 1500 formed on the substrate 101, 1501 is
constituted of A-Si(H,X) exhibiting photoconductivity
to the irradiated light having the semiconductor
characteristics as shown below.
(1) p-type A-Si(H,X) ... containing only
acceptor; or containing both donor and acceptor with
relatively higher concentration of acceptor (Na);
(2) p-type A-Si(H,X) ... in the type of (1),
that containing acceptor with lower acceptor con-
centration (Na) than (1), when containing only
acceptor, or containing acceptor with relatively lower
concentration as compared with (1), when containing
both acceptor and donor;
~ 3) n-type A-Si(H,X) ... containing only
donor; or containing both donor and acceptor with
relatively higher concentration of donor (nd);
(4) n-type A-Si(H,X) ... in the type of (3),
that containing donor at lower donor concentration
6~
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1 (Nd) than (3), when containing only donor, or contain-
ing donor with relatively lower concentration as
compared with (3), when containing both acceptor and
donor;
(5) i-type A-Si(H,X) ... Na ~ Nb s 0 or
Na ~ Nd
In the present invention, typical examples of
halogen atoms (X) to be incorp~orated in the photo-
conductive layer 103, 1502 are F, CQ, Br and I,
l~ especially preferably F and CQ.
In the present in~ention, formation of a
photoconductive layer 103, 1502 constituted of
A-Si(H,X) may be conducted according to the vacuum
deposition method utilizing discharging phenomenon,
such as glow discharge method, microwave discharge
method, sputtering method or ion-plating method For
example, for formation of a photoconductive layer 103,
1502 constituted of A-Si(H,X) according to the glow
discharge method, the basic process comprises
introducing a starting gas for introduct.ion of
hydrogen atoms (H) and/or a starting gas for intro-
duction of halogen atoms (X) together with a starting
~as for supplying silicon atoms (Si) into the
deposition chamber which can be internally brought to
reduced pressure, wherein glow discharge is generated
thereby to form a layer of A-Si(H,X) on the surface of
a substrate placed at a predetermined position in the
~3~16~L~
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chamber. When it is to be formed according to the
sputtering method, a starting gas for introduction of
hydrogen atoms (H) and/or a gas for introduction of
halogen atoms (X) may be introduced into the chamber
for sputtering, when effecting sputtering upon the
target formed of Si in a atmosphere of an inert gas
such as Ar, He or a gas mixture based on these gases.
The starting gas for supplying Si to be used
in the present invention may include gaseous or
gasifiable hydrogenated silicons (silanes) such as
SiH~ Si2H6' Si3H8' Si4H10 and others as effective
materials. In particular, SiH4 and Si2H6 are prefer-
red with respect to easy handling during layer
formation and efficiency of supplying Si.
As the effective starting gas for incorpo-
ration of halogen atoms to be used in the present
invention, there may be mentioned a number of halogen
compounds such as halogen gases, halides, interhalogen
compounds and silane derivatives substituted with
halogens which are gaseous or gasifiable.
Alternatively, it is also effective in the
present invention to use a gaseous or gasifiable
silicon compound containing halogen atoms which is
constituted of both silicon atoms and halogen atoms.
Typical examples of halogen compounds prefer-
ably used in the present invention may include halogen
gases such as of fluorine, chlorine, bromine or iodine
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1 and interhalogen compounds such as srF, ClF, ClF3,
BrF5, BrF3, IF3, IF7, ICl, IBr, etc.
As the silicon compound containing halogen atom,
silicon halides such ~5 SiF4, Si2F6, SiC14, SiBr4, or
the like are preferred.
When the speciic light-receiving member of
this invention is formed according to the glow discharge
method by use of such a silicon compound containing
halogen atoms, it is possible to form a layer con-
stituted of A-Si:H containing halogen atoms (X) as
constituent element on a given substrate without use
of a hydrogenated silicon gas as the starting gas
capable of supplying Si.
In forming the layer containing halogen atoms
1~ according to the glow discharge method, the basic
procedure comprises feeding a starting gas for supply-
ing Si, namely a gas of silicon halide and a gas such
as Ar, H2, ~e, etc. at a predetermined ratio in a
suitable amount into the deposition chamber for
formation of a photoconductive layer, followed by
excitation of glow discharge to form a plasma atmos ' ``
phere of these gases, thereby forming a photoconductive
layer on a substrate. It is also possible to form a
layer by mixing a gas of a silicon compound containing
hydrogen atoms at a suitable ratio with these gases in
order to incorporate hydrogen atoms therein.
Each of the gases for introduction of
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1 respective atoms may be either a single species or a
mixture of plural species at a predetermined ra~io.
For formation of a layer of A-~i(H,X) by the
reactive sputtering method or the ion-plating method,
S ~or example, a target of Si is used and sputtering is
effected thereon in a suitable gas plasma atmosphere in
the case of the sputtering method. Alternatively, in
the case of ion-plating method, a polycrystalline or
single crystalline silicon is placed as vaporization
source in a vapor deposition boat, and the silicon
vaporization source is vaporized by heating by re-
sistance heating method or electron beam method (EB
method) thereby to permit vaporized flying substances
to pass through a suitable gas plasma atmosphere.
During this procedure, in either of the sput-
tering method or the ion-plating method, for intro-
duction of halogen atoms into the layer formed, a gas
of a halogen compound as mentioned above or a silicon
compound containing halogen as mentioned above may be
introduced into the deposition chamber to form a plasma
atmosphere of the gas therein.
When hydrogen atoms are to be introduced, a
starting gas for introduction of hydrogen atoms such as
H2 or a gas such as silanes as mentioned above may be
introduced into the deposition chamber for sputtering,
followed by formation of a plasma atmosphere of the
gas.
~3Q~
n the present invention, as the starting gas
for introduction of halogen atoms, the halogen compounds
or silicon compounds containing halogens as mentioned
above can effectively be used. In addition, it is also
possible to use a gaseous or gasifiable halide con-
taining hydrogen as one of the constituents such as
hydrogen halide, including FP, HCl, HBr, HI and the like
or halo-substituted hydrogenated silicon, including
SiH2F2, SiH2I2 SiH2Cl2, SiHCl3, siH2sr2~ siHsr3 and
the like as an effective starting material for formation
o a photoconductive layer.
These halides containing hydrogen atom, which
can introduce hydrogen atoms very effectively for con-
trolling electrical or photoelectric characteristics
into the layer during formation of the photoconductive
layer simultaneously with introduction of halogen atoms,
can preferably be used as the starting material for
introduction of halogen atoms.
For incorporation of hydrogen atoms structural-
ly into the layer, H2 or a gas of hydrogenated silicon,
including SiH~, Si2H6, Si3H8, Si4Hlo and so on may be
permitted to be co-present with a silicon compound for
supplying Si in a deposition chamber, wherein dis-
charging is excited.
2S For example, in the case of the reactive
sputtering method, an Si target is used and a gas f~r
introduction of halogen atoms and H2 gas are
~3~
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1 introduced together with, if necessary, as inert gas
such as He, Ar, etc. into a deposition chamber, wherein
a plasma atmosphere is formed to effect sputtering of
the Si target, thereby forming a layer of A-Si(H,X) on
the substrate.
Further, there may also be introduced a gas
such as of B2H6 or others in order to eEfect dopiny
with impurities.
The amount of hydrogen atoms (H) or halogen
atoms (~) incorporated in the photoconductive layer in
the light-receiving member for electrophotography
according to the present invention, or total amount of
both of these atoms, may be preferably 1 to 40 atomic
~, more preferably 5 to 30 atomic ~.
The amount of hydrogen atoms (H) and/or halogen
atoms (X) in the photoconductive layer can be control-
led by controlling the substrate temperature, the
amounts of the starting materials for incorporation of
hydrogen atoms (H) and~or halogen atoms (X) to be
introduced into the deposition device system, the
discharging power, etc.
In the present invention, as the diluting gas
to be used during formation of the photoconductive
layer 103, 1502 according to the glow discharge method
or the sputtering method, there may be employed the
so-called rare gases such as He, Ne, Ar, etc~, as
preferable ones.
~3~
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n order to make the semiconductor charac-
teristic of the photoconductive layer 103, 1502 a
desired one of (1) - (5), n-type impurity, p-type
impurity or both impurities can be incorporated into
the layer in a controlled amount during formation of
the layer. As such impurities, p-type impurities may
include atoms belonging to the group III of the
periodic table such as B, Al, Ga, In, ~1, etc., as
preferable ones, while n-type impurities may include
1~ atoms belonging to the group V of the periodic table
such as N, P, As, Sb, Bi, etc. r as preferable ones,
particularly preferably B, Ga, P, Sb, etc.
In the present invention, when the impurity
typified by the atoms belonging to the group m or V
of the periodic table are contained throughout the
whole layer region of the photoconductive layer 103,
1502, the effect of controlling conduction type and/or
conductivity is primarily exhi~ited.
The content of the impurity in this case is
relatively smaller, preferably 1 x 10 3 to 3 x 102
atomic ppm, more preferably 5 x 10 3 to 10 atomic ppm,
optimally 1 x 10 2 to 50 atomic ppm.
Furthermore, at least one of oxygen atoms and
nitrogen atoms may be contained throughout the whole
layer region of the photoconductive layer in amounts
which do not impair the characteristics desired for the
photoconductive layer.
~3~4 Eii~9
- 25 -
I When oxygen atoms are contained in the whole
layer region of the photoconductive layer 103, 1502 in
the present invention, primarily the effects of higher
dark resistance and improvement of adhesion between the
substrate and the photoconductive layer and between the
photoconductive layer and the surface layer, etc. are
brought about. However, it is desirable that the
content of oxygen atoms should be made relatively
smaller in order to avoid deterioration of the photo-
conductive characteristics of the photoconductive layer103, 1502.
In the case of nitrogen atoms, in addition to
the above points, for example, improvement of photo-
sensitivity can be effected in the co-presence of the
group m atoms, especially B (boron). The content of
oxygen atoms, nitrogen atoms or the sum of both may be
preferably 5 x 10 4 to 30 atomic~, more preferably 1 x
10 3 to 20 atomic%, optimally 2 x 10 3 to 15 atomic%.
For doping of the impurity into the photo-
conductive layer 103 or 1502, the starting material for
introduction of the impurity may be introduced together
with the ~ain starting materials for formation of the
photoconductive layer 103 or 1502 under gaseous state
during layer formation. Such starting material for
introduction of the impurity should be desirably
selected which is gaseous under normal temperature and
normal pressure or readily gasifiable at least under
~3l:1146~
the layer forming conditions~
Specific examples of such starting materials for
introduction of the impurities may include PH3, P2H4,
PF3, PF5, PC13, AsH3, AsF3 AsFS, AsC13, SbH3, SbF3,
SbF5, BiH3, BF3, BC13~ BBr3~ B2H6~ 4 10 5 9 5 11
B6~10~ B6H12' B6H14~ AlC13~ GaC13, InC13, TlC13, and the
like.
For incorporating at least one kind of atoms
selected from oxygen atoms and nitrogen atoms, for
example, in the case of formation according to the glow
discharge method, a compound containing at least one
element of oxygen atoms and nitrogen atoms may be
introduced together with the starting gas for formation
of a photoconductive layer 103 or 1502 into a deposition
chamber which can be internally brought to reduced
pressure, wherein glow discharge is excited to form a
photoconductive layer 103 or 1502.
Examples of the oxygen atom containing compound
as the starting material for introduction of oxygen
atoms may include oxygen (2)' carbon monoxide (CO),
carbon dioxide (CO2), nitrogen monoxide, nitrogen
dioxide, etc.
As the nitrogen atom containing compounds for
the starting material for introduction of nitrogen
atoms, there may be employed, for example, nitrogen
(N2), nitrogen monoxide, nitrogen dioxide, ammonia,
etc.
~3~
- 27 -
On the other hand, for example, when the photo-
conductive layer 103 or 1502 is formed according to the
sputtering method, a taryet for sputtering molded by
mixing the components comprising, for example, (Si ~
Si3N4) or (Si + sio2) at a desired mixing ratio may be
used or two sheets of Si wafer and Si3N4 wafer or two
sheets of Si wafer and SiO2 wafer may be used as the
target for sputtering. Alternatively, a gas of a
nitrogen containing compound or a gas of an oxygen
containing compound may be introduced together with the
gas for sputtering such as Ar gas, etc., into a depo-
sition chamber, where sputtering may be effected with
the use of Si as the target to form a photoconductive
layer 103 or 1502.
During formation of the photoconductive layer
103 or 1502, the substrate temperature during layer
formation is an important factor which influences the
structure and the characteristic of the layer to be
formed, and in the present invention, the substrate
temperature during layer formation should desirably be
controlled strictly so that the photoconductive layer
103 or 1502 having the intended characteristic may be
prepared as desired.
The substrate temperature during formation of
the photoconductive layer 103 or 1502 for the purpose
of accomplishing effectively the ob~ects of the present
invention should be selected within the optimum range
~3~6~
- 28 -
1 corresponding to the method for formation of the
photoconductive layer 103 or 1502 to practice formation
of the photoconductive layer 103 or 1502, but it may be
generally 50C to 350C, preferably 100C to 300C.
For formation of the photoconductive layer 103 or 1502,
it is advantageous to employ the glow discharge method
or the sputtering method for the reasons such as
relatively easier severe control of the composition
ratio of the atoms constituting the layer or control of
the layer thickness, and in the case of forming a photo-
Gonductive layer 103 or 1502 according to these layer
forming methods, discharging power or gas pressure
during layer formation is also one of important factors
influencing the characteristic of the photoconductive
layer 103 or 1502 to be prepared similarly as the above
substrate temperature.
The discharging power condition for preparing
effectively the photoconductive layer 103 or 1502
having the characteristics for accomplishing the
objects in the present invention with good productivity
may be generally 10 to 1000 W, preferably 20 to 500 W.
The gas pressure within the deposition chamber may be
generally 0.01 to 1 Torr, preferably about 0~1 to 0O5
Torr.
In the present invention, the numerical value
ranges desirable for the substrate temperature, dis-
charging power during formation of the photoconductive
- ~L3~ 9
- 29 -
I layer 103 or 1502 may be the values within the ranges
as mentioned above, but these layer forming factors are
not determined independently and separately, but it is
desirable that the optimum values for the factors for
forming respective layers should be determined based
on the mutual organic relationship so that a photo-
conductive layer 103 or 1502 with desired charac-
teristics may be formed.
The layer thickness of the photoconductive
1~ layer 103 or 1502 may be determined suitably as desired
so that the photocarriers generated by irradiation of a
light having desired spectral characteristic may be
transported with good efficiency, and it is preferably
1 to 100 ~, more preferably 2 to 50 ~I~
The surface layer 10~ or 1503 formed on the
photoconductive layer 103 or 1502 has a free surface
105 or 1504, which is provided primarily for ac-
complishing the objects of the present invention in
humidity resistance, continuous repeated use charac-
teristic, dielectric strength, use environment
characteristic, durability, etc.
And, in the light-receiving member of the
present invention, it is an extremely important point
that the optical band gaps Eg opt of the both layers
?5 at the interface between the surface layer 104 or 1503
and the photoconductive layer 103 or 1502 should be
matched to each other or matched at least to the
~3a~
- 30 -
extent which can prevent substantially reflection of
the incident light at the interface betwe~n the surface
layer 104 or 1503 and the photoconductive layer 103 or
1502, and it is also an important point that this
presents an extremely specific preferable condition in
relationship with the hydrogen content. Further, in
the present invention, it is necessary to set the
hydrogen content at the region near the surface of the
surface layer 104 or 1503, at least at the outermost
surface at a predetermined concentrationO
For satisfying the various conditions as
mentioned above, the distribution states of the con-
stituent elements within the surface layer 104 or 1503
are required to be determined under strict condition
Control.
Further, in addition to the conditions as
described above, at the end portion on the free surface
side of the surface layer 104 or 1503, it is also
another point of consideration to constitute the
optical band gap Eg opt possessed by the surface layer
104 or 1503 sufficiently great at the end portion on
the free surface side of the surface layer 104 or 1503
in order to ensure sufficiently the dose of incident
light reaching the photoconductive layer 103 or 1502
provided beneath the surface layer 104 or 1503~ And,
simultaneously with constitution so that optical band
gaps Eg opt may be matched at the interface between
~3~ 9
- 31 -
I the surface layer 104 or 1503 and the photoconductive
layer 103 or 1502, when the optical band gap Eg opt is
constituted sufficiently great at the end portion of
the free surface side of the surface layer 104 or 1503,
the optical band gap Eg opt possessed by the surface
layer 104 or 1503 is constituted so as to contain at
least the region wherein it is continuously changed in
the layer thickness direction of the surface layer 104
or 1503.
For controlling the values of optical band gap
Eg opt in the surface layer 104 or 1503 in the layer
thickness direction, it can be typically practiced by
controlling of the amount of the carbon atom (C) which
is the main controlling atom for the optical band gap
1~ Eg opt to be contained in the surface layer 104 or
1503, and also for the hydrogen atoms having the
function of matching other characteristics of the
surface layer 10~ or 1503 to the optimum condition in
the form corresponding to the change in optical band
gap Eg opt, its content is controlled to a specific
~istribution state.
Reerring now to Fig. 6 through Fig. 9, some
typical examples of distribution states of carbon
atoms and hydrogen atoms in the layer thlckness
direction of the surface layer 104 or 1503 are
described, but the present invention is not limited by
these examples.
~31~
- 32 -
1 In Figs. 6 through 9, the axis of abscissa
indieates the distributed coneentration C of the
earbon atoms (C), silicon atoms (Si), and hydrogen
atoms (H), and the axis of ordinate the layer thiekness
t of the surfaee layer. In the Figures, tT shows the
interfaee position between the photoconductive layer
and the surface layer, tF the free surfaee position,
the solid line the change in distributed eoncentration
of the earbon atoms (C), the two-dot ehain line the
ehange in the distributed eoneentration of silieon
atoms tsi), and the one-dot chain line the change in
distributed coneentration of hydrogen atoms (~1),
respectively.
Fig. 6 shows a first typical example of the
distributed state in the layer thickness of the atoms
(C), silicon atoms (Si), and hydrogen atoms (H) to be
eontained in the surfaee layer. In said example, from
the interface position tT to the position tl, the
distributed concentration C of the atoms (C) ts
inereased from 0 to the concentration Cl as a first
order function, while the distributed concentration of
silicon atoms is redueed from the coneentration C2 to
the eoneentration C3 as a first order function and the
distributed concentration of hydrogen atoms in increas-
ed ~ro~ C4 to C5 as a first order function. From theposition tl to the position tF, the distributed
coneentration C of the atoms (C) and silicon atoms and
~3~6~
- 33 -
1 hydrogen atoms maintain the constant values of the
respective concentrations Cl, C3, and C5, respectively.
Here, for convenience in explanation, the inflection
points of the distributed states of the respective
components are all made tl, but there is substantially
no trouble if they may be deviated from one another.
In the example shown in Fig. 7, from the
position tT to the position tF, the carbon atoms (C)
are varied from 0 to the concentration C6, the silicon
atoms (Si) from C7 to Cg, and the hydrogen atoms (H)
from Cg to ClO, respectively, as a first order
function. In the case of this example, since the
components are varied over the entire region of the
surface layer, the troubles caused by discontinuity of
the components can be further improved.
Also, it is possible to use, for example, the
patterns in which the change rates of the components
are varied from time to time as shown in Figs. 8 and
9 and a combination of the typical examples as
described with reference to Figs. 6 to 9, which can
be selected suitably depending on the desired film
characteristics or the conditions in the preparation
apparatus, etc. Further, matching in optical band
gap Eg opt of the interface may be a substantially
sufficient value, and in that sense the carbon
content at tT is not limited to 0, but may also have
a finite value, and also stagnation in change of the
~L3~
- 3~ -
'~
1 components in the distributed region for a certain
interval may be also permissible from this standpoint.
Formation of the surface layer 104 or 1503 may
be practiced according to the glow discharge method,
the microwave discharge method, the sputtering method,
the ion implantation method, the ion plating method,
the electron beam method, etc~ These preparation
methods may be employed by suitable selection depend-
ing on the factors such as preparation conditions, the
degree of load of installation investment, preparation
scale, the desired characteristics for the light-
receivin~ number for electrophotography to be prepared,
but the glow discharge method or the sputtering method
may be preerably employed for such advantages as
xelatively easy control of the preparation conditions
for preparing the light~receiving member for electro-
photography having desired characteris~ics, easy
intxoduction of carbon atoms and hydrogen atoms
together with silicon atoms into the surface layer 104
~a or 1503, etc.
Further, in the present invention, the surface
layer 104 or 1503 may be formed by using the glow
discharge method and the sputtering method in combi-
nation in the same apparatus system.
For ormation o~ the surface layer 104 or 1503
by the glow discharge method, the basic procedure may
be the same in the distributed region or the constant
- 35 -
region of the constituents, and comprises introducing
the starting gases for formation of A-(SiXCl x)y Hl y,
optionally mixed with a diluting gas at a desired
mixing ratio, into a deposition chamber for vacuum
deposition in which a substrate 101 or 1501 is placed,
and exciting glow discharging of the gases introduced
to form a gas plasma, thereby depositing A(SiXCl_x)y:
Hl on the photoconductive layer 103 or 1502 already
formed on the above substrate 101 or lS01. Formation
f the distributed region can be easily done by set-
ting the components to be changed, for example, flow
rates of a carbon atom containing gas, of a silicon
atom containing gas, and of a hydrogen atom containing
gas, etc., respectively, to a desired distribution
pattern from the flow rate on start-up and increasing
the flow rates following a specific sequence.
In the present invention, as the starting
gases for formation of A-(SixCl_x?y Hl_y most of the
gaseous subs~ances or gasified gasifiable substances
containing at least one of Si, C, and H as the con-
stituent atoms can be used.
When employing a starting material gas con-
taining Si as one of Si, C, and H as the constituent
atom, for example, a starting gas containing Si as
the constituent atom, a starting material gas con-
taining C as the constituent atom, and a starting gas
containing H as the constituent atom may be used by
~L3~3~L6~
- 36 -
1 mixing at a desired mixing ratio, or alternatively a
starting material gas containing Si as the constituent
atom, and a starting gas containing C and H as the
constituent atoms may be mixed also at a desired ratio,
or a starting gas containing Si as the constituent
atom may be used as a mixture with a starting material
gas containing the three constituent atoms of Si, C,
and H.
Also, it is possible to use a mixture of a
starting material gas containing Si and H as the
constituent atoms with a starting material gas con-
taining C as the constituent atom. Also, in the
distributed region, the above mixing ratio may be
varied following a predetermined sequence.
The substance effectively used as the starting
materials for formation of the surface layer 1~4 or
1503 in the present invention may include hydrogenated
silicon hydride gases constituted of silicon atoms (Si)
and hydrogen atoms (H) such as silane, as exemplified
~0 Y 4, i2H6, Si3H8, Si4Hlo, etc., hydrocarbons
constituted of C and H such as saturated hydrocarbons
having 1 to 4 carbon atoms, ethylenic hydrocarbons
having 2 to 4 carbon atoms or acetylenic hydrocarbons
having 2 to 3 carbon atoms~
More specifically, typical examples are
saturated hydrocarbons such as methane (CH4~, ethane
(C2H6), propane (C3H8), n-butane (n~C4H10), pentane
~L3~)~6~
- 37 -
1 (C5H12), and the like; ethylenic hydrocarbons such as
ethylene (C2H4), propylene (C3H6), butene-l (C4H8),
butene-2 tC4H8), isobutylene (C4H8), pentene (C5Hlo)
and the like; and acetylenic hydrocarbons such as
5 acetylene (C2H2), methylacetylene (C3H4), butyne (C4H6),
and the like.
Typical examples of the starting gas having
Si, C, and H as constituent atoms are alkyl silanes
( H3)4, Si(C2~5)4, and the like, In addition
to these starting gases, H2 can of course be effective-
ly used as the starting gas for introduction of
hydrogen atoms (H).
For forrnation of the surface layer 104 or 1503
by the sputtering method, a single crystalline or
1~ polycrystalline Si wafer or C wafer or a wafer contain-
ing Si and C mixed therein is used as a target and
subjected to sputtering in an atmosphere of various
gases.
For example, when Si wafer is used as target,
a starting gas for introduction of C and H, which may
be diluted with a diluting gas, if desired, is intro-
duced into a deposition chamber for sputter to form a
gas plasma of these gases therein and effect sputtering
of said Si wafer. The distributed region in this case
n~ay be ~ormed by, for example, varying the concen-
tration of the starting material gas containing C
following a certain sequence.
~3~
- 38 -
1 Alternatively, Si and C as separate targets or
one sheet target of a mixture of Si and C can be used
and sputtering is effected in a gas atmosphere contain-
ing at least hydrogen atoms. The distributed region in
this case isreq~ired to be formed by using a gas
containing either one of C or Si in combination and
varying these gas concentrations following a certain
sequence.
As the starting gas for introduction of C or
H, there may be employed those as mentioned in the
glow discharge method as described above as effective
gases also in the case of sputtering.
In the present invention, as the diluting gas
to be employed in forming the surface layer 10~ or
1503 according to the glow discharge method or the
sputtering method, there may be included so called
rare gases such as He, Ne or Ar as suitable ones.
The surface layer 104 or 1503 in the present
invention is formed carefully so that it may have a
distributed region along the spirit of the present
invention as described above and the characteristics
required from the view point of entire layers may be
given exactly as desired.
That is, a substance constituted of Si, C and
H, can take various forms from crystalline to
amorphous, electrical properties from conductive
through semiconductive to insulating, and
~3~
- 39 -
photoconductive properties from photoconductive to
nonphotoconductive depending on the preparation
conductions. In the present invention, the preparation
conditions are severely selected as desired so that
there may be formed A-SixCl x having desired charac-
teristics depending on the purposes.
For example, for providing the surface layer
104 or 1503 primarily for the purpose of improving
dielectriC strength, A-(sixCl_x)y:Hl_y is arra g
an amorphous material with remarkable electrical
insulating behaviors in the use environment.
On the other hand, when the surface layer 104
or 1503 is provided primarily for the purpose of
improving continuous repeated use characteristics or
use environmental characteristics, the degree of the
above electrical insulating property is alleviated to
some extent and A-(SixCl X)y:Hl_y is arranged as an
amorphous material having some sensitivity to the
light irradiated.
~0 During formation of the surface layer 104 or
1503 comprising A-(SiXCl X)y:Hl y on the surface of
the photoconductive layer 103 or 1502, the substrate
temperature during layer formation is an important
factor which influences the structure and the charac-
teristic of the layer to be formed and, in the present
invention, the substrate temperature during layer
formation should desirably be controlled strictly so
~3~6~
- 40 -
1 that A-(SiXcl x)y Hl having desired characteristics
may be prepared as desired.
~ s the substrate temperature during formation
of the surface layer 104 or 1503 accomplishing ef-
fectively the object in the present invention, asuitable optimal range corresponding to the formation
method of the surface layer 104 or 1503 may be selected
to practice formation of the surface layer 104 or 1503,
but is may be preferably 50C to 350C, more preferably
100C to 300C. For formation of the surface layer
104 or 1503, it is advantageous to employ the glow
discharge method or the sputtering method for such
reasons as relatively easier severe control of the
composition ratio of the atoms constituting the layer
or the control of layer thickness as compared with
other methods. For formation of the surface layer 104
or 1503 according to these layer forming methods, the
discharging power or the gas pressure during layer
formation is one of important factors influencing the
characteristics of A-(SiXCl_x)y:Hl_y p p
The discharging power condition for preparing
effectively A-(SixCl X)y:Hl_y having the charac-
teristics for accomplishing the objects in the present
invention with good productivity may be preferably 10
to 1000 W, more preferably 20 to 500 W~ The gas
pressure in the deposition in chamber may be prefer-
ably 0.01 to 1 Torr, more preferably 0.1 to 0.5 Torr.
~] ~ ~
n the present invention, the desirable
numerical value ranges for the substrate temperature
and discharging power during formation of the surface
layer 104 or 1503 may be those as mentioned above, but
these layer formation factors are not determined
independently and separately, but it is desirable
that the optimum values of the respective layer
formation factors are desirably determined based on the
mutual organic relationship so that the surface layer
104 or 1503 comprising A-(Si~,Cl x)y:Hl_y having
desired characteristics may be formed.
The amounts of carbon atoms and hydrogen atoms
contained in the surface layer 104 or 1503 in the
light-receiving member for electrophoto~raphy of the
present invention are also important factors for
forming the surface layer 104 or 1503 having the
desired characteristics to accomplish the objects of
the present invention similarly as the preparation
conditions of the surface layer 104 or lS03.
The amount of the carbon atoms contained in
the surface layer 104 or 1503 in the present invention
should be desirably varied in the distributed region
preferably from 1 x 10 4 to 90 atomic %, more prefer-
ably 1 x 10 4 to 85 atomic %, optimally from 1 x 10 4
to 80 atomic % based on the total amounts of silicon
atoms and carbon atoms, and also should desirably in
the constant region preferably 1 x 10 to 90 atomic %,
~31[~69L9~
- 42 -
1 more preferably 1 to 90 atomic ~, optimally 10 to 80
atomic ~. The content of hydrogen atoms should be
desirably made constant or varied in the distributed
region within the range from 1 to 70 atomic % based on
the total amount of the constituent atoms, and also
should be desirably made in the constant region or at
least on the outermost surface of the surface layer
preferably 41 to 70 atomic ~, more preferably 45 to 60
atomic %.
The light-receiving member having the surface
layer prepared under the quantitative range as
specified abovè and the above distributed state and
further the above preparation conditions can be applied
sufficiently as the material which is extremely excel-
1~ lent as not found in the prior art in practical aspect.
Referring to several examples, its action is
described.
To describe about the aspect of matching in
band gap, for example, when there exists a clear
optical interface between the surface layer and the
photoconductive layer as in the case of the prior art,
reflection of incident light occurs at said interface,
whereby there is observed the phenomenon that the dose
of the incident light into the photoconductive layer
may be more or less influenced by the interference
between this reflection at said interface and the
reflection at the free surface. Particularly, when
~3~
43 -
1 coherent light such as laser beam is used as the ligh-t
source, this tendency is marked. On the other hand,
in the case of a copying machine using, for example,
the blade cleaning method, the surface layer will be
inevitably more or less abraded by prolonged use, and
the film thickness change of the surface layer by this
abrasion will cause a change in the above interference
state. That is, there is observed the phenomenon that
the dose of incident light into the photoconductive
layer will be more or less influenced by the abrasion.
Controlling of matching in band gap in the present
invention has one aspect of brin~ing about the effect
of minimizing reflection at the above interface from
the aspect of continuity of the components, and also
separately imparts continuity to light absorption
itself by changing the band gap, thus giving rise to
double preferable actions. Accordingly, the action
which should be specially mentioned in this case may be
said to be the outstanding effect concerning particular-
ly maintenance of the characteristics during prolongeduse among the preferable electrophotographic various
characteristics as already described.
Ne~t, the role of hydrogen in the surface layer
is described. The defects existing within the surface
layer ~primarily dangling bonds of silicon atoms or
carbon atoms) have been known to exert bad influences
on the characteristics as the light-receiving member
~L3@~
- 44 -
1 for electrophotography For example, there may be
caused deteriorat~on of charging characteristics by
injection of charges from the free surface, fluctuation
in charging characteristics due to change in the
surface structure under the use environment such as
high humidity, and further residual image phenomenon
during repeated use by injection of charges from the
photoconductive layer to the surface layer during
corona charging or light irradiation and trapping of
the charges by the defects within the surface layer as
mentioned above.
However, by controlling the hydrogen content
within the surface layer in at least the outermost
surface region to 41 atomic % or higher, all of the
lS above problems can be cancelled, and particularly a
dramatic improvement can be effected in the electrical
characteristics and high speed continuous use charac-
teristic as compared with the prior art product.
On the other hand, if the hydrogen content in
the above surface becomes 71 atomic % or higher, the
hardness of the surface layer will be lowered, whereby
the light-receiving member cannot stand repeated uses.
Therefore, it is one of very important factors in
obtaining extremely excellent desired electrophoto-
graphic characteristics to control the hydrogencontent in the surface layer within the range as
specified above~ The hydrogen content in the surface
~3~
- 45 -
1 layer can be controlled by the flow rate of H2 gas, the
substrate temperature, the discharging power, the gas
pressure r etc.
There is also a specific relationship between
the above matehing in the optical band gap Eg opt and
the hydrogen atoms containing state. Particularly, in
the distributed region of carbon atoms (C) which is
the representative change eomponent of the optical
band gap Eg opt, the hydrogen containing state is such
that its content is set so as to optimize the structure
in that region or/and minimize dangling bonds, and also
so as to become the value necessary for effecting the
aetion as described in the role of hydrogen in the
above surface layer. In other words, it is set in the
most natural form to make the content of hydrogen
atoms inereased toward at least the free surface side.
Thus, the hydrogen atoms containing state in
the surface layer in the present invention can be also
said to have another action of taking matching between
the following both aetions so that the action of
matehing in the optieal band gap Eg opt and the action
by the hydrogen atoms content itself may be both
exhibited to full extent.
The numerieal range of the layer thiekness in
the present invention is one of the important faetors
for aeeomplishing effectively the objects of the
present invention~
~3~
- ~6 -
The numerical range of the layer thickness of
the surface layer 104 or 1503 in the present invention
may be determined suitably as desired depending on the
initial purpose so that the objects of the present
invention can be effectively accomplished.
Also, the layer thickness of the surface layer
104 or 1503 is required to be determined suitably in
relationship with the layer thickness of the photo-
conductive layer 103 or 1502, as desired under the
organic relationship corresponding to the charac-
teristics demanded for the respective layer regions.
Further, in addition, it is desirably determined in
view of economical considerations including productivi-
ty or bulk productivity.
The layer thickness of the surface layer 104 or
1503 in the present invention should be desirably be
made generally 0.003 to 30 ~, pre~erably 0.004 to 20 ~,
optimally O.OOS to 10 ~.
The layer thickness of the light-receiving
layer of the light-receiving member 100 for electro-
photography in the present invention may be determined
suitably as desired as fitted for the purpose.
In the present invention, the layer thickness
of the light-receiving layer 102 or 1500 may be
determined suitably as desired in the layer thickness
relationship between the photoconductive layer 103 or
1502 and the surface layer 104 or 1503 so that the
~309L~9
-- ~7 --
characteristics imparted to the photoconductive layer
103 or 1502 and the surface layer 104 or 1503 con-
stituting the light-receiving layer 102 or 1500 can be
effectively utilized respectively to accomplish
5 effectively the objects of the present invention, and
it is preferable that the layer thickness of the
photoconductive layer 103 or 1502 should be made some
hundred to some thousand-fold or more relative to the
layer thickness of the surface layer 104 or 1503.
In the light-receiving member for electro-
photography of the present invention, for further
improvement of adhesion between the substrate 101 or
1501 and the photoconductive layer 103 or 1502, there
may be also provided an adhesion layer constituted of,
1~ for example, amorphous materials containing at least
one of Si3N4, SiO2, SiO~ hydrogen atoms, and halogen
atoms and at least one of nitrogen atoms, oxygen
atoms, and carbon atoms and silicon atoms, etc.
Fig. lB shows an example of the light-receiving
menber for electrophotography having such a layer
constitution.
The light-receiving member for electro-
photo~raphy 200 shown in Fig. lB has the same layer
constitution as the light-receiving layer for
2~ electrophotography 100 shown in Fig. lA except for
having an adhesion layer 206. That is, on the adhesion
layer 206 are provided successively the photoconductive
- 48 -
I layer ~03 and the surface layer 204, and the photo-
conductiv~ layer 203 is constituted of the same ~aterial
and has the same function as the photoconductive layer
103, and also the surface layer 204 as ~he surface
layer 104.
Adhesion layer
The adhesion layer of the light-receiving member
for electrophotography in the present invention is
constituted of an amorphous or polycrystalline material
containing at least one of nitrogen atoms, oxygen atoms
and carbon atoms, silicon atoms and optionally at least
one of hydrogen atoms and halogen atoms. Further, the
above adhesion layer 206 may also contain a substance
for controlling conductivity (valence electron con-
troller) as the constituent atom~
That is, the primary object of said adhesionlayer is to improve adhesion between the substrate and
the photoconductive layer Also, by containing a
substance for controlling conductivity in said layer,
the transport of charges between the substrate and
the photoconductive layer can be effected more
eficiently.
Nitrogen atoms, oxygen atoms, carbon atoms,
hydrogen atoms, halogen atoms and the substance for
controlling conductivity may be contained either
uniformly throughout said layer or under nonuniform
~.istribution state in the layer thickness direction~
~3ÇO~
I The amount of carbon atoms, oxygen atoms or
nitrogen atoms contained in the adhesion layer formed
in the present invention or the combined amount of at
least two of them must be determined suitably as
desired, but it may preferably be 0.0005 to 70 atomic
%, more preferably 0.001 to 50 atomic %, optimally
0.002 to 30 atom-c %.
The layer thickness of the adhesion layer 206
may be determined suitably in view of adhesion property,
transport efficiency of charge, production efficienty,
but it may preferably be 0.01 to 10 ~m, more preferably
0.02 to 5 ~m.
The amount of hydrogen atoms, the amount of
halogen atoms or the sum of the amounts of hydrogen
atoms and halogen atoms contained in the adhesion
layer may preferably be 0.1 to 70 atomic %, more
preferably 0.5 to 50 atomic %, optimally 1.0 to 30
atomic %.
Fig. lC and ~ig. lD illustrate schematically
layer constitutions of the third preferred embodiment
and the fourth preferred embodiment, respectively, of
the light-receiving member for electrophotography of
the present invention.
The light-receiving member for electro-
photography shown in Fig~ lC and Fig. lD has a light-
receiving layer 300, 400 on a substrate 301, 401 for
light-receiving member, said light-receiving layer
~3~
- so -
1 300, 400 having a layer constitution, comprising a
charge injection preventive layer 302, 402, a photo-
conductive layer 303, 403 having photoconductivity and
a surface layer 304, 404. Also, 406 represents an
adhesion layer.
The photoconductive layers 303, 403, the
surface layers 304, 404, the adhesion layer 404 in Figs.
lC and lD are respectively the same as the photo-
conductive layers 103, 203, the surface layers 104, 204
and the adhesion layer 206 shown in Figs. lA and lB,
and therefore description of these layers is omitted.
~ he charge injection preventive layers 302, 402
newly added in the light-receiving member for electro-
photography shown in Figs. lC and lD are described in
detail below,
~0
~31D~
- 51 -
1 Charge Injection Preventive Layer
The charge injection preventive layer 302, 402
in the present invention is constituted of A-Si (H,
X) or polycrystalline silicon and contains a substance
for controlling conductivity (valence electxon con-
troller) uniformly throughout the whole layer region
or preferably nonuniformly as enriched on the substrate
side in said layer 302, 402. Further, if necessary,
oxygen atomsor/and nitrogen atoms or/and carbon atoms
may be contained uniformly throughout the whole layer
region or a partial layer region of said layer 102 or
preferably nonuniformly as enriched on the substrate
side, whereby improvement of adhesion between the
charge injection preventive layer 102 and the substrate
and contrcl of band gap can be effected.
As the substance for controlling conductivity
to be contained in the charge injection preventive
layer 302, 402~ there may be mentioned so called
impurities in the field of semiconductors similarly as
in above description of photoconductive layer. In
the present invention, there may be employed the
atoms belonging to the group III of the periodic
table giving p-type conductivity characteristics
~the group III atoms) or the atoms belonging to the
group V atoms of the periodic table giving n-type
conductivity characteristics (the group V atoms).
Figs. 10 through 14 show typical examples of
- 5~ -
1 distributed states in the layer thickness direction
of the group III atoms or the group V atoms contained
in the charge injection preventive layer 302, 402~
In Figs. 10 through 14, the axis of abscissa indictes
the distributed concentration C of the group III atoms
or the group V atoms, and the axis of ordinate the
layer thickness t of the charge injection preventive
layer 302, 402 tB showing the interface position on
the substrate 301, 401 side, tT the interface position
10 on the side opposite to the substrate 301, 401 side.
That is, the charge injection preventive layer is
formed from the tB side toward the tT side.
Fig. 10 shows a first typical example of the
distributed state in the layer thickness direction
of the group III atoms or the group V atoms contained
in the charge injection preventive layer 302, ~02.
In the example shown in Fig. 10, from the
interface position tB to the position tl, the group
III atoms or the group V atoms are contained with
the concentration C taking a constant value of Cl,
and the distributed concentration C being reduced
fr~m C22 gradually and continuously from the position
tl to the interface position tT~ At the interface
position tT~ the distributed concentration is made
~5 C23'
In the example shown in Fig. 11, the distri-
buted concentration C of the group III atoms or the
~3~6~9
- 53 -
1 group V atoms contained is reduced from C24 gradually
and continuously Erom the position tB to the position
tT~ until it becomes C25 at the position tT~
In the example shown in Fig. 12, the distri-
buted concentration C of the group III atoms or thegroup V atoms is a constant value of C26 between the
position tB and the position t2 and made C27 at the
position tT~ setween the position t2 and the position
tT, the distributed concentration C is reduced as a
first order function from the position t2 to the
position tT~
In the example shown in Fig. 13, the distri-
buted concentration C takes a constant value of C28
from the position tB to the position t3, and is
reduced from C29 to C30 as a first order function
from the position t3 to the position tT
In the example shown in Fig. 14, the distri-
buted concentration C takes a constant value of C
from the position tB to the position tT~
In the present invention, when the charge
injection preventive layer 302, 402 contains the
group III atoms or the group V atoms in the distri-
bution state where they are enriched on the substrate
side, it is preferable that the layer should be
2~ formed to a distribution state such that the maximum
value of the distributed concentration value of the
group III atoms or the group V atoms may be 50 atomic
~3~
- 54 -
1 ppm or more, more preferably 80 atomic ppm or more,
optimally 100 atomic ppm or more.
In the present invention, the content of the
group III atoms or the group V atoms in the charge
S injection preventive layer 302, 402 may be determined
suitably as desired so as to accomplish effectively
the objects of the present invention, but preferably
30 to 5 x 104 atomic ppm, more preferably 50 to 1 x
104 atomic ppm, optimally 1 x 102 to 5 x 103 atomic
ppm.
The charge injection preventive layer 302, 402
has the effect of primarily improving adhesion
between the substrate 301, 401 and the charge in-
jection preventive layer 302, 402, improving adhesion
between the charge injection preventive layer 302,
402 and the photoconductive layer 303, 403 ox con-
trolling the band gap Egopt of the charge injection
preventive layer 302, 402 by containment of oxygen
atoms or/and nitrogen atoms or/and carbon atoms as
mentioned above.
Figs. 15 through 21 show typical examples of
distribution states in the layer thickness direction
of oxygen atoms or/and nitrogen atoms or/and carbon
atoms to be contained in the charge injection pre-
25 ventive layer 302, 402. In the examples shown in
Figs. 15 through 21, the axis of abscissa indicates
the distributed concentration C of oxygen atoms
s~
I or/and nitrogen atoms or/and carbon atoms, and theaxis of ordinate the layer thickness t of the charge
injection preventive layer 302, 402, tB showing
the interface position on the substrate side and the
tT the interface position on the side opposite to the
substrate side. That is, the charge injection
preventive layer is formed from the tB side toward
the tT side.
In Fig. 15, there is shown a first typical
example in which the distribution state in the layer
thicXness direction of oxygen atoms or/and nitrogen
atoms or/and carbon atoms contained in the charge
injection preventive layer 302, 402.
In the example shown in Fig. 15, from the
1~ interface position tB to the position t4, oxygen atoms
or/and nitrogen atoms or/and carbon atoms are contain-
ed while the concentration C taking a constant value
of C3~, and the distributed concentration C is gradual-
ly and continuously reduced from C33 from the position
t4 to the interface pos;tion tT. At the interface
position tT~ the distributed concentration is made
34'
In the example shown in Fig. 16, the distri-
buted concentration C of oxygen atoms or/and nitrogen
atoms or/and carbon atoms contained is reduced gradual-
ly and continuously from C35 from the position tB to
the position tT~ and at the position tT the concent-
~3~46~L~
- 56 -
l ration becomes C36.
In the case of Fig. 17, the distributed
concentration C of oxygen atoms or/and nitrogen atoms
or/and carbon atoms is made a constant value C37 from
the position tB to the position t5, and reduced
gradually and continuously from C38 between the
position t5 and the position tT, until it is made
substantially zero at the position tT.
In the case of Fig. l~, the distributed
concentration C of oxygen atoms or/and nitrogen atoms
or/and carbon atoms is reduced gradually and continu-
ously from C39 from the position tB to the position
tT~ until it is made substantially zero at the
position tT.
l~ In the example shown in Fig. l9~ the distri-
buted concentration C of oxygen atoms or/and nitrogen
atoms or/and carbon atoms takes a constant value of
C40 rom the position tB to the position t6, and
reduced as a first order function from C40 to C
from the position t6 to the position tT.
In the example shown in Fig. 20, the distri-
buted concentration C of oxygen atoms or/and nitrogen
atoms or/and carbon atoms is a constant value of
C4~ between the position tB and the position t7, and
made C44 at the position tT. Between the position t6
and the position tT~ the distributed concentration
C is reduced as a first order concentration from C43
~3~61~
- 57 ~
l at the position t6 to C44 at the position tT-
In the example shown in Fig. 21, the distri-
buted concentration takes a constant value of C45
from the position tB to the position tT.
In the present invention, when the charge
injection preventive layer 302, ~02 contains oxygen
atoms or/and nitrogen atoms or/and carbon atoms in a
distribution state as enriched on the substrate 301,
401 side, it is preferable that the maximum value of
the distribution concentration value of oxygen atoms
or/and nitrogen atoms or/and carbon atoms or the sum
of those of two kinds amongthem should be 500 atomic
ppm or more, preferably 800 ppm or more, optimally
lO00 atomic ppm or more.
lS In the present invention, the content of
oxygen atoms or/and nitrogen atoms or/and carbon
atoms or the sum of those of two kinds among them
contained in the charge injection preventive layer
302, ~02 may be determined suitably as desired so as
the accomplish effectively the objects of the present
invention, but may be preferably 0.001 to 50 atomic
~, more preferably 0.002 to 40 atomic %, optimally
0.003 to 30 atomic %.
In the present invention, the layer thickness
of the charge injection preventive layer may be
preferably 0.01 to lO ~, more preferably 0.05 to 8 ~,
optimally 0.1 to 5 ~, for obtaining desired electro-
~3a:~6~
- 58 -
1 photographic characteristics and also from the
standpoint of economy.
In the present invention, halogen atoms (X)
contained in the charge injeCtiQn preventive layer
302, 402 may preferably be F, Cl, sr, I, particularly
F, Cl.
In the present invention, for formation of
a charge injection preventive layer constituted of
a polycrystalline silicon or A-Si(H,X), for example,
1~ there may be employed the vacuum deposition method
utilizing discharging phenomenon such as the glow
discharge method, the microwave discharge method, the
sputtering method or the ion plating method. For
example, for formation of a layer constituted of a
polycrystalline silicon or A-Si(H,X), the basic
procedure comprises introducing a starting gas for
Si capable of supplying silicon atoms (Si) together
with a starting gas for introduction of hydrogen atoms
(H) or/and a starting gas for introduction of halogen
atoms (X) into a deposition chamber which can be
brought to a reduced pressure to excite glow dis-
charging within said deposition chamber and form a
layex comprising a polycrystalline silicon or a layer
comprising A-Si(H,X) on the surface of a predetermined
substrate which is previously placed at a prede-
termined position. On the other hand, for formation
according to the sputtering method, for example, when
~3~ 1.9
- 59 -
I sputtering a target constituted of Si in an atmosphereof an inert gas such as Ar, He, etc., or a gas mixture
based on these gases, the gas for introduction of
hydrogen atoms (H) or/and halogen atoms (X) may be
introduced into the deposition chamber for sputteringO
The substance which can be the starting
material gas for Si supply to be used in the present
invention may include gaseous or gasifiable hydro~
genated silicon (silanes) such as SiH4, Si2H6, Si3H8,
Si4Hlo and the like as effective ones, particularly
preferably SiH4, Si2H6 for easiness in handling
during layer formation working, good Si supply ef-
ficiency, etc.
As the effective starting gas for incorpo-
ration of halogen atoms to be used in the presentinvention, there may be mentioned a number of halogen
compounds such as halogen gases, halides, interhalogen
compounds and silane derivatives substituted with
halogens which are gaseous or gasifiable.
Further, it is also effective in the present
invention to use a gaseous or gasifiable silicon
compound containing halogen atoms which is constituted
of both silicon atoms and halogen atoms.
Typical examples of halogen compounds prefer~
ably used in the present invention may include halogen
gases such as of fluorine, chlorine, bromine or iodine
and interhalogen compounds such as BrF, ClE', ClF3,
~L3~
- 60 -
1 BrF5, BrF3, IF3~ IF7, ICl, IBr, etc.
As the silicon compound containing halogen
atom, namely the so-called silane derivatives substi-
tuted with halogen atoms, silicon halides such as Si~4,
Si2F6, SiCl4, SiBr4, or the like are preferred.
When the specific photoconductive member of
this invention is formed according to the glow dis-
charge method by use of such a silicon compound con-
taining halogen atoms, it is possible to form a layer
constituted of a polycrystalline silicon or A-Si:H
containing halogen atoms on a desired substrate
without use of a hydrogenated silicon gas as the
starting gas capable of supplying Si.
In the case of preparing a layer containing
halogen atoms according to the glow discharge method,
the basic procedure comprises introducing a silicon
halide as the starting material gas for Si supply
together with a gas such as Ar, H2, He~ etc. at a
predetermined mixing ratio and gas flow rates into a
deposition chamber for formation of a desired layer,
and exciting glow discharge to form a plasma atmos-
phere of these gases, whereby a desired layer can be
formed on a desired substrate. For effecting intro-
duction of hydrogen atoms, a gas of a silicon
~5 compound containing hydrogen atoms may be further
mixed into these gases in a desired amount for layer
formation.
~3~6~
- 61 -
The respective gases used are not limited
only to single species, but a plural number of gas
species may be used at a desired mixing ratio.
For formation of a layer comprising poly-
crystalline silicon or A-Si(H,X) by the reactive
sputtering method or the ion-plating method, for
example, a target of Si is used and sputtering is
effected thereon in a suitable gas plasma atmosphere
in the case of the sputtering method. Alternatively,
in the case of ion-plating method; a polycrystalline
or single crystalline silicon is placed as vapori-
zation source in a vapor deposition boat, and ~he
silicon vaporization source is vaporized by heating
by resistance heating method, electron beam method
(EB method) or the like thereby to permit vaporized
flying substances to pass through a suitable gas
plasma atmosphere.
During this procedure, in either of the
sputtering method or the ion-plating method, for
introduction of halogen atoms into the layer formed,
a gas of a halogen compound as mentioned above or a
silicon compound containing halogen as mentioned
above may be introduced into the deposition chamber
to form a plasma atmosphere of said gas therein.
When hydrogen atoms are to be introduced, a
starting gas for introduction of hydrogen atoms such
as H2 and a gas such as silanes as mentioned above
- 62 -
I may be introduced into the deposition chamber ~or
sputtering, followed by formation of a plasma
atmosphere of said gases~
In the present invention, as the starting
gas for introduction of halogen atoms, the halogen
compounds or silicon compounds containing halogens
as mentioned above can effectively be used. In
addition, it is also possible to use a gaseous or
gasifiable halide containing hydrogen atom as one
of the constituents such as hydrogen halide, includ~
ing HF, HCl, HBr, HI and the like or halo-substituted
hydrogenated silicon, including SiH2F2, SiH2I2,
SiH2C12, SiHC13, SiH2Br2, SiHBr3 and the like as an
effective starting material for formation of a
charge injection preventive layer and a photoconductive
layer.
These halides containing hydrogen atom, which
can introduce hydrogen atoms very effective for con-
trolling electrical or optical characteristics into
the layer during formation of the layer simultaneous-
ly with introduction of halogen atoms, can preferably
be used as the starting material for introduction of
halogen atoms.
For incorporation of hydrogen atoms structur-
ally into the layer formed, in addition to those asmentioned above, H2 or a gas of hydrogenated silicon,
including SiH4, Si2H6, Si3H8, Si4Hlo and so on may be
- 63 -
1 permitted to be co-present with a silicon compound
for supplying Si in a deposition chamber, wherein
~ischarging is excited.
For example, in the case of the reaction
sputtering method, a Si target is used and a gas for
introduction of halogen atoms and H2 gas are intro-
duced together with, if necessary~ an inert gas such
as He, Ar, etc. into a deposition chamber, wherein
a plasma atmosphere is formed to effect sputtering of
1~ said Si target, thereby forming a layer consisting
of a polycrystalline silicon or A-Si(H,X) on the
substrate.
Further, there may also be introduced a gas
such as of B2H6 or the like in order to effect also
doping of impurities.
The amount of hydrogen atoms (H) or halogen
atoms (X) incorporated in the charge injection
preventive layer 302, 402 in the light-receiving
member for electrophotography according to the present
invention, or total amount of both of these atoms,
may be preferably 1 to 40 atomic %, more preferably
5 to 30 atomic %.
For controlling the amounts of hydrogen atoms
(H) and/or halogen atoms (X) in the layer formed,
the substrate temperature and/or the amounts of the
starting materials for incorporation of hydrogen
atoms (H) or halogen atoms (X) to be introduced into
~3~
~ 6~ -
1 the deposition device system or the discharging power
may be controlled.
For incorporating the group III atoms or the
group V atoms, and the carbon atoms, oxygen atoms or
nitrogen atoms in the charge injection preventive
layer 302, 402, during formation of the charge
injection preventive layer by glow discharge method
or sputtering method, the starting material for
introduction of the group III atoms or the group V
1~ atoms, and the starting material for introduction of
oxygen atoms, nitrogen atoms or carbon atoms may be
used together with the starting material for formation
of the charge injection preventive layer as described
above, while controlling their amounts in the layer
formed,
As such starting materials for introduction
of carbon atoms, oxygen atoms and/or nitrogen atoms,
or the starting materials for introduction of the
group III atoms or the group V atoms, most of gaseous
substances or gasified gasifiable substances contain-
ing at least one of carbon atoms, oxygen atoms and
nitrogen atoms, or the group III atoms or the group V
atoms may be employed.
For example, for incorporating oxygen atoms,
2~ a startin~ gas containing silicon atom (Si) as the
constituent atom, a starting gas containing oxygen
atoms (O) as the constituent atom and optionally a
~30~L9
- 65 -
1 starting gas containing hydrogen atom (H) and/or
halogen atom (X) as the constituent atom may be used
as a mixture with a desired mixing ratio. Alternative-
ly, a starting gas containing silicon atom (Si) as
the constituent atom and a starting gas containing
oxygen atom (O) and hydrogen atom (H) as the consti-
tuent atoms may be mixed also at a desired mixing
ratio, or a starting gas containing silicon atoms
(Si) as the constituent atom and a starting gas
containing the three of silicon atom (Si), oxygen
atom (O) and hydrogen atom (H) as the constituent
atoms may be used as a mixture.
As another method, a gas mixture comprising
a starting gas containing silicon atom (Si) and
hydrogen atom (H) and a starting gas containing
oxygen atom (O) may be also employed.
As the starting gas for introduction of
oxygen atoms and nitrogen atoms, there may be in-
cluded, for example, oxygen (2)~ ozone (O3)~
nitrogen monooxide (NO), nitrogen dioxide (NO2),
dinitrogen monoxide (N2O), dinitrogen trioxide (N2O3),
trinitrogen tetraoxide (N2O4)) dinitrogen pentaoxide
(N2O5), nitrogen trioxide (NO3), nitrogen (N2),
ammonia (NH3), hydrogen azide (HN3), hydrazine
(NH2NH2). As the compound containing silicon (Si),
oxygen (O) and hydrogen atom (H) as the constituent
atoms, there may be included lower siloxanes contain-
~L3~
- 66 ~
1 ing silicon atoms (Si), oxygen atoms (O) and hydrogen
atoms (H) such as disiloxane (H3SiOSiH3), trisilo~ane
(H3SioSiH2oSiH3) and the like.
~ s carbon atom containing compounds for the
starting material for introduction of carbon atoms,
there may be included, for example, saturated hydro-
carbons having l to 4 carbon atoms, ethylenic hydro-
carbons having 2 to 4 carbon atoms, acetylenic
hydrocarbons having 2 to 3 carbon atoms, etc.
More specifically, typical examples are
saturated hydrocarbons such as methane (CH4), ethane
(C2H6), propane (C3H8), n-butane (n-C4Hl0), pentane
(C5Hl2); ethylenic hydrocarbons such as ethylene
(C2H4), propylene (C3~6), butene-l (C4H8), butene-2
15 (C4H8), isobutylene ~C4H8), pentene (C5Hlo); and
acetylenic hydrocarbons such as acetylene (C2H2),
methylacetylene (C3H4), butyne (C4H6) and the like.
Typical examples of the starting gas having
Si, C and H as constituent atoms are alkylsilanes
20 such as Si(CH3)4, Si(C2H5)4 and the like.
When the glow discharge method is used for
~orming a charge injection preventive layer contain
ing the group III atoms or the group V atoms, the
starting materials which become the starting gases
for ~ormation of the layer comprise one selected
suitably from among the starting materials for
formation of the charge injection preventive layer
~3~
- 67 -
1 constituted of polycrystaline silicon or A~Si(H,X)
as mentioned a~ove and a starting material for
introduction of the group III atoms or the group V
atoms added thereto. As such starting material ~or
introduction of the group III atoms or the group V
atoms may be any of gaseous substances or gasified
gasifiable substances containing the group III atoms
or the group ~ atoms as the constituent atom.
Specific examples of such starting materials
for introduction of the group III atoms may include
those for introduction of boron atoms such as hydro-
genated boron, including B2H6, B4Hlo, B5Hg, B5Hlo,
B6Hlo~ B6H12, B6H14 and the like, halogenated boron
such as BF3, BC12, BBr3 and the like. Otherwise,
AlC13, GaC13, InC13, TlC13 may be also employed.
The starting material for introduction of
the group V atoms which can be effectively used in the
present invention may include hydrogenated phosphorus
such as PH3, P2H4 and the like; halogenated phosphorus
~0 such as PH~I, PF3, PF5, PC13, PC15, PBr3, PBr5, PI3
and the like for introduction of phosphorus atoms.
Otherwise, AsH3, AsF3, AsC13, AsBr3, AsF5, SbH3,
SbF3, SbF5, SbC13, SbC15, BiH3, BiC13, BiBr3, etc.
may be also employed as effective starting ma~erials
for introduction of the group V atoms.
The content of the group III atoms or the
group V atoms in the charge injection preventive
~3~
- 68 -
1 layer containing the group III atoms or the group V
atoms can be controlled freely by cGntrolling the
gas flow rates, the gas flow rate ratios of the
starting materials for introduction of the group III
atoms or the group V atoms, the discharging power,
the substrate temperature and the pressure in the
deposition chamber, etc.
The substrate temperature for the purpose of
accomplishing effectively the objects of the present
invention should be selected suitably within the
optimum range. ~hen a charge injection preventive
layer 302, 402 consisting of A-Si(H,X) is formed, it
should be generally 50 to 350C, preferably 100 to
300C. When a charge injection preventive layex is
formed of polycrystalline silicon, it should be
generally 200C to 700C, preferably 250C to 600C.
For formation of the charye injection pre-
ventive layer in the present invention, it is de-
sirable to employ the glow discharge method or the
sputtering method for the reasons such as relatively
easier severe control of the composition ratio of the
atoms constituting the layer or control of the layer
thickness, and in the case of forming a charge
injection preventive layer according to these layer
2S forming methods, discharging power or gas pressure
during layer formation is also one of important
factors influencing the characteristic of the charge
~3~
~ 69 -
1 injection preventive layer to be prepared similarly
as the above substrate temperature.
The discharging power condition for preparing
effectively the charge injection preventive layer
having the characteristics for accomplished the
objects in the present invention with good productivity
and efficiency may be generally 1100 to 5000 W,
preferably 1500 to 4000 W for the substrate temper-
ature (Ts) of 200 to 350C and generally 100 to 5000
W, preferably 200 to 4000 W for the substrate temper-
ature of 350 to 7Q0C, in the case of forming a
charge injection preventive layer constituted of
polycrystalline silicon, or generally 10 to 1000 W,
preferably 20 to 500 W in the case of forming a
charge injection preventive layer constituted of A-
Si(H,X). The gas pressure within the deposition
chamber may be 1~ 3 to 0.8 Torr, preferably 5 x 10 3 to
0.5 Torr in the case of forming a charge injection
preventive layer constituted of polycrystalline
20 silicon or 0.01 to 1 Torr, preferably 0.1 to 0.5
Torr in the case of forming a charge injection pre-
ventive layer of A-Si(H,X).
In the present invention, the numerical
value ranges desirable for the substrate temperature,
discharging power for preparing a charge injection
preventive layer may be the values within the ranges
as mentioned above, but these layer forming factors
~3~6~
- 70 -
I are not determined independently and separately, but
it is desirable that the optimum values for the
factors for forming respective la~ers should be
determined hased on the mutual organic relationship
so that a charge injection preventive layer with
desired characteristics may be formed.
Fig. lE and Fig. lF illustrate schematically
the fifth and sixth pr~ferred embodiments of the
light-receiving member for electrophotography of the
present invention.
The light-receiving member for electrophoto-
graphy shown in Fig. lE and Fig. lF has a light-
receiving layer 500, 600 on the substrate 501 r 601
on the substrate for light-receiving member, said
15 light-receiving layer 500, 600 comprising a longer
wavelength light absorbing layer 507 ~ 607 r a charge
injection preventive layer 502, 602, a photoconductive
layer 503, 603 comprising A-Si(H,X) and having photo-
conductivity, and surface layer 504, 604. 606 shows
an adhesion layer.
The light-receiving member 500, 600 shown in
Fig. lE and lF corresponds to the light-receiving
member for electrophotography 300, 400 shown in Fig.
lC, lD and, except for having a longer wavelength
light absorbing layer (IR layer~ 507, 607 ~ the light-
receiving member for electrophotography 500 shown in
Fig. lE is entirely the same as the light-receiving
- 71 -
member for electrophotography 300 shown in Fig. lC,
and the light-receiving member for electrophoto-
graphy 600 shown in Fig. lF as the light-receiving
member for electrophotography 400 shown in Fig. lD.
Accordingly, description except for the
longer wavelength light absorbing layer 507, 607 is
omitted below.
Longer Wavelength Absorbinq Layer
_ _ _
The longer wavelength absorbing layer 507,607
in the present invention is constituted of an in-
organic material containing silicon atoms and germanium
atoms (polycrystalline material or amorphous material),
and the germanium atoms contained in said layer may
be contained uniformly throughout the layer, or
alternatively may be contained throughout the layer
but with nonuniform distributed concentration in the
layer thickness ~irection. However, in either case,
it is required also for uniformi~ation of the
characteristics in the interplanar direction that
they should be contained ~hroughout the layer with
uniform distribution in the interplanar direction in
parallel to the surface of the substrate. That is r
the germanium atoms may be contained throughout the
layer thickness direction in the longer wavelength
absorbing layer 507,607 and in the state enriched
toward the above substrate side opposite to the side
tthe free surface side of the light-receiving layer)
~3~
1 where the above substrate is provided, or in the
distribution state opposited thereto.
In the light-receiving member of the present
invention, the distrihution state of germanium atoms
5 contained in the longer wavelength absorbing layer
507,607 as mentioned above should desirably take the
distribution state as mentioned above in the layer
thickness direction, while a uniform distribution
state in the interplanar direction in parallel to
the surface of the substrate.
Also, in one preferred embodiment, the
distribution state of germanium atoms in the longer
wavelength absorbing layer 507,607 is such that
germanium atoms are distributed continuously through-
o~t the whole layer region and the distributedconcentration C in the layer thickness direction is
given a change in which it is reduced from the
substrate side toward the charge injection preventive
layer, and therefore affinity between the longer
wavelength absorbing layer 507,607 and the charge
injection preventive layer 502,602 is excellent,
and also by making extremely greater the distributed
concentration C of germanium atoms at the end portion
on the substrate side as described later, the
light on the wavelength side which cannot substantial-
ly be absorbed by the photoconductive layer 503, 603
can be absorbed substantially completely by the longer
~3~46~
- 73 -
I wavelength absorbing layer, whereby interference by
reflection from the subs-trate surface can be prevented.
Figs. 2~ through 27 show typical examples
when the distribution state in the layer thickness
direction of germanium atoms contained in the longer
wavelength absorbing layer 507, 607 of the light
receiving member in the present invention is non-
uniform .
In Figs. 22 through 27, the axis of abscissa
indicates the distributed concentration C of germanium
atoms, and the axis of ordinate the layer thickness
of the longer wavelength absorbing layer, tB showing
the position of the end face of the longer wavelength
absorbing layer 507, 607 on the substrate side, tT
the position of the end face of the longer wavelength
absorbing layer 507, 607 on the opposite side to the
substrate side. ~That is, the longer wavelength
absorbing layer containing germanium atoms is formed
from the tB side toward the tT side.
Fig. 22 shows a first typical example of the
distribution in the layer thickness direction of
germanium atoms contained in the longer wavelength
absorbing layer.
In the example shown in Fig. 22, from the
~5 interface position tB where thé surface on which the
longer wavelength absorbing layer 507, 607 containing
germanium atoms is formed contacts the surface of
~3~6~
- 7~ -
said longer wavelength absorbing layer 507, 607 to
the position t8, germanium atoms are contained in
the longer wavelength absorbing layer 507, 607 formed
while the distributed concentration C of germanium
atoms taking a constant value of C46, and the
concentration is reduced gradually and continuously
from the concentration C2 from the position tl to the
interface position tT. At the interface position t
the distributed concentration C of germanium atoms
is made C48.
In the example shown in Fig. 23, the distri-
buted concentration C of germanium atoms contained
is reduced from the concentration C49 gradually and
continuously from the position tB to the position
1~ tTI until it becomes the concentration C50 at the
position tT~
In the case of Fig. 24, the distributed
concentration C of germanium atoms is made a constant
value of C51 from the position tB to the position
t9, and reduced gradually and continuously between
the position tg and the position tT~ until the
distributed concentration C is made substantially
zero at the position tT (here, substantially zero
means the case of less than detectable limit of
~5 amount).
In the case of Fig. 25, the distributed
concentration C of germanium atoms is reduced from
~3~
1 the concentration C53 continuously and gra~ually
from the position tB to the position tT, until it
is made substantially zero at the position tT~
In the example shown in Fig. 26, the distri-
buted concentration C of germanium atoms is constantlya value of C54 between the position tB and the
position tlo, and is made a concentration ~55 at the
position tT. setween the positions tlo and tT~ the
distributed concentration C is reduced as a first
order function from the position tlo to the position
tT .
In the example shown in Fig. 27, the distri-
buted concentration C of germanium atoms is reduced
from the concentration C56 to substantially zero as
a first order function from the position tB to the
pOSition tT.
As described above about some typical ex-
amples of distribution state in the layer thickness
direction of germanium atoms contained in the longer
wavelength absorbing layer by referring to Figs. 22
through 27, in the present invention, the case of
providing a distribution state of germanium atoms
having a portion of higher distributed concentration
C of germanium atoms on the substrate side and having
a portion of the above distributed concentration C
which has been made considerably made lower as
compared with the substrate side on the interface
~L3a~ 9
- 76 -
tT side may be mentioned as a preferable example.
As the distribution state in the layer thickness
direction of germanium atoms, it is desirably that the
layer formation should be effected so that the
maximum value Cmax of the distributed concentration
of germanium atoms should preferably be 1000 atomic
ppm or more, more preferably 5000 atomic ppm or more,
optimally 1 x 104 atomic ppm or more, based on the
sum with silicon atoms.
In the present invention, the content of
germanium atoms contained in the longer wavelength
absorbing layer 507, 607 may be determined as
desired so as to accomplish effectively the objects
of the present invention, but may be preferably 1 to
10 x 10 atomic ppm, more preferably 100 to 9.5 x
105 atomic ppm, optimally 500 to 8 x 105 atomic ppm,
based on the sum with silicon atoms.
The above-mentioned longer wavelength
absorbing layer 507, 607 may also contain at least
one of substances for controlling conductivity
(valence electron controller), oxygen atoms, nitrogen
atoms and carbon atoms.
As the substance for controlling conductivity
to be contained in the charge injection preventive
layer 102, there may be mentioned such impurities
in the field of semiconductors as described in the
explanation of the charge injection preventive
~L3~4~
I layer 302, ~02.
In the present invention, the ~ontent of the
su~stance for controlling conductivity characteristic
to be contained in the longer wavelength absorbing
layer 507, 607 may be preferably 0.01 to 5 x 105
atomic ppm, more preferably 0.5 to l x 104 atomic ppm,
optimally 1 to 5 x 103 atomic ppm.
The content of nitrogen atoms (N), oxygen
atoms (O), carbon atoms (C) or the sum of the contents
of two or more of these in the longer wavelength
absorbing layer 507, 607 may be preferably 0.01 to
40 atomic ~, more preferably 0.05 to 30 atomic ~,
optimally 0.1 to 25 atomic %.
In the present invention, the layer thickness
1~ of the longer wavelength absorbing layer 507, 607
-may preferably be 30 A to 50 ~m, more preferably 40 A
to 40 ~m, optimally 50 A to 30 ~m.
In the present invention, typical examples
of halogen atoms (~) to be incorporated in the longer
~n wavelength light absorbing layer 507, 607 are F, Cl,
Br, I, especially preferably F and Cl.
In the present invention, formation of the
longer wavelength light absorbing layer 507, 607
may be conducted according to the vacuum deposition
method utilizing discharging phenomenon, such as
glow discharge method, sputtering method or ion-
plating method.
~3~6~L93
- 78 -
1 For example, for formation of the longer
wavelength absorbing layer 507, 607 constituted of
a polycrystalline or amorphous material containing
silicon atoms and germanium atoms according to the
glow discharge method, the basic procedure comprises
introducing a starting gas for Si supply capable of
supplying silicon atoms (Si) and a starting gas for
Ge supply capable of supplying germanium atoms (Ge),
optionally together with a starting gas for intro-
duction of hydrogen atoms (H) or/and a startinggas for introduction of halogen atoms (X) into a
deposition chamber which can be internally brought
to a reduced pressure to excite glow discharging
within said deposition chamber and form a layer on
the surface of a predetermined substrate which is
previously placed at a predetermined position. On
the other hand, f~or formation according to the
sputtering method, a target constituted of Si or two
sheets of said target and a target constituted of Ge,
or a target of a mixture of Si and Ge may be used
in an atmosphere such as of an inert gas of Ar, He,
etc. or a gas mixture based on these gases, and a
starting gas for Ge supply optionally diluted with
a diluting gas such as He, Ar, etc. is introduced,
optionally together with a gas for introduction of
hydrogen atoms (H) or/and halogen atoms (X), into
the deposition chamber for sputtering and form a
~3~1191 E;~9t
- 79 -
1 plasma atmosphere of desired gases.
The substance which can be the starting
material gas for Si supply to be used in the present
invention may include gaseous or gasifiable hydro-
genated silicon (silanes) such as Si~4, Si2H6, Si3H8,
Si4Hlo and the like as effective ones, particularly
preferably SiH~, Si2H6 for easiness in handling during
layer formation working, good Si supply efficiency,
etc.
1~ The substance which can be the staring
material gas for Ge supply may include gaseous or
gasifiable hydrogenated germanium such as GeH4, Ge2H6,
Ge H , Ge4H10, Ge5H12~ Ge6H14' Ge7H16' 8 18 9 20
and the like as effective ones, particularly preferably
15 GeH4, Ge2H6, Ge3H8 for easiness in handling during
layer formation working, good Ge supply efficiency,
etc.
As the effective starting gas fox incorporation
o halogen atoms to be used in the present invention,
~0 there may be mentioned a number of halogen compounds
such as halogen gases, halides, interhalogen compounds
and silane derivatives substituted with halogens which
are gaseous of gasifiable.
Further, it is also effective in the present
~5 invention to use a gaseous or gasifiable silicon
compound containing halogen atoms which is consti-
tuted of both silicon atoms and halogen atoms.
3L3~
- 80 -
I Typical examples of halogen compounds
preferably used in the present invention may include
halogen gases such as of fluorine, chlorine, bromine
or iodine and interhalogen compounds such as BrF,
ClF, ClF3, BrF5, BrF3, IF3~ IF7, ICl, IBr, etc.
As the silicon compound containing halogen
atom, namely the so-called silane derivatives substi-
tuted with halogen atoms, silicon halides such as
SiF~, Si2F6, SiC14, SiBr4, or the like are preferred.
1~ When the specific light-receiving member of
this invention is formed according to the glow dis-
charge method by use of such a silicon compound
containing halogen atoms, it is possible to form a
layer constituted of A-Si:H containing halogen
1~ atoms on a desired substrate without use of a hydro-
genated silicon gas as the starting gas capable of
supplying Si.
In the case of preparing a layer containing
halogen atoms according to the glow discharge method,
the basic procedure comprises introducing a silicon
halide as the starting material gas for Si supply
together with a gas such as Ar, H2, He, etc. at a
predetermined mixing ratio and gas flow rates into
a deposition chamber for formation of a layer, and
e~citing glow discharge to form a plasma atmosphere
of these gases, whereby a desired layer can be
formed on a desired substrate. For effecting
~3~4~
- 81 -
I introductlon of hydrogen atoms, a gas of a silicon
compound containing hydrogen atoms may be further
mixed into these gases in a desired amount for layer
formation.
S In the case of forming a longer wavelength
light absorbing layer 507, 607, as the starting gas
for introduction of halogen atoms, the halogen com-
pounds or silicon compounds containing halogens as
mentioned above can effectively be used. In
addition, it is also possible to use a gaseous or
gasifiable substance such as halides containing
hydrogen atom as one constituent, for example~ hydro
genated germanium halide such as GeHF3, GeH2F2, GeH3F,
GeHC13, GeH2C12, GeH3Cl, GeHBr3, GeH2Br2~ GeH2Br,
GeHI2, GeH2I2, GeH3I and the like; and halogenated
germanium such as GeF4, GeC14, GeBr4, GeI4, GeF2,
GeC12, GeBr2, Gel2 and the like as an effective
starting material for formation of a longer wave-
length light absorbing layer.
The respective gases used are not limited
only to single species, but a plural number of gas
species may be used at a desired mixing ratio.
For formation of a layer comprising A-Si(H,X)
by the reactive sputtering method or the ion-plating
method, for example, a target of Si is used and
sputtering is effected thereon in a suitable gas
plasma atmosphere in the case of the sputtering
~3g~
- 82 -
1 method. Alternatively, in the case of ion-plating
method, a polycrystalline or single crystalline
silicon is placed as vaporization source in a vapor
deposition boat, and the silicon vaporization source
is vaporized by heating by resistance heating method
or electron beam method (EB method) thereby to permit
vaporized flying substances to pass through a suitable
gas plasma atmosphere.
During this procedure, in both of the sputter-
ing method and the ion-plating method, for introduction
of halogen atoms into the layer formed, a gas of a
halogen compound as mentioned above or a silicon
compound containing halogen as mentioned above may
ba introduced into the deposition chamber to form a
plasma atmosphere of said gas therein.
When hydrogen atoms are to be introduced, a
starting gas for~introduction of hydrogen atoms such
as H2 and a gas such as silanes as mentioned above
may be introduced into the deposition chamber for
sputtering, followed by formation of a plasma
atmosphere of said gases.
In the present invention, as the starting
gas for introduction of halogen atoms, the halogen
compounds or silicon compounds containing halogens
or germanium compounds containing halogens as
mentioned above can effectively be used. In
addition, it is also possible -to use a gaseous or
~L3g[~6~9Ç
- 83 -
1 gasifiable halide containing hydrogen atom as one of
the constituents such as hydrogen halide, including
E~F, HCl, HBr, HI and the like or halo-substituted
hydrogenated silicon, including SiH2F2, SiH2I2,
SiH2C12, SiHC13, SiH2Br2, SiHBr3and the like as an
effective starting material for formation of a longer
wavelength light absorbing layer.
These halides containing hydrogen atom, which
can introduce hydrogen atoms very effective for
controlling electrical or optical characteristics
into the layer during formation of the layer simul-
taneously with introduction of halogen atoms, can
preferably be used as the starting material for
introduction of halogen atoms.
For incorporation of hydrogen atoms structur
ally into the layer formed, in addition to those as
mentioned above, H2 or a gas of hydrogenated silicon,
including SiH4, Si2H6, Si3H8, Si4Hlo
permitted to be co-present with a silicon compound
~o for supplying Si in a deposition chamber, wherein
discharging is excited.
For example, in the case of the reactive
sputtering method, a Si target is used and a gas
for introduction of halogen atoms and H2 gas are
~5 introduced together with, if necessary, an inert
gas such as He, Ar, etc. into a deposition chamber,
wherein a plasma atmosphere is formed to effect
~3~
- 84 -
I sputtering of said Si target, thereby forming a layer
of A-Si (H,X) on the substrate.
Further, there may also be introduced a gas
such as of B2H6 or others in order to effect also
doping of impurities.
The amount of hydrogen atoms (H) or halogen
atoms (X) incorporated in the longer wavelength
light absorbing layer in the light-receiving member
for electrophotography according to the present
invention, or total amount of both of these atoms,
may be preferably 0.01 to 40 atomic ~, more prefer~
ably 0.05 to 30 atomic %, optimally 0.1 to 25 atomic ~.
For controlling the amounts of hydrogen atoms
(H) or/and halogen atoms (X) in the layer formed,
1~ the substrate temperature or/and the amounts of the
starting materials for incorporation of hydrogen
atoms (H) or halogen atoms (Xj to be introduced into
the deposition device system or the discharging power
may be controlled.
For incorporating the group III atoms or the
group V atoms, and the carbon atoms, oxygen atoms
or nitrogen atoms in the longer wavelength light
absorbing layer 507, 607, during formation of the
longer wavelength light absorbing layer 507, 607,
by glow discharge or reactive sputtering method,
the starting material for introduction of the group
III atoms or the group V atoms, and the starting
- 85 -
material for in-troduction ofoxygen atoms, nitrogen
atoms or carbon atoms may be used together with the
starting material for formation of the longer wave-
length light absorbing layer as described above,
5 wllile controlling their amounts in the layer formed.
As such starting materials for introduction
of carbon atoms, oxygen atoms or/and nitrogen atoms,
or the starting materials for introduction of the
group III atoms or the group V atoms, most of gaseous
substances or gasified or gasifiable substances con-
taining at least one of carbon atoms, oxygen atoms
and nitrogen atoms, or the group III atoms or the
group V atoms may be employed.
For example, for incorporating oxygen atoms,
a starting gas containing silicon atom (Si) as the
constituent atom, a starting gas containing oxygen
atoms (O) as the~constituent atom and optionally a
starting gas containing hydrogen atom or/and halogen
atom (X) as the constituent atom may be used as a
mixture with a desired mixing ratio. Alternatively,
a ~tarting gas containing silicon atom (Si) as the
constituent and a starting gas containing oxygen atom
(O) and hydrogen atom (H) as the constituent atoms may
be mixed also at a desired mixing ratio, or a starting
gas containing silicon atom (Si) as the constituent
atom and a starting gas containing the three of sili-
con atom (Si), oxygen atom (O) and hydrogen atom (H)
g
- 86 -
1 as the constituent atoms may be used as a mixture.
As another method~ a gas mixture comprising
a starting gas containing silicon atom (Si) and
hydrogen atom (H) and a starting gas containing
oxygen atom (o) may be also employed.
As the starting gas for introduction of
oxygen atoms and nitrogen atoms, there may be
included, for example, oxygen (2)' ozone (O3),
nitrogen monooxide (NO), nitrogen dioxide (NO2),
dinitrogen monooxide (N2O), dinitrogen trioxide
tN2O3), dinitrogen tetraoxide (N2O4), dinitrogen
pentaoxide (N2O5), nitrogen trioxide (NO3), nitrogen
(N2), ammonia (NH3), hydrogen azide (HN3), hydrazine
(NH2NH2). As the compound containing silicon (Si),
oxygen (O) and hydrogen atom (H) as the constituent
atoms, there may be included lower siloxanes such as
disiloxane (H3SiOSiH3), trisiloxane (H3SiOSiH2OSiH3)
and the like.
As carbon ato-n containing compounds for the
starting material for introductionof carbon atoms,
there may be included, for example, saturated hydro-
carbons having 1 to 4 carbon atoms, ethylenic hydro-
carbons having 2 to 4 cartons, acetylenic hydrocarbons
having 2 to 3 carbon atoms, etc.
More specifically, typical examples are
saturated hydrocarbons such as methane (CH4), ethane
(C2H6), propane (C3H~), n-butane (n-C4H10), pentane
~3~
- 87 -
1 (C5Hl2); ethylenic hydrocarbons such as ethylene
(C2H4), propylene (C3H6), butene-l (C4H8), butene-2
(C4H8), isobutylene (C4H8), pentene (C5Hlo); and
acetylenic hydrocarbons such as acetylene (C2H2),
methylacetylene (C3H4)~ butyne (C4H6) and the like.
Typical examples of the starting gas having
Si, C and H as constituent atoms are alkylsilicides
such as Si(CH3)4, Si(C2H5)4 and the like.
When the glow discharge method is used for
1~ forming a longer wavelength light absorbing layer
507, 607 containing the group III atoms or the group
V atoms, the starting materials which become the
starting gases for formation of said layer comprise
one selected suitably from among the starting
materials for formation of the longer wavelength
light absorbing layer 507, 607 and a starting material
for introduction of the group III atoms or the group
V atoms added thereto. As such starting material
for introduction of the group III atoms or the group
V atoms may be any of gaseous substances or gasified
gasifiable substances containing the group III atoms
or the group V atoms as the constituent atom.
Specific examples of such starting materials
for introduction of the group III atoms may include
those for introduction of boron atoms such as hydro-
genated boron, including B2H6, B4Hlor B5~9, B5Hlo,
B6Hlot s6Hl2, B6Hl4 and the like, halogenated boron
~31~46~LSI
- 88 -
I such as BF3, sC12, ssr3 and the like. Otherwise,
AlC13, GaC13, InC12, TlC13, etc., may be also employ-
ed.
The starting material for introduction of
the group V atoms which can be effectively used in
the present invention may include hydrogenated
phosphorus such as PH3, P2H4 and the like; haloge-
nated phosphorus such as PH4I, PF3, PF5, PC13 PC15,
PBr3, PBr5, PI3 and the like for introduction of
phosphorus atoms. Otherwise, AsH3, AsF3, AsC13,
AsBr3, AsF5 r SbH3, SbF3, SbF5, SbC13, SbC15, BiH3,BiC13,
BiBr3, etc. may be also employed as effective start-
ing materials for introduction of the group V atoms.
The content of the group III atoms or the
group V atoms in the longer wavelength light absorb-
ing layer 507, 607 containing the group III atoms or
the group V atoms can be controlled desirably by
controlling the gas flow rates, the gas flow rate
ratios of the starting materials for introduction of
2~ the group III atoms or the group V atoms, the dis-
charging power, the substrate temperature and the
pressure in the deposition chamber, etc.
The substrate temperature for the purpose
of accomplishing effectively the objects of the
present invention should be selected suitably within
the optimum range. When a longer wavelength light
absorbing layer 507, 607 is formed of a polycrystal-
- 89 -
I line material, it should preferably 200 to 700C,
more preferably 250 to 600C. When a longer wave-
length light absorbing layer is formed of an amorphous
material, it should preferably 50C to 350C, more
preferably 100C to 300C.
For formation of the longer wavelength light
absorbing layer 507, 607, it is desirable to employ the
glow discharge method or the sputtering method for
the reasons such as relatively easiness in delicate
control of the composition ratio of the atoms consti-
tuting the layer or or the layer thic~ness compared
to other methods, and in the case of forming a longer
wavelength light absorbing layer 507, 607 according
to these layer forming methods, discharging power or
gas pressure during layer formation is also one of
important factors influencing the characteristic of
the longer wavelength light absorbing layer 507, 607
to be prepared similarly as the above substrate
temperature.
The discharging power condition for preparing
effectively the longer wavelength light absorbing
layer 507, 607 having the characteristics for
accomplishing the objects in the present invention
with good productivity and efficiency may be prefer-
ably 100 to 5000 W, more preferably 200 to 2000 W, in
the case of forming a longer wavelength light absorb-
ing layer 507, 607 constituted of a polycrystalline
~3~
- 90 -
1 material, or preferably lO to lO00 W, more preferably
20 to 500 W in the case of forming a longer wave-
length light absorbing layer 507, 607 constituted of
an amorphous material. The gas pressure within the
5 deposition chamber may be preferably lO 3 to 0.8
Torr, more preferably 5 x lO 3 to 0.5 Torr in the
case of forming a longer wavelength light absorbing
layer 507, 607 constituted of a polycrystalline
material, or preferably O.Ol to l Torr, more prefer-
ably O.l to 0.5 Torr in the case of forming a longerwavelength light absorbing layer 507, 607 constituted
of an amorphous material.
In the present invention, desirable numerical
value ranges of substrate temperature and discharging
power for preparing a longer wavelength light absorb-
ing layer 507, 607 may be the values within the ranges
as ~entioned above, but these layer forming factors
are not determined independently and separately, but
it is desirable that the optimum values for the
factors for forming respective layers should be
determined based on the mutual organic relationship
so that a longer wavelength light absorbing layer 507,
607 with desired characteristics may be formed.
Fig. lG and Fig. lH show the seventh and the
~5 eighth examples of the preferred embodiments of the
light-receiving member for electrophotography of the
present invention.
~30~
~/ -
1 The respective layer constitutions of the
light-receiving members for electrophotography shown
in Fig. lG and Fig. lH are the same as the respective
light-receiving members shown in Fig. lC and Fig. lD
except that the longer wavelength light absorbing
layers (IR layers) 707, 807 posessed by the light-
receiving members for electrophotography shown in
Fig. lE and Fig. lF are provided in place of the
charge injection preventive layers 302, 402 posessed
by the light-recei~ing members for electrophotography
shown in Fig. lC and Fig. lD.
The respective light-receiving members for
electrophotography shown in Fig. lG and Fig. lH can
absorb effectively the longer wavelength light ef-
fectively by providing longer wavelength light absorb-
ing layers 707, 807 between the substrates 701, 801
and the photoconductive layers 703, 803, whereby
interference when using a coherent light such as
laser beam can be effectively prevented.
Fig. 28 through Fig. 32 respectively show
examples of light-receiving members for electrophoto-
graphy having light-receiving layers with the same
layer constitutions as the light-receiving me~bers
for electrophotography shown in Figs. lC through lG
on the same substrate as the substrate 1501 of the
light-receiving member for electrophotography 1500
shown in Fig~ 3.
~3~9~9~
That is, in Figs. 28 through 32, 900, 1000,
1100, 1200, and 1300 represent light-receiving layers,
901, 1001, 1101, 1201, and 1301 substrates, 902,
1002, 1102, and 1202 charge injection preventive
layers, 903, 1003, 1103, 1203, and 1303 photoconductive
layers, 904, 1004, 1104, 1204, and 1304 surface layers,
905, 1005, 1105, 1205, and 1305 free surfaces, 906 and
1206 adhesion layers, 1107, 1207, and 1307 longer
wavelength light absorbing layers, respectively.
1~ Next, the method for forming the light-
receiving member is outlined below.
Fig. 33 shows an example of the apparatus
for preparation of the light-receiving member for
electrophotography.
I~ The gas bombs 3302 through 3306 in the Figure
are hermetically filled with the starting gases for
formation of the respective layers of the present
invention. For example, 3302 is a SiH4 gas (purity
99.999%) bomb, 3303 a B2H6 gas diluted with H2
~0 (purity 99.999 %, hereinafter abbreviated as B2H6/H2)
bomb, 3304 a H2 gas (purity 99.99999 %) bomb, 3305 a
NO gas (purity 99.999 ~) bomb, and 3306 a CH4 gas
(purity 99.99 %) bomb.
For permitting these gases to flow into the
~5 reaction chamber 3301, on confirmation that the valves
3322 to 3326 of the gas bombs 3302 to 3306 and the leak
valve 3335 are closed, and also on confirmation that
~ 1314~
- 93 -
1 the inflow valves 331~ to 3316, the outflow valves
3317 to 3321, and the auxiliary valves 3332 to 3333
are opened, first the main valve 3334 is opened to
evacuated the reaction chamber 3301 and the gas
pipelines. Next, when the reading on the vacuum
gauge 3336 becomes about 5 x 10 6 Torr, the auxiliary
valves 3332 to 3333 and the outflow valves 3317 to
3312 are closed.
Referring to an example when a light-
receiving member for electrophotography with a layer
constitution shown in Fig. lF is formed on the
substrate cylinder 3337, SiH4 gas from the gas bomb
3302, H2 gas from the gas bomb 3304, B2H6/M2 gas
fxom the gas bomb 3303, and NO gas from the gas bomb
1~ 3305 are permitted to flow into the mass flow con-
trollers 3307 to 3310 by opening the valves 3322 :
through 3325 to control the pressures at the outlet
pressure gauges 3327 to 3330 to 1 Kg/cm and opening
gradually the inflow valves 3312 to 3315. Subse~uent-
~0 ly, by opening gradually the outflow valves 3317 to3320 and the auxiliary valve 3332, the respective
gases are permitted to flow into the reaction chamber
3301. During this operation, the outflow valves
3317 to 3320 are controlled so that the ratio o~ SiH4
gas flow rate, B2H6/He gas ~low rate, and NO gas
flow rate may become a desired value and also the
opening of the main valve 3334 is controlled while
~3C~ L9
- 94 -
1 seeing the reading on the vacuum gauge 3336 so that
the pressure within the reaction chamber may become
a desired value. And, after the temperature of the
substrate cylinder 3337 is confirmed to be set at
a temperature of 50 to 350~ by the heater 3338, the
power 3340 is set at a desired power to excite glow
discharging within the reaction chamber 3301 and at
the same time the operation of changing gradually
the valve 3318 or/and 3320 manually or by use of an
externally driven motor to change the flow rate of
B2H6/H2 gas or/and NO gas following the change rate
curve pre~iously designed,thereby controlling the
distributed concentration of boron atoms or/and
oxygen atoms in the layer thickness direction contain-
ed in the layer formed.
At the point when a charge injection pre-
ventive layer containing boron atoms and oxygen
atoms to a desired thickness is formed, the outflow
valves 3320 and 3318 are closed, with shut down
of inflow of B2H6/He gas and NO gas, and at the same
time with control of flow rates of SiH4 yas and H2
gas by controlling the outflow valves 3317 and 3319,
layer formation is subsequently performed, thereby
forming a photoconductive layer containing none of
oxygen atoms and boron atoms on the charge injection
preventive layer to a desired thickness.
Also, when a photoconductive layer contain-
~3~
- 95 -
1 ing oxygen atoms or/and boron atoms is formed, the
outflow valves 3318 or/and 3320 may be controlled
to desired flow rates in place of being closed.
When halogen atoms are contained in the
charge injection preventive layer and the photo-
conductive layer, for example, SiF4 gas in further
added to the above gases to be delivered into the
reaction chamber 3301.
In formation of the respective layers,
depending on the selection of the gas species, the
layer forming speed can be enhanced. For example,
when layer formation is performed by use of Si2H6 gas
in place of SiH4 gas, the speed can be enhanced by
several times to improve productivity.
1~ For formation of the surface layer on the
photoconductive layer as prepared above, according
to the same valve~operations as in the case of
forming the photoconductive layer, for example, SiH4
gas, CH4 gas, and optionally a diluting gas such as
~0 H2, etc., may be flowed at desired flow rate ratio
into the reaction chamber 3301, followed by excitation
of glow discharging following desired conditions.
The content of carbon atoms contained in the
surface layer can be controlled as desired by varying
freely the flow rate ratio of SiH4 gas and CH4 gas
introduced into the reaction chamber 3301 as desired.
Also~ the content of hydrogen atoms contained
~L3 [~
- 96 -
in the surface layer can be controlled by, for
example, varying freely the flow rate of ~2 gas
introduced into the reaction chamber 3301 as desired.
All of the outflow valves other than those
S for necessary gases during formation of the respective
layer are closed as a matter of course and also, in
order to avoid remaining of the gases employed for
formation of the previous layer during formation of
each layer in the reaction chamber 3301, and in the
1~ pipelines from the outflow valves 3317 to 3321 to
the reaction chamber 3301, the operation of evacuating
internally the system once to high vacuum by closing
of the outflow valves 3317 to 3321 and full opening
of the main valve 3334 by opening of the auxiliary
valve 3332 is practiced, if necessary.
Also, durin~ layer formation, in order to
effect uniformiza~tion, the substrate cylinder 3337
may be also rotated at a desired constant speed by a
motor 3339.
~0 Example lA
By use of the preparation device shown in
Fig~ 33, a light-receiving member for electrophoto-
gxaphy was formed on an aluminum cylinder appli.ed
with mirror surface working following the prepar-
ation conditions in Table lA. The light-receiving
member (hereinafter expressed as drum) was set on an
electrophotographic device, and, under various
~L3~
- 97 -
1 conditions, electrophotographic characteristics such
as initial charging ability, residual potential,
ghost, etc., were checked, and also lowering in
charging ability, sensitivity deterioration and in-
5 crease of image defects after successive copying of1,500,000 sheets were examined Further, the image
flow of the drum in an atmosphere of high temperature
and high humidity of 35C and 85 % was also evalu-
ated. And, the drum completed of evaluation was
cut out at the portions corresponding to the upper,
middle and lower portions of the image portion to
prepare a samples, which were provided for quantitative
analysis of hydrogen contained in the surface layer
by utilization of SIMS, and also the component
lS profiles in the layer thickness direction of silicon
atoms (Si), carbon atoms (C) and hydrogen atoms (H)
in the surface layer were examined. The above
evaluation results and the maximum value of the
hydrogen content in the surface layer are shown in
Table 2A, and the above component profiles are
shown in Table 34. As shown in Table 2A, remarkable
superiority was observed in the respective items
particularly of initial charging ability, image
flow, residual potential, ghost and photosensitive
~5 irregularity in the axial direction, sensitivity
deterioration.
~3~ 9
- 98 -
1 Comparative example lA
Except for changing the preparation con-
ditions as shown in Table 3A, the drum and samples
for analysis were prepared by the same device and
method as in Example lA and provided for the same
evaluation and analysis. The results are shown in
Table 4A.
As can be seen from Table 4A, it was
recognized that the respective items were inferior
as compared with Example lA.
Example 2A, Comparative example 2A
The preparation conditions of the surface
layer were changed variously as shown in Table SA,
1~ with other conditions being the same as in Example
lA, to prepare a plural number of drums and
samples for analysis. These drums and samples were
evaluated and analyzed similarly as in Example lA
to obtain the results as shown in Table 6A.
~0
Example 3A
The preparation conditions of the photo-
conductive layer were changed variously as shown
in Table 7A, with other conditions being the same
~5 as in Example lA, to prepare a plural number of
drums. These drums were evaluated similarly as in
Example lA to obtain the results as shown in Table
~3~
99
1 8A.
Example 4A
The preparation conditions of the photo-
conductive layer were changed variously as shown inTable 9A, with other conditions being the same as
in Example lA, to prepare a plural number of drums.
These drums were evaluated similarly as in Example
lA to obtain the results as shown in Table 10A.
Example 5A
On substrate cylinders were formed adhesion
layers under several conditions as shown in Table
llA, followed further by formation of the light
receiving member thereon under the same preparation
conditions as in Example lA. Separately, samples
having only adhesion layers formed thereon were
prepared. The light-receiving members were subjected
to the same evaluation as in Example 1~, and a part
of the sample was cut out for examination of presence
or absence of crystallinity by determining the
diffraction pattern corresponding to Si (111) around
the diffraction angle 27 by means of a X-ray dif~
fraction device. The results are shown in Table 12.
Example 6A
On substrate cylinders were formed adhesion
- 100 -
1 layers under several conditions as shown in Table
13A, followed further by formation of the light
receiving member thereon under the same preparation
conditions as in Example lA. Separately, samples
having only adhesion layers formed thereon were
prepared. The light-receiving members were subject-
ed to the same evaluation as in Example lA, and a
part of the sample was cut out for examination of
presence or absence of crystallinity by deter~ining
the diffraction pattern corresponding to Si (111)
around the diffraction angle 27 by means of a X-
ray di~fraction device. The results are shown in
Table 14A.
Example 7A
A cylinder applied with mirror surface working
was further subiected to lathe working with sword
bit having various angles to prepare a plural number
of cylinders having a cross-sectional shape as shown
in Fig. 35 and various cross-sectional patterns as
shown in Table 15A. Said cylinder was successively
set in the prepatation device shown in Fig. 33 and
subjected to drum preparation under the preparation
cinditions similarly as in Example lA. The drum
prepared was evaluated variously by means of an
electrophotographic device of a digital exposure
function with the use of a semiconductor laser
~30~
-- 101 --
1 having a wavelength of 780 nm as the light source to
give the results shown in Table 16A.
Example 8A
The surface of the cylinder applied with
mirror surface working was applied with the so
called surface dimple formation treatment in which
it was subsequently exposed to falling of a large
number of balls for bearing to form numberless hitted
marks on the cylinder surface, to prepare a plural
number of cylinders having a cross-section shape as
shown in Fig. 36 and various cross-section patterns
as shown in Table 17A. Said cylinder was successive-
ly set in the preparation device shown in Fig. 33
and subjected to drum preparation under the prepar-
ation conditions similarly as in Example lA. The
drum prepared was evaluated variously by means of
an electrophotographic device of a digital exposure
~unction with the use of a semiconductor laser
h`aving a wavelength of 780 nm as the light source
to give the results as shown in Table 18A.
Table lB
By use of the preparation device shown in
~S Fig. 33, a light-receiving member for electrophoto-
graphy was formed on an aluminum cylinder applied
with mirror surface working following the preparation
~L3~
- 102 -
1 conditions in Table lB. Also, by use of the device
of the same model as shown in Fig. 33, samples having
only charge injection preventive layers formed on
the cylinder with the same specification were separate-
ly prepared. The light-receiving member (hereinafter
expressed as drum) was set on an electrophotographic
device, and, under various conditions, electrophoto-
graphic characteristics such as initial charging
ability, residual potential, ghost, etc., were
checked, and also lowering in charging ability,
sensitivity deterioration and increase of image
defects after successive copying for 1,500,000 sheets
were examined. Further, the image flow of the drum
in an atmosphere of high temperature and high humi-
dity of 35C and 85 % was also evaluated. And, thedrum completed of evaluation was cut out at the
portions corresponding to the upper, middle and
lower portions of the image portion to prepare
samples, which were provided for quantitative analysis
~o of hydrogen contained in the surface layer by
utilization of SIMS. Also, the sample having only
the charge injection preventive layer was cut out
in the same manner, and the diffraction pattern
corresponding to Si (lll) around the diffraction
~5 angle 27 was determined by a X-ray diffraction
device for examination of presence of crystallinity.
The above evaluation results, the maximum value of
- 103 -
l the hydrogen content in the surface layer and also
presence o~ crystallinity ~f the charg~ injection
preventive layer are comprehensively shown in Table
2B. As shown in Table 2B, remarkable superiority
5 was observed in the respective items particularly
of initial charging ability, image flow, residual
potential, ghost, increase of image defects and
photosensitive irregularity in the axial direction,
sensitivity deterioration.
Comparative example lB
Except for changing the preparation conditions
as shown in Table 3B, the drum and samples for
analysis were prepared by the same device and method
l~ as in Example lB and provided for the same evaluation
and analysis. The results are shown in Table 4B.
As can be seen from Table 4B, it was recog-
nized that the respective items were inferior as
compared with Example lB.
~0
Example 2B
By use of the preparation device shown in
Fig. 33, a light-receiving member for electrophoto-
graphy was formed on an aluminum cylinder applied
~5 with mirror surface working following the prepar-
ation conditions in Table 5B. Also, by use of the
device of the same model as shown in Fig. 33, samples
~3~ g
- 104 -
I having only charge injection preventive layers
formed on the cylinder with the same specification
were separately prepared. The light-receiving
member (hereinafter expressed as drum) was set on
5 an electrophotographic device, and, under various
conditions~ electrophotographic characteristics
such as initial charging ability, residual potential,
ghost, etc., were checked, and also lowering in
charging ability, sensitivity deterioxation and
l~ increase of image defects after successive copying
for l,500,000 sheets were examined. Further, the
image flow of the drum in an atmosphere of high
temperature and high humidity of 35C and 85 % was
also evaluated. And, the drum completed of evalu-
l~ ation was cut out at the portions corresponding tothe upper, middle and lower portions of the image
portion to prepare samples, which were provided for
quantitative analysis of hydrogen contained in the
surface layer by utilization of SIMS, and also the
~0 component profiles in the layer direction of silicon
atoms (Si~, carbon atoms (C) and hydrogen atoms (~)
in the surface layer were examined~ Further, the
component profiles of boron (B) and oxygen (O) in
the charge injection preventive layer were examined.
~5 Also, the sample having only the charge injection
preventive layer was cut out in the same manner,
and the diffraction pattern corresponding to Si ~lll)
~3119L~
- 105 -
1 around the diffraction angle 27 was determined by
a X-ray diffraction device for examination of
presence of crystallinityO The above evaluation
results and the maximum value of the hydrogen content
in the surface layer, and also presence or absence
of crystallinity of the charge injection preventive
layer are comprehensively shown in Table 6B. Further,
the component profiles of said elements in the above
surface layer are shown in Eig. 37, and the com-
ponent profiles of said elements in the above charge
injection preventive layer are shown in Fig. 37.
As shown in Table 6B, remarkable superiority
was observed in the respective items particularly of
initial charging ability, image flow, residual
potential, ghost, increase of image defects and
photosensitive irregularit~ in the axial direction,
sensitivity deterioration.
Example 3B, Comparative example 2B
The preparation conditions of the surface
layer were changed variously as shown in Table 7B,
with other conditions being the same as in Example
lB, to prepare a plural number of drums, which were
provided for the same evaluation. And the drums
completed of evaluation were cut out in the same
manner as in Example lB to give samples, which were
subjected to the same analysis. The above results
~3q~6~L9
- 106 -
1 are shown in Table 8B.
Example 4B
The preparation conditions of the photo-
conductive layer were changed variously as shown inTable 9B, with other conditions being the same as
in Example lB, to prepare a plural number of drums.
These drums were evaluated similarly as in Example
lB to obtain the results as shown in Table lOB.
Example 5B
The preparation conditions of the charge
injection preventive layer were changed variously
as shown in Table llB, with other conditions being
the same as in Example lB, to prepare a plural
number of drums and samples having only charge
injection preventive layers formed. These drums
and samples for analysis were subjected to the same
evaluation and analysis similarly as in Example lB
~0 to o~tain the results as shown in Table 12B.
Example 6B
The preparation conditions of the charge
injection preventive layer were changed variously
~5 as shown in Table 13B, with other conditions being
the same as in Example lB, to prepare a plural
number of drums and samples having only charge
~L3~ g
- 107 -
injection preventive layers formed. These drums
and samples for analysis were subjected to the same
evaluation and analysis similarly as in ~x~mple ls
to obtain the results as shown in Table 14s.
Example 7
On a substrate cylinder, an adhesion layer
was formed under several preparation conditions as
indicated in Table 15B, and further a light-receiving
member was formed under the same preparation con-
ditions as in Example lB. Separately, samples
having only adhesion layers formed were prepared.
The light-receiving member was subjected to the same
evaluation as in Example lB, while a part of the
sample was cut out and the diffraction pattern
correspondin~ to Si (111) around the diffraction
angle 27 was determined for examination of presence
or absence of crystallinity. The above results are
shown in Table 16B.
~0
Example 8B
On a substrate cylinder, an adhesion layer
was formed under several preparation conditions as
indicated in Table 17B~ and further a light-receiving
~5 member was formed under the same preparation con-
ditions as in Example lB. Separately, samples
having only adhesion layers formed were prepared.
~3~4 E;~
- 108 -
The light-receiving member was subjected to the same
evaluation as in Example lB, while a part of the
sample was cut out and the diffraction pattern
corresponding to Si (111) around the diffraction
angle 27 was determined for examination of presence
or absence of crystallinity. The above results are
shown in Table 18B.
Example 9B
A cylinder applied with mirror surface
working was further subjected to lathe working with
sword bit having various angles to prepare a plural
number of cylinders having a cross-sectional shape
as shown in Fig. 35 and various cross-sectional
patterns as shown in Table l9B. Said cylinder was
successively set in the preparation device shown
in Fig. 33 and subjected to drum preparation under
the preparation conditions similarly as in Ex-
ample lB. The drum prepared was evaluated various-
ly by means of an electrophotographic device of adigital exposure function with the use of a semi-
conductor laser having a wavelength of 780 nm as
the light source to give the results shown in Table
20B.
~5
Example lOB
The surface of the cylinder applied with
-- 109 --
I mirror surface working was applied with the so called
surface dimple formation treatment in which it was
subsequently exposed to falling of a large number of
balls for bearing to form numberless hitted marks on
the cylinder surface, to prepare a plural number of
cylinders having a cross section shape as shown in
Fig. 36 and various cross-section patterns as shown
in Table 21B. Said cylinder was successively set in
the preparation device shown in Fig. 33 and subjected
to drum preparation under the preparation conditions
similarly as in Example lB. The drum prepared was
evaluated variously by means of an electrophoto-
graphic device of a digital exposure function with
the use of a semiconductor laser having a wavelength
1~ of 780 nm as the light source to give the results
as shown in Table 22B.
Example lC
By use of the preparation device shown in
Fig. 33, a light-receiving member for electrophoto-
graphy was formed on an aluminum cylinder applied
with mirror surface working following the prepar-
ation conditions in Table lC. The light-receiving
member (hereinafter expressed as drum) was set on
an electrophotographic device, and, under various
conditions, electrophotographic characteristics such
as initial charging ability, residual potential,
~3~
-- 110 --
1 ghost, etc., were checked, and also lowering in
charging ability, sensitivity deterioration and
increase of image defects after successive copying
for l,500,000 sheets were examined. Further, the
image flow of the drum in an atmosphere of high
temperature and high humidity of 35C and 85 ~ was
also evaluated. And, the drum completed of evaluation
was cut out at the portions corresponding to the
upper, middle and lower portions of the image portion
to prepare samples, which were provided for quantita-
tive analysis of hydrogen contained in the surface
layer by util zation of SIMS. The above evaluation
results and the maximum value of the hydrogen content
in the surface layer are shown in Table 2C. As shown
in Table 2C, remarkable superiority was observed in
the respective items particularly of initial charging
ability, image flow, residual potential, ghost and
photosensitive irregularity in the axial direction,
sensitivity deterioration.
Comparative example lC
Except for changing the preparation conditions
as shown in Table 3C, the drum and samples for analy-
sis were prepared by the same device and method as
in Example l and provided for the same evaluation and
analysis. The results are shown in Table 4C.
As can be seen from Table 4C, it was recogni-
~3~
-- 111 --
I zed that the respective items were inferior as
compared with Example lC.
Example 2
By use of the preparation device shown in
Fig. 33, a light-receiving member for electrophoto-
graphy was formed on an aluminum cylinder applied
with mirror surface working following the preparation
conditions in Table 5C. The light-receiving member
1~ ~hereinafter expressed as drum) was set on an electro-
photogxaphic device, and, under various conditions,
electrophotographic characteristics such as initial
charging ability, residual potential, ghost, etc.,
were checked, and also lowering in charging ability,
sensitivity deterioration and increase of image
defests after successive copying for l,500,000 sheets
in a real machinç were examined~ Further, the image
flow of the drum in an atmosphere of high temperature
and high humidity of 35~C and 85 % was also evaluated.
And, the drum completed of evaluation was cut
out at the portions corresponding to the upper, middle
and lower portions of the image portion to prepare
samples, which were provided for quantitative analysis
of hydrogen contained in the surface layer by utili-
zation of SIMS, and also the component pxofiles in
the layer direction of silicon atoms (Si), carbon
atoms (C) and hydrogen atoms (H) in the surface layer
~3~
- 112 -
I were examined. Further, the component profiles o~
boron (s) and oxygen (o) in the charge injection
preventive layer were examined. The above evaluation
results and the maximum value of the hydrogen content
5 in the surface layer are shown in Table 6C. Also,
the component profiles of said elements in the above
surface layer are shown in Fig. 37, and further the
component profiles of said elements in the above
charge injection preventive layer are shown in Fig.
42. As shown in Table 6C, remarkable superiority
was observed in the respective items particularly
of initial charging ability, image flow, residual
potential, ghost and photosensitive irregularity in
the axial direction, sensitivity deterioration.
Example 3C, Comparative example 2C
The preparation conditions of the surface
layer were changed variously as shown in Table 7C,
~ith other conditions being the same as in Example
lC, to prepare a plural number of drums and samples
for analysis. These drums and samples were evaluated
and analy~ed similarly as in Example lC to obtain
the results as shown in Table 8C.
?5 Example 4C
The preparation conditions of the photo-
conductive layer were changed variously as shown in
~3~
- 113 -
l Table 9C, with other conditions being the same as
in Example lC, to prepare a plural number of drums.
Tnese drums were evaluated similarly as in Example lC
to obtain the results as shown in Table lOC.
Example 5C
The preparation conditions of the charge
injection preventive layer were changed variously as
shown in Table llC, with other conditions being the
same as in Example lC, to prepare a plural number
of drums. These drums were evaluated similarly as
in Example lC to obtain the results as shown in
Table 12C.
Example 6
The preparation conditions of the charge
injection preventive layer were changed variously
as shown in Table 13C, with other conditions being
the same as in Example lC, to prepare a plural number
of drums. These drums were evaluated similarly as
in Example lC to obtain the results as shown in
Table 14C.
Example 7C
A cylinder applied with mirror surface
working was further subjected to lathe working with
sword bit having various angles to prepare a plural
- 114 -
number of cylinders having a cross-sec~ional shape
as shown in Fig. 35 and various cross-sectional
patterns as shown in Table 15C. Said cylinder was
successively set in the preparation device shown in
Fig. 33 and subjected to drum preparation under the
preparation eonditions similarly as in Example lC.
The drum prepared was evaluated variously by means
of an elect~ophotographic device of a digital
exposure function with the use of a semieonduetor
laser having a wavelength of 780 nm as the light
souree to give the results shown in Table 16C.
Example 8
The surface of the eylinder applied with
mirror surface working was applied with the so called
surfaee dimple formation treatment in which it was
subsequently exposed to falling of a large number of
balls for bearing to form numberless hitted marks
on the eylinder surfaee, to prepare a plural number
of eylinders having a eross-seetion shape as shown
in Fig. 36 and various eross-seetion patterns as
shown in Table 17C. Said cylinder was sueeessively
set in the preparation deviee shown in Fig. 33 and
subjeeted to drum preparation under the preparation
~5 conditions similarly as in Example lC. The drum
prepared was evaluated variously by means of an
eleetrophotographic deviee of a digital exposure
~3~
- 115 -
function with the use of a semiconductor laser having
a wavelength of 780 nm as the light source to give
the results as shown in Table 18C.
Example lD
By use of the preparation device shown in
Fig. 24, a light-receiving member for electrophoto-
graphy was formed on an aluminum cylinder applied
with mirror surface working following the preparation
conditions in Table lD~ The light-receiving
member thereinafter expressed as drum) was set on
an electrophotographic device of a digital exposure
function with a semiconductor laser having a wave-
length of 780 nm as the light source, and, under
various conditions, electrophotographic character-
istics such as initial charging ability, residual
potential, ghost, etc., were checked, and also
lowering in charging ability, sensitivity deterio-
ration and increase of image defects after successive
copying for 1,500,000 sheets in a real machine were
examined. Further, the image flow of the drum in an
atmosphere of high temperature and high humidity of
35C and 85 % was also evaluated. And, the drum
completed of evaluation was cut out at the portions
corresponding to the upper, middle and lower portions
of the image portion to prepare samples, which were
provided for quantitative analysis of hydrogen
~3~ 9
- 116 -
1 contained in the surface layer by utilization of
SIMS. The above evaluation results and the maximum
value of the hydrogen content in the surface layer
are shown in Table 2D. As shown in Table 2D, remark-
able superiority was observed in the respective itemsparticularly of initial charging ability, image flow,
residual potential, ~host and photosensitive irregu-
larity in the axial direction, sénsitivity deterio-
ration.
Comparative example lD
Except for changing the preparation conditions
as shown in Table 3D, the drum and samples for
analysis were prepared by the same device and method
as in Example lD and provided for the same evaluation
and analysis. The results are shown in Table 4D.
As can be~ seen from Table 4D, it was recog-
nized that the respective items were inferior as
compared with Example lD.
Example 2D
By use of the preparation device shown in
Fig. 33, a light-receiving member for electrophoto-
graphy was formed on an aluminum cylinder applied
with mirror surface working following the prepar-
ation conditions in Table 5D. The light-receiving
member (hereinafter expressed as drum) was set on an
~L3~
- 117 -
1 electrophotographic device of a digital exposure
function with a semiconductor laser having a wavelength
of 780 nm as the light source, and, under various
conditions, electrophotographic characteristics such
as initial charging ability, residual potential,
ghost, etc., were checked, and also lowering in
charging ability, sensitivity deterioration and
increase of image defects after successive copying
for 1,500,000 sheets in a real machine were examined.
1~ Further, the image flow of the drum in an atmosphere
of high temperature and high humidity of 35C and
85 ~ was also evaluated. And, the drum completed
of evaluation was cut out at the portions correspond-
ing to the upper, middle and lower portions of the
1~ image portion to prepare samples, which were provided
for quantitative analysis of hydrogen contained in
the surface layer by utilization of SIMS, and also
the component profiles in the layer direction of
silicon atoms (Si), carbon atoms (C) and hydrogen
2~ atoms (H) in the surface layer were examined.
Further, the component profiles of boron (B) and
oxygen ~O) in the charge injection preventive layer
and the component of germanium (Ge) in the layer
thickness direction in the longer wavelength
absorbing layer were examined. The above evaluation
results and the maximum value of the hydrogen content
in the surface layer are shown in Table 6D. Also,
- 118
1 the component profiles of said elements in the above
surface layer are shown in Fig. 37, and further the
component profiles of said elements in the above
charge injection preventive layer and the component
profile of said element in the longer wavelength
absorbing layer are shown in Fig. 39. As shown in
Table 6D, remarkable superiority was observed in the
respective items particularly of initial charging
ability, image flow, residual potential, ghost and
photosensitive irregularity in the axial direction,
sensitivity deterioration and increase of image
defects as well as interference fringe.
Example 3D, Comparative example 2D
The preparation conditions of the surface
layer were changed variously as shown in Table 7D,
with other conditions being the same as in Example
lD, to prepare a plural number of drums and samples
for analysis. These drums and samples were evaluated
and analyzed similarly as in Example lD to obtain
the results as shown in Table 8D.
Example 4D
The preparation conditions of the photo~
conductive layer were changed variously as shown in
Table 9D, with other conditions being the same as in
Example lD, to prepare a plural number of drums.
-- 119 --
These drums were evaluated similarly as in Example
lD to obtain the results as shown in Table lOD.
Example 5
The preparation conditions of the charge
injection preventive layer were changed variously
as shown in Table llD, with other conditions being
the same as in Example lD, to prepare a plural
number of drums. These drums were evaluated similarly
as in Example lD to obtain the results as shown in
Table 12D.
Example 6D
The preparation conditions of the charge
injection preventive layer were changed variously
as shown in Table 13D, with other conditions being
the same as in Example lD, to prepare a plural
number of drums. These drums were evaluated similar-
ly as in Example lD to obtain the results as shown
in Table 14D.
Example 7
The preparation conditions of the longer
wavelength absorbing layer were changed variously
~5 as shown in Table 15D, with other conditions being
the same as in Example lD, to prepare a plural
number of drums. These drums were evaluated similar-
~3i~
- 120 -
ly as in Example lD to obtain the results as shown
in Table 16D.
Example 8
The preparation conditions of the longer
wavelength absorbing layer were changed variously as
shown in Table 17D, with other conditions being the
same as in Example lD, to prepare a plural number
of drums. These drums were evaluated similarly as
in Example lD to obtain the results as shown in
Table 18D.
Example 9D
A cylinder applied with mirror surface
1~ working was further subjected to lathe working with
sword bit having various angles to prepare a plural
number of cylinders having a cross-sectional shape
as shown in Fig. 29D and various cross-sectional
patterns as shown in Table l9D. Said cylinder was
~0 successively set in the preparation device shown in
Fig~ 33 and subjected to d~-um preparation under the
preparation conditions similarly as in Example lD.
The drum prepared was evaluated variously by means
of an electrophotographic device of a digital e~-
posure function with the use of a semiconductor
laser having a wavelength of 780 nm as the light
source to give the results shown in Table 2OD.
~3~6~
- 121 ~
I Example 10
The sur~ace of the cylinder applied with
mirror surface working was applied with the so called
surface dimple formation treatment in which it was
subsequently exposed to falling of a large number
of balls for bearing to form numberless hitted marks
on the cylinder surface, to prepare a plural number
of cylinders having a cross-section shape as shown
in Fig. 36 and various cross-section patterns as
shown in Ta~le 21D. Said cylinder was successively
set in the preparation device shown in Fig. 33 and
subjected to drum preparation under the preparation
conditions similarly as in Example lD. The drum
prepared was evaluated variously by means of an
electrophotographic device of a digital exposure
function with the use of a semiconductor laser having
a wavelength of 780 nm as the light source to give
the results as shown in Table 22D.
Example lE
By use of the preparation device shown in
Fig. 33, a light-receiving member for electrophoto-
graphy was formed on an aluminum cylinder applied
with mirror surface working following the prepa-
ration conditions in Table lE. Also, by use of adevice of the same model as shown in Fig. 33,
samples for analysis having only the charge injection
~3@1~9Lg
- 122 -
1 preventive layer and only the longer wavelength
absorbing layer on the cylinder with the same specifi-
cation, respectively, were prepared separately. The
light-receiving member (hereinafter expressed as
drum) was set on an electrophotographic device of a
digital exposure function with a semiconductor laser
having a wavelength of 780 nm as the light source,
and, under various conditions, electrophotographic
characteristics such as initial charging ability,
residual potential, ghost~ etc., were checked, and
also lowering in charging ability, sensitivity
deterioration and increase of image defects after
successive copying for 1,500,000 sheets in a real
machine were examined. Further, the image flow of
the drum in an atmosphere of high temperature and
high humidity of 35C and 85 ~ was also evaluated.
And, the drum completed of evaluation was cut out
at the portions corresponding to the upper, middle
and lower portions of the image portion to prepare
samples, which were provided for quantitative
analysis of hydrogen contained in the surface layer
by utilization of SIMS. On the other hand, the
sample having only the charge injection preventive
layer and the sample having only the lon~er wave-
length absorbing layer were cut out in the same
manner, and then diffraction patterns corresponding
to Si (111) around the diffraction angle 27 were
- 123 -
determined by use of a X-ray diffraction device for
examination of presence or absence of crystallinity.
The above evaluation results and the maximum value
of the hydrogen content in the surface layer, and
further presence or absence of crystallinity of the
charge injection preventive layer and the longer
wavelength absorbing layer are comprehensively shown
in Table 2E. As shown in Table 2E, remarkable
superiority was observed in the respective items
particularly of initial charging ability, image flow,
residual potential, ghost, image defects and photo-
sensitive irregularity in the axial direction~
sensitivity deterioration.
Comparative example 1
Except for changing the preparation con-
ditions as shown~in Table 3E, the drum and samples
for analysis were prepared by the same device and
method as in Example lE and provided for the same
evaluation and analysis. The results are shown in
Table 4E.
As can be seen from Table ~E, it was
recognized that the respective items were inferior
as compared with Example lE.
Example 2E
By use of the preparation device shown in
~3~fi~
- 124 -
I Fig. 33, a light-receiving member for electrophoto-
graphy was formed on an aluminum cylinder applied
with mirror surface working following the preparation
conditions in Table 5E. Also, by use of a device
of the same model as shown in Fig. 33, samples for
analysis having only the charge injection preventive
layer and only the longer wavelength absorbing
layer on the cylinder with the same specification,
respectively, were prepared separately. The light-
receiving member (hereinafter expressed as drum)was set on an electrophotographic device of a digital
e~posure function with a semiconductor laser having
a wavelength of 780 nm as the light source, and,
under various conditions, electrophotographic charac-
teristics such as initial charging ability, residualpotential, ghost, etc., were checked, and also
lowering in charging ability, sensitivity deterio-
ration and increase of image defects after successive
copying for l,S00,000 sheets in a real machine were
examined. Further, the image flow of the drum in
an atmosphere of high temperature and high humidity
of 35C and 85 % was also evaluated. And, the drum
completed of evaluation was cut out at the portion
corresponding to the upper, middle and lower portions
of the image portion to prepare samples, which were
provided for quantitative analysis of hydrogen
contained in the surface layer by utilization of
~L3~
- 125 -
1 SIMS, and also -the component profiles in the layer
direction of silicon atoms (Si), carbon atoms (C)
and hydrogen atoms (H) in the surface layer were
examined. Further, the component profiles of boron
(B) and oxygen (O) in the charge injection preventive
layer and the component of germanium (Ge) in the
layer thickness direction in the longer wavelength
absorbing layer were examined. On the other hand,
the sample having only the charge injection preventive
layer ànd the sample having only the longer wave-
length photosensitive layer were cut out in the same
manner, and then diffraction patterns corresp~nding
to Si (lll) around the diffraction angle 27 were
determined by use of a X-ray diffraction device for
examination of presence or absence of crystallinity.
The above evaluation results and the maximum value of
the hydrogen content in the surface layer, and
further presence or absence of crystallinity of the
charge injection preventive layer and the longer
wavelength absorbing layer are comprehensively
shown in Table 6E. Further, the component profiles
of said elements in the above surface layer are
shown in Fig. 37 and the component profiles of said
element in the above charge injection preventive
~5 layer and the component prorile of said element in
the longer wavelength photosensitive layer are shown
in Fig. 40.
~3~
- 126 -
1 As shown in Table 6E, remarkahle superiority
was observed in various and many items particularly
of initial charging ability, image flow, residual
potential, ghost, image defects and photosensitive
irregularity in the axial direction, sensitivity
deterioration and increase of image defects as well
as interference fringe.
Example 3E, Comparative example 2E
The preparation conditions of the surface
layer were changed variously as shown in Table 7E,
with other conditions being the same as in Example
lE, to prepare a plural number of drums, which were
provided for the same evaluation. And, the drums
completed of evaluation were cut out into samples
and subjected to the same analysis. The above
results are shown in Table 8E.
Example 4E
The preparation conditions of the photo-
conductive layer were changed to several conditions
as shown in Table 9E, with other conditions being
the same as in Example lE, to prepare a plural
number of drums. These drums were evaluated similar-
ly as in Example lE to obtain the results as shown
in Table lOE.
- 127 -
1 Example 5E
The preparation conditions of the charge
injection preventive layer were changed to several
conditions as shown in Table llE, with other
conditions being the same as in Example lE, to
prepare a plural number of drums and samples having
only the chaxge injection preventive layer formed.
These drums and samples for analysis were subjected
to evaluation and analysis as in Example lE to obtain
the results as shown in Table 12E.
Example 6E
The preparation conditions of the charge
injection preventive layer were changed to several
conditions as shcwn in Table 13E, with other con-
ditions being the same as in Example lE, to prepare
a plural number of drums and samples having only the
charge injection preventive layer formed. These
drums and samples for analysis were subjected to
evaluation and analysis as in Example lE to obtain
the results as shown in Table 14E.
Example 7E
The preparation conditions of the longer
wavelength absorbing layer were changed to several
conditions as shown in Table 15E, with other con-
ditions being the same as in Example lE, to prepare
~3~6~
- 128 -
I a plural number of drums and samples for analysis
having only longer wavelength photosensitive layer
formed. The drum was subjected to the same evalu-
ation as in Example lE, while a part of the sample
S was cut out and the diffraction pattern corresponding
to Si (111) around the diffraction angle 27 was
determined for examination of presence or absence of
crystallinity. The above results are shown in
Table 16E.
Example 8
The preparation conditions of the longer
wavelength absorbing layer were changed to several
conditions as shown in Table 17EI with other con-
ditions being the same as in Example lE, to preparea plural number of drums and samples for analysis
having only longer wavelength absorbing layer formed.
The drum was subjected to the same evaluation as in
Example lE, while a part of the sample was cut out
and the diffraction pattern corresponding to Si
~111) around the diffraction angle 27~ was determined
~or examination of presence or absence of crystal-
linity. The above results are shown in Table 18E.
~5 E~ample 9E
The preparation conditions of the longer
wavelength absorbing layer were changed to several
- 129 -
1 conditions as shown in Table l9E, with other con-
ditions being the same as in Example lE, to prepare
a plural number of drums and samples for analysis
having only longer wavelength absorbing layer formed.
The drum was subjected to the same evaluation as in
Example 1, while a part of the sample was cut out and
the diffraction pattern corresponding to Si (111)
around the diffraction angle 27 was determined for
examination of presence or absence of crystallinity.
The above results are shown in Table 20E.
Example 10
The preparation conditions of the longer
wavelength absorbing layer were changed to several
lS conditions as shown in Table 21E, with other con-
ditions being the same as in Example lE, to prepare
a plural number of drums and samples for analysis
having only longer wavelength absorbing layer formed.
The drum was subjected to the same evaluation as in
Example lE, while a part of the sample was cut out
and the diffraction pattern corresponding to Si (111)
around the diffraction angle 27 was determined for
examination of presence or absence of crystallinity.
The above results are shown in Table 22E.
Example 11
On a substrate cylinder, an adhesion layer
~3~
- 130 -
1 was formed under several preparation condi-tions as
indicated in Table 23E, and further a light-receiving
member was formed under the same preparation conditions
as in Example lE. Separately r samples having only
adhesion layers formed were prepared. The light-
receiving member was subjected to the same evaluation
as in Example lE, while a part of the sample was cut
out and the diffraction pattern corresponding to
Si (lll) around the diffraction angle 27 was de-
l~ termined for examination of presence or absence ofcrystallinity. The above results are shown in Table
24E.
Example 12E
On a substrate cylinder, an adhesion layer
was formed under several preparation conditions as
indicated in Table 25E, and further a light-
receiving member was formed under the same prepa-
ration conditions as in Example E. Separately,
samples having only adhesion layers formed were
prepared. The light-receiving member was subjected
to the same evaluation as in Example lE, while a
part of the sample was cut out and the diffraction
pattern corresponding to Si (lll) around the
diffraction angle 27 was determined for examination
of presence or absence of crystallinity. The above
results are shown in Table 26E.
~3~
- 131 -
I Example 13E
A cylinder applied with mirror surface work-
ing was further subjected to lathe working with
sword bit having various angles to prepare a plural
number of cylinders having a cross-sectional shape
as shown in Fig. 35 and various cross-sectional
patterns as shown in Table 27E. Said cylinder was
successively set in the preparation device shown in
Fig. 33 and subjected to drum preparation under the
preparation conditions similarly as in Example lE.
The drum prepared was evaluated variously by means
of an electrophotographic device of a digital ex-
posure function with the use of a semiconductor
laser having a wavelength of 780 nm as the light
source to give the results shown in Table 2~E.
Example 14
The surface of the cylinder applied with
mirror surface working was applied with the so
called surface dimple formation treatment in which
it was subsequently exposed to falling of a large
number of balls for bearing to form numberless hitted
marks on the cylinder surface, to prepare a plural
number of cylinders having a cross-section shape as
shown in Fig. 36 and various cross-section pat~erns
as shown in Table 29E. Said cylinder was successive-
ly set in the preparation device shown in Fiy. 33
~L31~L6~
- 132 -
and sub~ected to drum preparation under the prepa-
ration conditions similarly as in Example lE. The
drum prepared was evaluated variously by means of an
electrophotographic device of a digital exposure
S function with the use of a semiconductor laser
having a wavelength of 780 nm as the light source
to give the results as shown in Table 30E.
Example lF
By use of the preparation device shown in
Fig. 33, a light receiving member for electrophoto-
graphy was formed on an aluminum cylinder applied
with mirror surface working following the prepa-
ration conditions in Table lF. The light-receiving
lS member (hereinafter expressed as drum) was set on an
electrophotographic device, and, under various
conditions, electrophotographic characteristics such
as initial charging ability, residual potential,
ghost, etc., were checked, and also lowering in
charging ability, sensitivity deterioration and
increase of image defects after successive copying
for 1,500,000 sheets in as real machine were examined.
Further, the image flow of the drum in an atmosphere
o~ high temperature and high humidity of 35C and
5 ~ was also evaluated. And, the drum completed
of evaluation was cut out at the portions correspond-
ing to the upper, middle and lower portions of the
13~46i~
- 133 -
image portion to prepare samples, which were provided
for quantitative analysis of hydrogen contained in
the surface layer by utilization of SIMS. The above
evaluation results, the maximum value of the hydrogen
content in the surface layer are shown in Table 2F.
As shown in Table 2F, remarkable superiority was
observed in the respective items particularly of
initial charging ability, image flow, residual
potential, ghost, image defects and photosensitive
irregularity in the axial direction, sensitivity
deterioration.
Comparative example lF
Except for changing the preparation conditions
as shown in Table 3F, the drum and samples for
analysis were prepared by the same device and method
as in Example lF and provided for the same evaluation
and analysis. The results are shown in Table 4.
As can be seen from Table 4F, it was recog-
nized that the respective items were inferior as
com~ared with Example lF.
Example 2F
By use of the preparation device shown in
Fig. 33, a light-receiving member for electrophoto-
graphy was formed on an aluminum cylinder applied
with mirror surface working following the preparation
:~L3a~6~
- 134 -
1 conditions in Table 5F. The light-receiving
member (hereinafter expressed as drum) was set on
an electrophoto~raphic device, and, under various
conditions, electrophotographic characteristics such
as initial charging ability, residual potential,
ghost, etc., were checked, and also lowering in
charging ability, sensitivity deterioration and
increase of image defects after successive copying
for 1,500,000 sheets in a real machine were examined.
Further, the image flow of the drum in an atmosphere
of high temperature and high humidity of 35C and
85 ~ was also evaluated. And, the drum completed
of evaluation was cut out at the portions correspond-
ing to the upper, middle and lower portions of the
image portion to prepare samples, which were provided
for quantitative analysis of hydrogen contained in
the surface layer by utilization of SIMS, and also
the component profiles in the layer direction of
silicon atoms (Si), carbon atoms (C) and hydrogen
atoms (H) in the surface layer were examined.
Further, the component profiles of boron (B) and
oxygen (O) in the charge injection preventive layer
and the component profile of germanium (Ge) in the
layer thickness direction in the longer wavelength
absorbing layer were examined. The above evaluation
results and the maximum value of the hydrogen
content in the surface layer are shown in Table 6F,
~3~
- 135 -
I the component profiles of said elements in the above
surface layer in Fig. 37 t and the component profile
of said elements in the charge injection preventive
layer and the component profile of said element in
the longer wavelength photosensitive layer in Fig.
41. As shown in Table 6F, remarkable superiority
was observed in the respective items particularly of
initial charging ability, image flow, residual
potential, ghost, increase of image defects and
photosensitive irregularity in the generator di-
rection, sensitivity deterioration and increase of
image defects, as well as interference fringe
Example 3F, Comparative example 2F
The preparation conditions of the surface
layer were changed variously as shown in Table 7F,
with other conditions being the same as in Example
lF, to prepare a plural number of drums and samples
for analysis. These drums and samples were subjected
to the same evaluation and analysis as in Example lF
to obtain the results as shown in Table 8F.
Example 4
The preparation conditions of the photo-
conductive layer were changed to several conditions
as shown in Table 9F, with other conditions being
the same as in Example lF, to prepare a plural
~3~
- 136 -
number of drums. These drums were evaluated similarly
as in Example lF to obtain the results as shown in
Table lOF.
Example 5F
The preparation conditions of the charge
injection preventive layer were changed to several
conditions as shown in Table llF, with other con-
ditions being the same as in Example lF, to prepare
a plural numbex of drums. These drums were subjected
to the same evaluation similarly as in Example lF toobtain the results as shown in Table 12F.
Example 6F
1~ The preparation conditions of the charge
injection preventive layer were changed to several
conditions as shown in Table 13F, with other con-
ditions being the same as in Example lF, to prepare
a plural number of drums. These drums were subjected
~O to the same evaluation similarly as in Example lF
to obtain the results as shown in Table 14F.
Example 7F
The preparation conditions of the longer
wavelength absorbing layer were changed to several
conditions as shown in Table 15F, with other con-
ditions being the same as in Example lF, to prepare
~3~
- 137 -
I a plural number of drums. These drums were subjected
to the same evaluation similarly as in Example lF to
obtain the results as shown in Table 16F.
5 Example 8F
The preparation conditions of the longer
wavelength photosensitive layer were changed to
several conditions as shown in Table 17F, with other
conditions being the same as in Example lF, to
prepare a plural number of drums. These drums were
subjected to the same evaluation similarly as in
Example lF to obtain the results as shown in Table
18F.
Example 9F
On a substrate cylinder, an adhesion layer
was formed under several preparation conditions as
indicated in Table l9F, and further a light-
receiving member was formed under the same prepa-
?O ration conditions as in Example lF. These light-
receiving members were subjected to the same
evaluation as in Example lF to obtain the results
as shown in Table 20F.
Example 10F
A cylinder applied with mirror surface
working was further subjected to lathe working with
- 13~ -
1 sword bit having various angles to prepare a plural
number of cylinders having a cross-sectional shape
as shown in Fig. 35 and various cross-sectional
patterns as shown in Table 21F. Said cylinder was
successively set in the preparation device shown in
Fig. 33 and subjected to drum preparation under the
preparation conditions similarly as in Example lF.
The drum prepared was evaluated variously by means
of an electrophotographic device of a digital ex-
posure function with the use of a semiconductorlaser having a wavelength of 780 nm as the light
source to give the results shown in Table 22F.
Example llF
1~ The surface of the cylinder applied with
mirror surface working was applied with the so called
surface dimple formation treatment in which it was
subsequently exposed to falling of a large number
of balls for bearing to form numbeLless hitted
o marks on the cylinder surface, to prepare a plural
number of cylinders having a cross-section shape as
shown in Fig. 36 and various cross-section patterns
as shown in Table 23F. Said cylinder was successive-
1~ set in the preparation device shown in Fig. 33
and subjected to drum preparation under the prepa-
ration conditions similarly as in Example lF. The
drum prepared was evaluated variously by means of
- 139 -
I an electrophotographic device of a digital exposure
function with the use of a semiconductor laser
having a wavelength of 780 nm as the light source to
give the results as shown in Table 24F.
~3~
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-- 145 --
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-- 146 --
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- 147 -
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- 148 -
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-- 149 --
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- 150 -
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-- 151 --
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- 152 _ ~L30~ g
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.,
18~
Table 2D
Initial
charging O
ability
s ens it iv i t y O
S
Image flow
Interference
fringe O
_
Residual
potential
_
Ghost O
. _ .
Photosensitivity
irregularity
in generator
direction
... _ .
Image defect O
_ ,_
Sensitivity`
deterioration O
. ._ . .
Increase of O
image defect
._
Maximum value
of hydrogen 52
content (atomic %
1~7
. . ~ ~
10 3 ~ ~ o o
~ Q. ,1 ~ ~ o
tY7 _
h h
~0 E O In o o o
15 O a)
.. ._,~
oE o o o
o o ~,0 0 Q o o E o o t 1 1`
raIn o Q~ m ul In o ~:4,J m In In
~: ^ ~1 ~1 ~ ~ ~ ~ r7 r~ O O o
0 ~ _ _ m m
E ~ o o
h ~ ~:1
0 ~ ~
~r ~D ~ ~ ~ ~r ~r
~ C X ~ C :}:
.~ ~ O ~ ~ ~ ~ O ~ rl r~ .,
cq al z ~ ~ u~ m Z 2 u~ u~
.._
~ ~ 0~ ~
oh u ,D O ~ ~ U
o oa) ~I h h tJI U a) h O ~ h 0 h
E ~1 ~n a) O O h O ~ o ~ ~ a)
0 0~ ~ 0~n o ~ O ~ :~ h :~
æ ~o 0 ~ 0 ~ ~ h 0 ~ O ) ::~ 0
3 a-I ~ ~4 V
_ _
1~
Table 4D
Initial _
charging x
ability
Initial
sensitivity O
S __
Image flow O
Interference O
fringe
.
Residual
potential X
Ghost
__
Photosensitivity
irregularity
in generator
direction
_
Image X
defect
, _ .
Sensitivity O
deterioration .
_ _ _
Increase of
image defect X
__ _ _ _
Maximum value
of hydrogen 87
content(atomic%)
2~
i 8 !~ ~3~4~
~ _~ - T
~ o ~ o
,~
_
~ ~r
h I~ ~ o
s~ ~ ~ ~ ~ ~r
~ a~ o O O O er
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H R~--
_ _
_ O
3 u~ u~ o ~1
~ ~ ~ ~ o
a ~ ~
U~ _ . . . .. _
,1 ~ h
0 1~
E~h ~ o o o o
~ ~ u~ U7 Lr) Ul
Q ~ ~) ~I ~`I ~ ~J
~ a~o
. _
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o ~ ,1~ o o o
o o o o c3 O O o
u~n ~ u~ u~ u~ ~ ~ ~
~^ ~^~7 ,~_ ~ r~ ~ o o o
a :~ :c~ ~:, u~ u~
U~ U~
O ~
~ O O
Q~3 a) O
0 ~ ~ r ~ ~D ~ ~r
C ~ :1
.rl ~ O ~ ~ .r~ ~ O ~ r1 ~ .,~
v~ m z ~ ~: u~ a: z :c u~ ~c u~
.. _
O .
O ~.,1 ,1
h h C).D o ~ s:: I t~ ~
a) a) a) ~I h h tll O O h O ::1 h 0 h
E~ :>1 to a) o ~ h a) ~ ~J ~ ~ O 4
~ (a c~ q ~ (a r-~ o ~ O C~ ~ h
z ~1 o ,a ,Q la 1: ~ h 11~ .C O la ~1 ,a
~1 3 ~1 t)~rl R,~l ~ l ~
. __ . _ _ .. .
1 ~B 13046~l9
Table 6
____ _~ .
Initial
charging
abilitv
_ __
Initial O
sensitivity
~ ..
Image flow O
. . _
Interference
fringe
._. .. ~
Residual
potential
_ _ ._
Ghost O
_ . _ - --1
Photosensitivity
irregularity
in generator
direction
Image defect O
.. . .__ _
Sensitivity
deterioration O
.. ._ ._ .,
Increase of
image defect O
. _ _ _
Maximum value
of hydrogen 46
content(atomic~)
_
: .~
,.~, ~ ,
3q:346~
oo
O O O O ~D Il-
~r ~ ~ r o o o
o o o o
~ ~ o o
a
O ~ ~ o ~
5 ~ O O O o
u~ ~ o
O O
O O O
3 ~ ~ o In
~ o o o o
a ~ O ~ o u.
3~ ~r o ~r
~1 $ ~ O O
. _
O O O
a ~ O O u~
u~ u~ O ~r In
rD :~ ~r ~ o o
o .,~ $ ~
E~ _
o O o
o o O
u~ u~
a O O o u.
,,
~ oo
v~ u ~ _ ~ O
o O _ ~ -
~u~
O O o o
~ O o u~
~ ~ o ~ o~ u~
a
.,~ ~ ~ O
. u~ ~ o '.~
a~
. ~ ~ _ ~q
O ~ ~ 3 rD rn
z ,a ~ _ ~
3 0 :~: h h ~ h n ~ ,Y
~ o ~ ~J ~n ~^ ~ ~ n
::~ ~I rd U~ E~ U3 C: ~ O ~1 rl
~ IL~ ~ aJ~4 0 ~ ~ ~ rl,~
a _ c~ ~ _~ Q. H Q,~ ~4 ~ _
;_ _
1'32 ~
_ _ -
a) o o
~ ~ ~ u~ a:) L~
~ o~ o 3 o ~
I`~ a) o o o n
~ ~ ~ o ~
a~ ~ ~r In ~ ~
RE~ la ~ ~r o r~
~O X ~1 X ~ o
E~C~ O V~ , (~ O
_ _
~ O 0 ~D
~ ~ o ~r u.
a ~ ~ I o ~ ~ ~ J
~ ~ o
V~O~ r~ O
o o
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O oOO O O ~ In
~ ~x~ ~ o ~ ~
. ,~ ~ o o
_ _
~3~
l'able 8D
Drum No. D301D 3 0 2 D 3 0 3 D 3 0 4 D 3 0 5 D306 ~ ti ve
_~n _
Initial charging O O O O O O X
Initial _
sensitivity O O O O O O O
.. _ _
Image flow
O~ ~ ~> O ~ O
._
Interference
fringe O O O O O O O
_
Residual O O O O O O x
_ _
Ghost O ~ ~ O O O Q
__ ..
15 Photosensitivity
irregularity O O O O ~ O
in generator
direction
. _ ..
Image defect O O O O O O x
._ . _ .__ _
Sensitivity
deterioration O O O O O ~ O
.. ~_ .. _
Increase of
image defect O O O O O O X
. . . ._ . .. _ Compa=
D301 D302 D303 D304 D305 D306 eatmve
Sample No. -1 -1 -1 -1 -1 -12-lD
~ . __ _ . ~_ _
Maximum value of
hydrogen content 5l 60 62 63 70 5585
(atomic ~)
. _, _ _ _ _
1 ~ 0~
__ -oOooO~ _ .
`5:> ~ uo~ o o o
- u~u~ x
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a) ~ Lt~ o . o
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a ~ ~ o o o
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. .. _ ... . _
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h _ Q E~ U 3 ~ O O r~
a :: ~O ~ o ~ h ~ ~
.__ __ _. . Q~ . H Q~ _ ___
Ofl~
Table lOD
l Drum No.D40l D402 D4D3 D404 D405 D406
. __ _
abiIity O O O O O O
_
Initial ~ O O O O O
. _
Image flow O O O O O O
...
Interference
fringe O O O O O O
__
Resi.dual O O O O O O
.
Ghost O O O O ~
_ __ _ ,_
Photosensitivity
irregularity in O O O O O O
generator direction
,..._
Image defect~ O O O O O O
. _ .. . .
deter iorat ion ~ O O ~) O O
_ _
Increase of O O O O O O
image defect
2~
lt~
46~
o o o ~ o o __ _ ~ __ a
o ~ o o u~ r Z
.~ l Q ~o ~`J ~1 ~ o ~I E~
tn u~ O Z :I~ h
5 ~ o o Q, ~ o ~ ~ la
o ~ O o o ~ E
u~ m~ Q O ~ ~
_ , ~
00~ U~
o ~ 1: O O ~
~:, x~ x'5' ra "7 ~ ~ O ~ la
C~ ~ 1 D 1~ 0 h
~ u~ m o 2; ~:
~1 O O Q~ ~ O U
Q o u~ o a -` ~ o o O ~ a
_ I D o zO ~1 .C
o o ~ r) o _ .. _ 4~
L o ~, _ L~ Ln O
~ ~ o o ~ o
o u~ m Q o Z ~ ~ o ~ ~
O E o o _ _ _ o
O ~ " Q, - ~ L~O~ Lr~ L~ O
L -rl ~1 D ~ O~ t~l ~1 O ~7
m ~ o Z ~:: __. _ th
o~ ~ 3 ~ ~
ZO ~ O (a Id h h JJ
h~4 h u~ h h O h ol h ,~
a Q 6u~ ~ o ~rl e o
_ ._ ~ 0 ~~ ~ ~" a :l
~4~
I Tabl~ 12D
Drum No. D501 D502 D503 D504 D505 D506
Initial charging
ability O O O O O O
Initial O O O O O O
sensitivity _
Image flow O ~ O O 3 O
Interference
10 fringe O O O O O O
Residual O O O O O O
potentlal ~
Ghost O O O O O O
Photosensitivity
irregularity O O O O O O
in generator
direction
_
Image defect O O O O O O
Sensitivity
deterioration 63 O O O ('3
Increase of O O O O O O
image defect
Remark char
1"~
~3~1g
.~
----~ o oo, a ~ o _ _ _ ~_ a
a o o o~ o o o o o ,~ E
5 ~ O E a o O _ ~
L ~r~
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a a x ~ o ~ ~ ~ o
a) .. .
~ o~ o o~ o o o ~ a~
a ~ ~ ~ ~ o ~ o
~o 3~o ~ - -
~o ~ Z ~ o U~ o
o o~ ~ ~ o ~ _ _
~ ~ J ~t ~ ~
æ 3 a) ~ ~ ~ h o u~
::1 ~ 0 C~ h h 3 h u) ~ C ~1
h _ tn R- ^ Ql a) ol h 1~ 0 ^ ~:
a Q E~ O ~: ~1 0 ~ O
~ ~ o ~4 C: ~/ ~ ''I .~ ~L
_ _ _ ~ ~- ~, ~ ~ p, ~ h ~ _
1~.9
~L~30~19
Table 14D
__ _ ... _ .
Drum No. D601 D602 D603 D604 D605 D606
_
Initial charging
ability ~ O O O O O
Initial
sensitivity O O O O O O
..................... .__ ~
Image flow O O O O O O
Interference
fringe O O O O O
._ _ _ __
Residual
potential O O ~ O O
_ .. _ _
Ghost O O O O O O. ~ ._ ._ .
Photosensitivity
irregularity O O O O ~ O
in generator
direction
._ ~ _ ._ ..
Image defect O O O O O O
. _ _ ._ . .. _
deterioration O O O O O O
._ _ . _
Increase of
image defect ~ O O O O
Table 15D
r
U~ O p, O i~ Ln I_
10 a x~ x~ ~ O O O O
~ O a~ ~
I c~ Z~C l ~ _ . ,, I
~ o ~ o O
o I ~ o ~,o ~ u~ o o ~ ul
~ ~ ~, ~ .~ ~ N ~ O O
~ O O ~1
1~ ~q m -- z
o o ~,~ o o o
o ~noQ,O ~ o o r~ In
a ~r$~ ,O ~ ~ ~ o o
.D tn O a
l ~ cq m -- ~; ~ x
20 E 3 ~: a Ec~ 3 ~ Q~ h
~ ~ ~ o ~ h ~ .,~ ~ ~L a~
. _ ~ ~ ~ ~ ~ ~ I
~(Jl 130~6~L~
Table 15D '
~ ._ _
O OQ, C O O O
o o o o ~ n ~n
Ln o ~ o o r~
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o~ ~r ~ ~ .
X ~r o o
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rJ o
er
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P~ ~ ~ 0 ~ ~ ~
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-- ~ ~ u~
X :C 0 ~ $
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n m ~ z ~ ~
~304~
I Table 16D
_ ._ ___ __ . __I . _
Drum No. D701 D702 D703 D704 D-7io5 D7205 D706
ability _ _ O ~ O ~
Initial
sensitivity O O O O O O O
~ .. .
Image flow O ~ O O ~ O O
Interference
fringe O O O O O O
_. _ ._
Residual O ~ _ _ _ ~ ~
Ghost O O ~ O O O O
_ . __ . . . _ ._
Photosensitivity
irregularity O O O O O ~ O
in generator
direction
. _ ~ _ .
Image defect O O ~ O O O O
- ._ _ . ._
Sensitivity O O O O O O O
deterioratlon. _ _ _
image defect O O O O O O
13q~
Tab le 17 D
l o~cul~O __ _ ,
u~ O ~, o o ~ t-
o ~ O O ~ U~
Q ~ ~ x~ ~ ~ o o
~C ~ 0 rl 0 a
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O~c In~ o
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..
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` In In .
o a) ~r ~P ~ ~ o o
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a $ 3~ o au
u~ m~ ~ $
.. .
20 . ~, h ~ t~
æ 3 ~ S~ h _h ~7 Ll C
a ~ h V~ D ~3 U 3 C a) O ~ (.)--
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...._ .
1~0~6~
T~ble 1 7D '
--k - I --
o O oL2~ o 0 1` o
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a) ~ ~r ~) ~ .
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Table 18D
_ _ _ _ _ _ _ D805 D805
Drum No.D801 D802 D803 D804 -1 -2 D806
. _ ._
5 Initial charging ~ O O O O O
Initial
sensitivity O O O O O O O
.. _
Image flow O ~ O O ~ ~ O
lO Interference
f r lnge O (~ (~ O O (~) 1~)
Residual
potential O O O O O
.. __ . , .. _ _ _
Ghost O O O O O ~ O
_ _
15 Photosensitivity
irregularity O O O O O ~ O
in generator
direction ~
Image defect O O O O O O O
. ......... _ ._ . ... _.
20 Sensitivity
deterioration O O O O ~ O O
~ .. .. .. _
Increase of O O O O O O O
image defect _
_
a
a
~o~
I'able 20D
Drum No. D901 D902 D903 D904 D905
ability ~9 ~ ~9 O
Initial O O O A O
Image flow O {'9 C~9 O _ _
Interference
fFinge O (~ O ~) O
Residual O O O
potential
Ghost ~ O ~ O
Photosensitivity
irregularity O O O O
in generator
direction .
Image defect O O O O O
__
Sensitivity
deterioration ~9 O ~ ~ ~9
Increase of O O O O O
~ . . _ _
Resolving
power of image O O ~ O O
2 ~ 0fL~,g
15 . ~ _
__ _ a
~3~
1 'rable 22D
. . _ . _ .__
Drum No. DlOOl Dl002 Dl003 Dl004 Dl005
_ _ _ l -__
Initial charging
S ability ~ ~ ~ O
Initial _ _
sensitivity O O O O O
._ _
Image flow O ~ O ~
__ ..
Interference
fringe ~ ~ O O O
_ _
potential O O O ~
_ _ .
Ghost O O O O O
_
Photosensitivity
irregularity ~ O O O
in generator
direction
~ . _ _ ._
Image defect O O O O O
_ . . _ . .. ~
Sensitivity
deterioration O O O O O
._ _ .... _ ._
Increase of O O O O O
._ . _ ,
Resolving A~o A_O ~ O
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R ~ ~ (~) ~) ~) ~) ~) ,1 h .
Z _ _ ", _ _ R 3 _ __ d' Ln
25 ~ w w w w ~w 8 ~ ~w O ~w ~w w
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s ~ o ~ o ~ ;
pl- --- - ~ ~ o
3 1n In u~ o o
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O O ::~
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E~ S~ h o o o o o
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~ ~ ~ ~ ~
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OQ. o o o o o
o OQ~O O O O ~ O O O O O ~ O O O O ~ Lr~ In
In ~ ~ U~ U~ O Q,~ ~ O ~ O Q~ In U~ U~ ~ ~ ~
~_~ ~ ~ ~ ~ ~ ~ ~ oo o
-~1 ~:: :S r~
0~ U~
~1 ~ O O
~ ~ a
E~ ~ ~ Q a)
~q ~ ~, Q .-
O 3 ~ ~ _ ~
~O O X ~ d' ~ ~r ~r ~D ~ er
O ~`I X ~ ~: ~ ~C
u~ m Z Z .,~ ~, o ~ ~ ~1 ~ O ~ ,
u~ V :C tn m ~ ~ u, ~: u~
.. ~ . . .. ~__ _ .... _
~ O ~: ~ O rl ,~ a)
O -r~ ~ 1 O ~ C h I t~ 1)
a) a) h ~--~ o h h O ~ O ~ h (IJ h
0 la ~ ~ 1~ ~ ~: ~ h 1~ ~ O
Z~1 ~ 1 ~ l ~ 1 Ul~1
. ~ ..
~2 ~3~ 9
1 Table 2F
__ __ _ .
Initial
charging ~)
ability _ ~ --- Very yood
Initial O O --- Good
sensitivity
_ I ~--- Practically
acceptable
Image flow O
_ ~ Slightly poor
Interference in practical use
fringe O
Residual
potential
.
Ghost
Photosensitivity
irregularity
in generator
direction
__ ._
Image defect O
Sensitivity
deterioration
_
Increase of
image defect O
Maximum value
of hydrogen 52
content (atomic %)
.3
~IL3
r 1 0 ~ 1
S .__ .
h h t~l ~1 u~ ~ o
~ o o o o o o
H ~2~-- O
,_ _ .
h o
3 1n o o ~
1:4 r~
_
~1h
R~ ~ o o o o
~h 5~ ~ In u~ ~n O
E~ ~ ~ ~ ~ ~
15 ~ ~ ~ ~
o o'o
o ~oo oo ~oo o o o ~oo o o ~ U~O
o o ~ ~ u~ u~ o p~ n u7 o ~2, ~ ~~ In ~ .
u~ O Q. ~ ~ o ~, ~ ~ o Q, ~ ~ ~ O O
t~ ~ ~ ~ U~ o
C~ X 3: :I:
0~ U~ U~ U~
a~ o o o
Ei ~a 'C~ ~
u~ S~ O a) ~7)
0 ~1 D
~1 ~r ~ ~ r ~ ~> ~ ~
:I:X XX ~ X X X X ~r
rl r~ O t~l ~1 t~l O a) ~ ,~ t~l o t~l ~ . .,~ T t~l
u~ m æ 3:: u~ m z ~ x ~J~ m z x ." ~:: ." ~
~ tJl ~: O rl D
O tn h h tD ~ tV ~ C~ tD
htD tD tD ~I h h tJI t.) tD h O ::1 h 0 h
tV tD.t. ~1 to tD O tD h tD :~ tl) ~ ~ tD 4-1 tD
~a ~ ~ ~a~ v ~ o c :~ h
~a ra~ ,~ 0 ~a p ~a ~ ~ h ~a ~ o ~a ~ ra
æ,~ ~ 3 a,~ tJ~ l ~ 1 U~l
. ._ _ ___
34~ 9
1 Table 4F
Initial
charging x
abilitv
,
Initial O
sensitivity
__
Image Elow O
.~
Interference
fringe O
. _
Residual X
potential
._
Ghost
~_
Photosensitivity
irregularity
in generator
direction
_ _ _
Image defect X
_
Sensitivity
deterioration O
.
Increase of X
image defect
.. _
Maximum value
of hydrogen 87
cQntent (atomic %)
~ ~ 5 ~L30~ 9
... __ . _ ___ _ _
U~
n u~
~^ o o ~ o
_ ~_
5h ~ r~ L~ o
h ~n h t`l ~`1 ~`1 ~r
C: ~ ~ o o o o o
~^ _ o
h o o o o o
~ ~ ~o
a~
a) ~
h h o o o
E~ ~ ~ u~ u~ o In O
15 ~) ~`! ~1 ~1 r~l `J
__ .. _ . o o
o O ~ O O ~ O R~ O
u~ o ~ n u~ o ~,~ o ~r~ u~ 0 ~2~ ~ LO u~
~ ~^ ~ ~ ~ ~ ~ ~ u~ u~
20 ~ o 1:: o
~ ~ ,~ ,~ ,~
h ~ Q
7 4 1 ~ X~ ~ X~r 1
,~ ~I O ~ ~ I O ~ ~ ,~ ~I O ~ ,~
cn m æ x u~ m z ~7 ~: u~ m z X u~ X u~ C~
2540 h '~ tJ) ,~ ~ ~
~ ~ h r h h h O ~ O ~ '~1 a) 4~ O
z ~ ~ ~ o ta ~ ~a ~ ~ h ~ ~ ~ ~ h
~r~ ~1 3 ~ ~ r~ 1:4 V~-~ u~,~
. _ _
~ ~1 6 ~3~4~L9
Table 6F
. _ ___
Initial
charging
ability
Initial O
sensitivity
S
Image flow
Interference
fringe
Residual
potential
_
Ghost
Photosensitivity
irregularity
in generator
direction
Image defect
_
Sensitivity
deterioration
.
Increase of
image defect
:
Maximum value
of hydrogen ~6
: content (atomic ~)
~7
13(~1'
. . - _ .. _ . _
~,~ g ~3~
o
~,~x .~ o o o
15 '-~.` o o u~ o
~o Ir~ o
~ 1 9 ~L3~
1 Table 8F
~ Drum No. F301 F302 F~303 F304 F305 F306 ~ ti v
Initial charging O O O O O O X
. _ _
Initial
sensitivity O O O O O O O
_ _ _ ._ _ ~_
Image flow O O O O O ~ O
_ _
Interference O O O O O O O
l . _ _
Residual
potential O O O O O O X
._ _ . . I
Ghost O O O O O O ~
l _.......... .__ _ ._ l .
Photosensitivity
irregularity O O O O O O
in generator
direction
. __
Image defect O O O ~ O O X
. . _ _ _ I
Sensitivity
20 deterioration O O ~ O O O O
._ ._ -I
Increase of
image defect O O O O O O X
. _ . --- - I
Compa-
Sample No. F301 F302 F303 F304 F305 F306 erxaatmve
-1 -1 -1 -1 -1 -1 2-lF
- 25
.__ _ ._ . _
Maximum value of
hydrogen content 48 58 63 64 69 56 85
(atomic %)
. . . _ _ _ __ __ ....... . . .. _
~so
---~ -- - -- -
oo o o
~ ~ ~ ~ co
o o o ~ o
~r o
~ -- --- ------- -
o o
Lr) U~ o
o ~r ~D X~r O 0 ~r o
:4 :~ X ~ ~ ~ ~ o
m~ Q u~ .
o o
~r o o
O ~r In U~ . O
,X~ ~ ~ o ~
'--1n ~ ~0 ~ ~ '--i ''
o a) ~ro o ~r
~r ~ tq X u~ o . o
~ ~ ~ ~ o r~l
1 X~ m~ Q cn ~ . I ~ _ _¦
o o
o ~ ~ ~
~r o o ~r o
~: ~ ~ ~r o
cq ~:
20 1~ ~ o o lo I _
~ ~ ~ ~ ~o o ~o
.
o a) h ~ o~
Z 3 a) ~: h h h h
~ ~1 (a O ~ O O S~ .Y
::1 h S~ u~ u~ ~, ~ ~ o u~ h 1 o ^
h _ Q El ~) C a) l ,
a ~ ~ ~ ,~
U~ ~; H Q,--I ~ --
.__ _ __ . ._ ~ _ ~1 ._
~5
~3
I Table lO~
~ ur~ ~
S Initial charging O ~) O (~ O S~)
l . 1 -- --- --I -
Initia ~ O O O O O
l . . ~ ._ _ _
Image flow O ~ O ~ O O
I I . --- - - -I --
Interference O O O O O O
i _ _ ._ j _ ._ _ I ._ _ _
Residual
potential ~ O O O
I . _ ... __ ._ ~ _._ ._
Ghost O O ~ O O O
. _ _ _ ._ _ j . ._
irregularity O ~ O O ~ O
in generator
direction
_ _ ~ _ __ . ..
Image defect O O O O O O
_ _ _ _ _ ._ --
Sensitivity
deterioration ~ ~ O ~ O O
_ ._ _ _ ._ .~ _
Increase of
image defect O O O O O O
._ ... ~ _ ... _ _ ..... ._ ._
3(3~
Lr)
_. . , o
o o oR, ~ oo o
oL~70~, x~ln o o In~ I_ Z
O a) u, LO n . .
:I: ~ X 1~ C O t~l ~`I~1 O ~1 h
l Q o Z ~ u~
;~ . . __ (a
o o o E ^ o o u) u~
a~ u~ o o ~I a~
U~ L~ .
o
rl r~l Q O C
u~ m -- z x
... _ _ h
o o ~ ^ o o h
u~ o R. ~ u
~
o ~ a
rl m~ Q Z ;~ .
._ __
E~ ~ o 7 o u~ O
o c~ cq o o ~ o
~4 C~ ~ C~ ~ r-l O ~) O
r~X R z !T ~
. ._ ._ _ ~_
O O ~ ~' u7 O
Is~ O ~ ~r 11)
o ~r ~D ~ O O "~ r~
~ ~q m~ Q ~I t~l r--~ ~ r~
~ u. ~ ~ ~ o
~o ~ o o ~
u~ ~ ~I ~1 O ~ h
1:~ r~ ~1 R O z ~
.. .. _ 3 .. Q.
. a) ~ _ ~n a~
æ - 3 0 ~) 111 tl~ 3 ~ _ .C
E~ r ~ 1~ O ~) ~D O h t~ h ~:
~ ~ ~ u~ ~ ~ Q~ ~ E~ ~ ~ rl
5-1 _ R ~ ~) ~ ~D O r-l rJ Ei
a ~ ~ O ~ ~ ~ ~ r~ ~ ~ O
. ~ V~ .~J _ ~ H p~ _ 14 ~1 _ *
~3~f~fi~
1 Table 12F
_ .... . _ ._ _ __ ___ ~
Drum No. F501 F502 F503 F504 F505 F506
.
abili-ty ~ O O O O O
Initial ~
sensitivity O O O O O O
_
Image flow O O O O ~
Interference
fringe O O O O O O
10 _
Residual O O O O O O
_
Ghost O O O O O O
_ . _ _
Photosensitivity
15 irregularity O O O O O O
in generator
direction
.
Image defect O O O O O
deterioration ~ O O O O O
. ~
Increase of
image defect O O O O O O
. ._
(-)
Remark _ _ ch rg- _ .
~ L~ ~I
~IL3~
_ _ __ _ __ In
_ _ o
o o o ~, ~ o h
o Ln o ~ o o Ln Ln
~~1 Ln r-l ~7 O O 1`~ t~
~D ~5 ^ Ln Ln . . O
o ~ ~r L~l ~ o ~ Z
~D
~4 5 ~4 ~ O ~`J
~ ~ ~ Q v~ ::~
u~ ~ m ~ _ h
O ~ O
Ln o ~2, o ~ Ln
~ ~ o ~ Ln
Ln ~ ~ Ln Lonr~l ~
O ~ ~ r ~ ~ o ~ ~q
~9 ~c ~c 0 ~:
~4 rl t'`l R rl O
u~ z; X
. _._
o ~7
o o p, ~: ~ o .,
Ln o ~2, o Ln
~ ~ Ln o Lr~ O O L a~
o ~ -- Ln Ln .
~D ~ ~ U) ~ ~ ~ O r~
~ ~ X ~1
h .~ 1 ~ rl O h
u~ z
.~
a) ~ o ~,
o o $2, ~ ,~, o t)
P ~n o~ ~4 o L ~
E~ ~ ~ o o Ln
o ~1) ^ Ln In ~I O
~D ~ r ~ ~ . ~ c~
~ ~ o o
~ o ~ ~
u~ P.. _ u~ z ~: O
_ ..._
o O ~ ~: 1` L
Ln o p, o Ln
o ~ ~l Ln ~ Ln Ln ~n O
~ ~ ~ r L~l ~ o ~ ~
~4 X :1: 0
I Q
m -- ~ ~
~ o _ o
o o Q, ~ ~ o
'n o R. O O ~ Ln G
_~ ~:S ~ o o ~ "
o o ^ Ln Ln '
~D ~ n er ~ ~ o
~:C $
.~ L~l ,D r~ O ~
u~ m _u~ z ~c a)'
. . R
. ~ S~ 3 u~ a)
Z _ 0 0 ~ h .C
3 ~ h ~ a) ~^ 1::
~ O ~ V ~ a) 3 S~ u~ h .Y
~ ~ 0 O u~ Ri^ O
h ~4 ~ R Ei C~ ~ ~ ~ o ,~ ~::
_ ~ ~ O c: h ~ .,~ ~ O
._ v~ ~ _ o~ ~ R,--h ~_ *
_ __ .. .
~ 5 ~ j
I Table 14F
.
Drum No. F601 F602 F603 F604 F605 F606
_ .
Initial charging
ability O O O O O
Initial O O O O O O
sensitivity
_ _ ._ _
Image flow O ~ O O ~ O
.. ._ .
fringe ~ O O O ~ O
.
Residual
potential O O ~ O O
._ .
Ghost O O O O O O
. .. _ . _ _ .. _
lS Photosensitivity
irregularity O O O O O O
in generator
direction
. .. _
Image defect O O O O O O
~ ._ ._ _
Sensitivity
deterioration ~ O O O O G
._ ._ .. _ .. _ ... _
Increase of O O O O O O
image defect
~ ................... . .__ _ . ._
~3~4~
Tab le 15 F
l .__
o o ~ ~ o o
~ n o p~ o r- u~ t-
o ~ ^ o o ~ Lr,
r~ a) ~r u~ u~ .
10 ~ ~ r ~ ~ o o
.,1 ~: Q v~ O
U~
'
o o ~ o o
. Lr~ o p~ o U~ U~
o ~ ^ o o ~ U~
I~ ~ X~r u O O O
rl ~ ,~ U~ O a
U~ I
__ . ___
oO 6c: oo o
,~ u O ~ o
o ~ ~_ o o r~l u~
t~ a) ~ u~ ~ .
~ x~ ~ ~ o o
~1 ~ ,D U~ O
v~ m ~ z ~ ~c
.. ~ .__
20 ZO o~ 00 _ ~ ~ X
~:1 ~4 h u~ ~h h h h ~ L~ X
s~ ~ ~ a) ~ e ~^ a)
a Q ~ C~ 3: c: o O ~ ~:;
~ a) O ~ o ~:: h ~ ." ,q
tn ~ _ K Q. ~ ~ 1~
__ _ _.__
~ tj 7 ~ )4~Lg
Table lSF"
O O O ~ -oOo _ ___ ,
O ~ O ~ d~ In ~
~ o ~ o o,_
~ ~--1 rd r~lSl 11'1 ~1 Lr)
O a) u, ~,~ .
r~ ~ o o
o O a
v~ c~ m ~ z c~
.
rd a) o c~ ~
0~ Z
h
r~ U~ O 11~ ~d
rd ~ ~ ~ h ~a
_~ O ~d ~ ~ O
~r o a~
10~o o~'wO ~00 ~00 ~r~ Lo~
x x ~ O x ~ C ~ æ
~ e ~ h~
15 ~ ~ 0 0 1 0 d
O ~d 0 ~ U') ~ h
~4 h h ' ~ ~O
O ~0 0 0r~
)~ h tJI ~r l
a~ ~1 0 ~ Co
~ 0 ~ h ~ r10
o o~ o o o
Ul o~o ~ ~ U t-
I ,~ U~ ~ ~ o ot`~ U~
~r rd Inu~ .
a) 1:~ ~`I ~
d' ~ rl ~
rl t`~l Q O ~L) h
u~ al ~ æ ~ ~
..
~'it5 ~ 3
1 Table 16F
Drum No.F70; F702 F703 E'704 F7015 F705 F706
.~ .. _ ._ _
S Initial charging O O O O O O O
Initial _
sensitivity O O O O O O O
. _
Image flow O O O O O O O
_ . ,
I-nterference
10 fringe O O O O O O O
... _ ~ .
Residual ~ O O O O O
potential l _
Ghost ~ O O O O O O
__
15 Photosensitivity
irxegularity ~ O O O ~ ~ O
in generator
direction
_
Image defect O O O ~ O ~ ~
_ .. _
Sensitivity
2C deterioration O O O O O O O
_
Increase of ~ O O O O
3~
Table 17F
-- o
o o ~ o
10~ ~ ~ ~ ~ r~ ~ o o r u~
o o ~n ~ u~ .
oo ~ r r~J ~ o o
~ 3 ~ a cO O ~c ~
~
o o o c~ n o o o r~ o
o~ ~r ~ ~n
~ ~ X
r~ O O a) ~c
u~ m -- Z ~
_
o o ~2, ^ 1`
O S: ,~ o Ino o r Lr~
~ a) u~ In In .
o ~ r ~ ~ o o
~ ~ ~ P g o ~ ~1
u~ m z~ x
20. s~
æ ~ ~a a 5~ h u3 ~
1~ a) X s~ h
~ ,~ t,~ ~ ~ a) a~ ~Q hE~ o--
a ~ Q e ~ 3 ~ ~ o ~ ~;
O ~ o ~: ~ ~ ~
u~ ~ _ K ~ ~ Q, _ ~ ~ _
L3q3qL~
Tab le 17 F '
. .
1 . _
o o o ~ o o
o u~ O Q~ O ~ oln ~_
,~ o u )~) o o ~`
~Dr~ rd-- u 7 n .
o ~ ~ t~l ,~ o o
ct) ~r ~ ~ u~
X ~ ~ ~ r~ X
r~ r~ `1 Q u~ O o t'
5u~ u~ m -- æ ~ __
rd
~ o O
o U h ~
~1 ~
,~ ~ ~ ,a h
rl
~ ~ ~ h ~
~ ~ ~ ~I h ~ ~ O
oV~ o O ~ ~ o 0 ,~
C:) o o o ~ o .C Z 0 ~1
It~ O ~: r~l U) P.~ S l u~ 01 r1
--I o o o ~ a) ~ h a) r~
In ~_ ~ ~ O ~ ;0
rd u~ o ~J u~ ,C ~d ~l h,C ~ 0
r ~ ,~ o o
~ ~ ~1
r~ ~ R O o o ,~
u~ m ~ z ~ ::c ~ 0~c ~ o o
h ~ æ
~4 '~ o a ~a ~ a
o a) a)
~ z a) ~ 3
Q. h 0
a) ~ u
.C ~ l h ~ -r~ o u
. .. __ ___ E~ r~ ~ rc o ~ o ~
o
o o ~
U~ o ~ o o o
~ ~ U~ ~ o U~
o ,~ o o~ U~
co a) ~r u~ n.
~ ~r ~ 0 :~ ~r ~ ,~ o o
,~ ~ p cn O ~ ~`
~ m -~ æ
glL3~
1 Table 18F
__ _ __ __ ._
Drum No. F801 F802 F803 F804 F_105 F805 F'806
Initial charging O O O O O O O
5 ability
Initial _
sensitivity O O O O O O O
. _
Image flow O O O O ~ ~ O
Interference
10 fringe O O O O O O O
.._
Residual ~ O ~ O O O O
potential
_ .
Ghost ~ O O O O O O
..._
15 Photosensitivity
irregularity O O O O O O O
in generator
direction
. .
Image defect O O O O O
Sensitivity
20 deterioration O O O O O O O
._ .
Increase of O O O O O O O
image defect
~2
Table 19F
~ l
o o~ ~o
O U~Op~O ~ O O In ~
~ ~ ~J ~ o o
j4 ~ X~ p ~n O h
u~ m -- æ ~
o o ~ ~ oo
~ OQ~O ~ O O u~ ~
~ a) ~r In ~ .
o ~ u~ X ~ ~ o o
a~ $ ~ z ~
o o ~:2, G O o
U~O~O ~ O O In ~
~ O ~ U~ In .
o ~ x' ~a ~ ~1 ~1 o o
1:4 rl ~ O (~I
u~ m ~ - æ :C
_
O O P, G o o
m O ~0 ~ In
~o ~ o o ~ ,~
C~ ~ ~D U~ 1~ ~I ~ O O
1:4 ~
~ D u7 Z Xt~l -
h ~ u~
Z ~1 (~ O h 11 3h h E~ O--¦ h
~ ~4 h ~n u~ ~:4-- 3 G O O ~ ~;
a ~ ~ ~ o H ~ ~) i~
U~
I'able l9F"
l ~o ooo~ oo ~ u~
~ 0 3 .
rl ~ Q u~ O ti
,,u~ Z ~ _
., ~ _
. h .C O ~ 1 0
~ a) ~ 0~ U~ Z
o O a) P h
~ ~ a) o ~ a ~rh I
~ a) o
d Q Id h O h u~
. _ 3
~: e -
h.C O lo ,a O
~r a) ~ ~ ~ Ul Z
X ~C ~ O
Il ) Qlr I
O u~ O O (~ h ~
c5~ O O O O ~1 ~I h ~ rl ~J h I
i 4 11~ O ~ ~1 111 O O O Q~ ra ra ~
.~ o ~ o ~ a) o
. u~ .~: ~a Q al h O h u~ c4
r~ O O t~ ~1 E~ 3 (a vl ~ O
a) 1~ L~ . .
~ 0 ~ ~ O O a)
Q Oz ~ h~ O u~ ~d O
a) ~ Z
l ~ O
u~ ~ r l a) E~
O O ~ Q
~1 ~I h h 0 rl ~) h
a) ,o a~ ~ ~ ra u
o
11~ Q (d h O h v~ r~
. E~ 3
.
-1 h 5~ O ~ 0
U~ ~ ~ ~ ~ O
o
Q h ~ S
14 r-1 ~I h h ia -l ~) h I
IL) O O R~ ra ra In
a) ~ ) o
d Q 1~5 h O S~
. E~ 3
.
~L3~ L9
I'able 20F'
._
Drum No. F'901 F'902 F'903 F904
_ __
Initial charging
ability O O O ~
S Initial . _ . _ __
sensitivity O O O O
Image flow O O O O
Interference
fringe O O O O
Residual O O O O
potential
Ghost O O O
.._
Photosensitivity
irregularity O O O O
in generator
direction _
Image defect ~ O
Sensitivity
deterioration O O O O
_ _
image defect O O O
~3~
Table 20F"
Drum No. F90S F90S F905 F90S F906
_
In t1al charging O O O
sensitivity O O O O O
Image flow ~ ~ O ~ O
.
Interference
fringe O ~ O O O
Residual
potential O ~ O ~
Ghost ~3 O ~3 cg 63
Photosensitivity
irregularity O ~ ~ O
in generator
direction
~ , .
Image defect C~3 ~3 O O ~3
Sensitivity
deterioration O ~ ~ O
Increase of O O O O O
image defect
~iG
~o ~
~IL3
I Table 22F'
Sample No. E'1001 F10021F1003 F1004 F1005
_ _ _ ~ ... _
Initia charging ~ ~ ~ ~
Initial O O O O O
Image flow ~ ~ O
Interference
f ringe O ~ O O O
potential ~ O O O
Ghost ~ O ~ O O
Photosensitivity
li~ irregularity ~ O
in generator
direction
Image defect O O ~ O O
Sensitiv ty ~ O ~ O
Increase of O O O O O
_
Resolving
power of lmage O O O O
<IMG>
13~4~
1 Table 24F
Sample ~ ~ F 110 . ~ Fl I O' Fl 10 5
Initial charging
5 1 abllity ~ ~
l sensitivity~ O ~ O
¦ Image flow
Interference
fringe - '~' ~}) O ~}) O
pot eidtua 11 1
I Ghost
Photosensitivity
irregularity
in generator
direction ~ ~
Image defect ~ O ~ I _ ~ O
Sensitivity
deterioration
Increase of
image defect O O ~ ~
Resolving
power oP image j ~ ~ ~
