Note: Descriptions are shown in the official language in which they were submitted.
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DEMANDES OU BREVETS VOLUMlNEUX
LA PRESENTE PART1E DE CETTE DEMANDE OU CE BREVET
COMPREND PLUS D'UN TOME. - .-
CECt EST LE TOME - ~ DE
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THAN ONE VOLUME -. ,
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PlOTE: For additional voiumes~please contact'the Canadian Patent Office
~. . ~=~:= 2046 288 ..~ B674a
272/17
- 1 -
ZINC-BASE GALVANIZED SHEET STEEL EXCELLENT IEd
PRESS-FORMABILITY, PHOSPHATABILITY, ETC.
AND PROCESS FOR PRODUCING THE SAME
1 TECHNICAL FIELD
The present invention relates to a zinc-base
galvanized sheet steel excellent in weldability, press-
formability, phosphatability, etc., and to a process for
producing the same.
BACKGROUND ART
Several methods have been proposed for improving
the weldability of zinc-base galvanized sheet steel. For
example, it has been proposed, as disclosed in Japanese
Patent Application Kokai (Laid-open) No. 55-110,783
published August 26, 1980, to form a film of oxides such
as A120~ on the surface of galvanized sheet steel,
thereby, taking advantage of the high melting point and
high electric resistance o~ the oxides, to improve
weldab~.lity and at the same time to prevent the contact
of the electrode tip with the plating metal, thus
preventing the melt loss of the tip and prolonging the
life thereof.
Further, it has been proposed, as disclosed in
Japanese Patent Application Kokai (Laid-open) No. 59-
104,463, published June 16, 1984, to form an oxide film
of a Zn0/Zn ratio of 0.1-0.70 on the surface of
galvanized sheet steel by heat treatment, thereby to
improve weldability in a similar manner to above.
,.
2046 288
- 2 -
1 However, even these methods hardly give a
satisfactory result on an industrial scale, and the
improvement of weldability in galvanized sheet steel is
eagerly desired.
As to the methods for improving the press-
formability of zinc-base galvanized sheet steel, it has
been disclosed to form a hard film on zinc-base galvanized
sheet steel thereby to prevent galling between the plating
and the die and improve lubricity in press working by, for
example, a method of applying an electrolytic chromate
treatment to the galvanized sheet steel surface to form an
oxide film of Cr203 as described in Japanese Patent
Application Kokai (Laid-open) No. 62-185,883 published
August 14, 1987 and a method of applying an iron-zinc
alloy plating as described in Japanese Patent
Application Kokai (Laid-open) No. 62-192,597 published
August 24, 1987.
Further, it has been disclosed, as described in
Japanese Patent Application Kokai (Laid-open) No. H-1-
136,952 published May 30, 1989, to coat or cover such
organic substances as organic lubricating film,
lubricating oil, etc. on the galvanized sheet steel
surface to improve its press-formability.
However, galvanized sheet steel products
obtained by these methods are unsatisfactory for use in
the automotive industry in the following respects.
Galvanized sheet steel is employed by users in
the automotive industry through a process comprising, in
outline, the step of washing the sheet steel with oil, the
~i.-
. , . ...s~~
L
2446 288
_' - 3 -
1 pressing step, the degreasing step. the phosphating step,
and the painting step. In the case of electrolytic
chromate-treated sheet steel, a phosphate film fails to be
formed in the phosphating treatment. In the case of sheet
steel coated with lubricating oil or lubricating film, a
satisfactory lubricating property is not exhibited since
the coated materials fall off in the washing step.
Further, extra load is put on the degreasing step
precedent to the phosphating treatment, resulting.in a
higher cost. In the case of zinc-base galvanized sheet
steel to which iron-zinc alloy flash plating has been
applied, on the other hand, the sheet is of a higher cost
as compared with those obtained by electrolytic chromate
treatment.
DISCLOSURE OF THE INVENTION
The present inventors have found out that by
forming on the surface of the plating layer an inorganic
covering layer consisting of specified amounts of oxides
of inorganic compounds, etc., an adhesion preventing
function is developed through which said covering layer
sticks fast to the plating layer surface at the time of
press working and the covering layer adhered thereto deforms
according as the plating layer deforms, and by providing,
as desired, in the covering layer a film composed of
specific oxoacids, etc., a rolling lubricating function is
imparted between the die and the plating layer, whereby a
A
2046 288
- 6 -
1 to a draw bead sliding test. Fig. 4 is an electron probe
microanalysis chart of the surface of the sheet steel
shown in Fig. 3. Fig. 5 is a diagram illustrating the
result of glow discharge spectroscopic analysis. in the
thickness direction, of an amorphous oxide-base film
formed in a gradient function type on the surface of an
electrogalvanized sheet steel.
BEST MODE FOR CARRYING OUT THE INVENTION
The zinc-base galvanized sheet steel, the
improvement of which is intended in the present invention,
may be produced by various processes including, for
example, hot dipping, electroplating, vapor deposition,
metal spraying, etc. As to the compositions of the
plating, they may be pure Zn, or they may be alloys which
comprise Zn as the major component, for example, Zn and
Fe, Zn and Ni, Zn and A1, Zn and Mn, Zn and Cr, Zn and Ti,
Zn and Mg, etc., and may further comprise, to improve some
properties such as corrosion resistance, one or more alloy
elements selected from Fe, Ni, Co, A1, Pb, Sn, Sb, Cu, Ti,
Si, B, P, N, S, O, etc. and impurity elements. Further,
they may contain fine particles of ceramics such as
Si02, A1203, etc., oxides such as Ti02, BaCr04,
etc. or organic polymers such as acrylic resins, etc.,
dispersed in the plating layer. The composition may be
uniform in the thickness direction of the plating layer,
or it may vary continuously or in layers. Further, in
2046 288 -.
1 multi-layer plated steel sheets, the uppermost plating
layer may be of pure Zn or it may be an alloy which
comprises Zn as the major component, for example, Zn and
Fe, Zn and Ni, Zn and A1, Zn and Mn, Zn and Cr, Zn and Ti,
Zn and Mg, etc. and may further comprise, to improve some
properties such as corrosion resistance, one or more alloy
elements and impurity elements. Further, it may contain
fine particles of ceramics such as Si02, A1203, etc.,
oxides such as Ti02, BaCr04, etc., and organic polymers
such as acrylic resins, etc., dispersed in the plating
layer.
As specific examples of the galvanized sheet
steel, there may be mentioned hot-dip galvanized sheet
steel, vapor-deposition galvanized sheet steel,
galvannealed sheet steel, zinc-aluminum, iron or the like
alloy coated sheet steel, half-alloyed galvannealed sheet
steel whose lower layer, in the cross-sectional direction
cf the plating layer, has been alloyed (generally called
"half alloy"), differentially coated sheet steel with
galvannealed layer on one side and galvanized layer on the
other side, double layer coated sheet steel with zinc or
zinc-rich, iron or nickel alloy electroplated, or vapor
deposited upper layer on the hot-dip galvanized lower
layer, electrogalvanized sheet steel, sheet steel
electroplated with alloys of zinc, nickel, chromium, etc.,
further, single alloy layer or multi-alloy layer
electroplated sheet steel, and sheet steel galvanized by
~C
.~ _. 2046 288 -
_8_
1 vapor deposition of zinc or zinc-containing metals.
Further, mention may be made of dispersion plated sheet
steel having fine particles of ceramics such as Si02,
A1203, etc., fine particles of ozides such as Ti02,
or organic polymers, dispersed in the zinc or zinc alloy
plating layer.
The present invention intends to improve the
press-formability, phosphatability and, as desired, also
the weldability of such zinc-base galvanized sheet steel
by coating, as described above, a plating metal adhesion
promoting agent, a lubricant, etc. on the surface of the
galvanized sheet steel.
Since the plating layer of zinc-base galvanized
sheet steel is generally soft, the layer readily undergoes
plastic deformation and fits itself to the surface
roughness profile of the die, in press working, to
increase the actual contact area with the die and increase
the frictional force. As a result, the plating layer
tends to be torn off and the resulting peeled o-ff piece of
the layer acts as a binder to cause the plating layer to
be torn off in succession and be accumulated in the die,
which may readily lead to the ultimate rupture of the
material.
The surface of zinc-base galvanized sheet steel
usually has a rust preventive oil applied thereto and, if
desired, a press oil is applied thereto prior to press
working. The function of the oil film is to form a fluid
E~
2046 288
_ g _
1 layer between the die and the plating surface, thereby to
prevent the direct contact between metals. Although the
above-mentioned phenomenon is reduced to a certain extent
by such oil treatments, the oil film is apt to break off
on the sliding face with the die and the above-mentioned
problem is not overcome sufficiently.
Attempts have been made to enhance the oil film
strength by using a high viscosity lubricating oil or a
hot melt type solid lubricating oil, which are effective
in reducing the frictional force in their own way. Such
methods, however, are accompanied by such disadvantages
that, in the steps of degreasing, phosphating treatment
and painting subsequent to the press working, the
degreasing is poorly effected, the degreasing liquid is
contaminated to shorten its life, the phosphating
treatment fails to form a film on the surface or the film
formed by phosphating treatment is poor in corrosion
preventive property.
Another known method is to apply flash plating
of a hard metal, such as Fe-base alloy. onto the zinc-base
plating surface. This method, by coating the soft zinc-
base plating with a hard metal, functions to enhance the
hardness as the composite system and thereby to decrease
the actual contact area with the die. Accordingly, a
thick surface layer plating of about 0.5 um or more is
necessary to exhibit a satisfactory effect, which results
in a high cost.
2046 288
- to -
1 According to the present invention, a novel film
which acts through a working mechanism utterly different
from those in the above-mentioned methods is formed on
zinc-base galvanized sheet steel. Thus, on the surface of
zinc-base plating, there are formed a film having an
adhesion promoting function which is composed mainly of
1-500 mg/mz (in terms of the weight of metallic elements)
of inorganic oxides and/or inorganic hydroxides and a
film, which may be provided as described, having a rolling
lubricating function which is composed mainly of 1-500
mg/m2 (in terms of the weight of metallic elements) of
oxoacids and/or inorganic oxide colloids. These films are
of an amorphous structure constituted mainly of metal-
oxygen bonds. When the film possesses both a structure
having an adhesion promoting function and a structure
having a rolling lubricating function, the two structures
are present mingling with each other via oxygen bonds and
cannot be separated as individual layer structures. They
can only be discriminated as such functions at the time of
press working.
In press working, the amorphous metal-oxygen
bond structure deforms in pursuance of the newly developed
surface of the deforming zinc plating layer and sticks
fast to zinc via oxygen bonds, to prevent the adhesion of
zinc to its die. On the other hand, part of the film is
broken into the form of powders, which then exert the
rolling lubricating function on the sliding face with the
die. This is conceivably the reason why the film of the
!~
2046 288
- 11 -
1 present invention ezhibits a striking lubricity in spite
of being an extremely thin inorganic film.
By way of illustration, an electron photo-
micrograph of the surface of electrogalvanized sheet steel
having an amorphous oxide-base film comprising 8 mg/m2
of Mn and 5 mg/m2 of P formed thereon is shown in Fig.
1. Only zinc plating crystals can be observed in the
Figure and the thin surface film is not recognizable at
all. When the surface is subjected to electron probe
microanalysis. the presence of Mn and P can be confirmed
as shown in Fig. 2. The surface condition of the sheet
steel ezamined with an electron microscope after the sheet
has been subjected to a draw bead sliding test is shown in
Fig. 3. The zinc plating surface has been rubbed by the
bead part of the die, leaving not a trace of original zinc
crystals. Though the test conditions are such that the
rupture Of the sheet would take place in an untreated
electrogalvanized sheet steel, the galvanized sheet steel
having the film of the present invention formed on the
surface maintains a good lubricating condition, the
friction coefficient being 0.17. Fig. 4 shows an electron
probe microanalysis chart of the present sheet steel after
being subjected to a draw bead sliding test. Although the
amounts of Mn and P present in the film are both lower
than those before the sliding test. no rift is observed in
the film and the film remains approximately uniform.
This conceivably shows that the film is reconstructed even
when a new zinc surface develops as the result of
r
_.~ 2046 288
- 12 -
1 sliding. with respect to the Mn/P ratio, it can be seen
that P has decreased to a relatively larger extent as
compared with the ratio before the sliding. It can be
considered that P in the film was selectively broken into
the form of powders and as such contributed to rolling
lubrication.
It can be considered that in a film having an
adhesion promoting function, the function comes mainly
from an amorphous structure comprising mainly oxides
and/or hydroxides of metals as Mn, Mo, Co, Ni, Ca, Cr, V,
W, Ti, A1, Zn, etc., while, in a film having a rolling
lubricating function, which may be formed as desired, the
function comes mainly from a structure wherein colloids
formed of oxoacids comprising P, B etc. and/or oxides of
Si, A1, Ti etc., are bonded to the above-mentioned
amorphous structure via oxygen bonds. However, in the
film forming reaction, the constituents of the film are
precipitated as a harmonious whole from an aqueous
solution by making use of the pH increase at the inter-
face, and hence the working functions cannot be discrimi-
nated strictly. Accordingly, it is more reasonable to
- consider that a part of the film carries the adhesion
promoting function and another part carries the rolling
lubricating function.
The constituents of the film mentioned above are
all inorganic substances, so that no extra load is put on
the degreasing liquid used after press working. Since the
film constituents dissolve with decrease in pH at the time
tC
2046 288
- 13 -
1 of phosphating treatment, the phosphate film can be formed
in a normal manner.
The film formation can be performed with
certainty by dipping zinc-base galvanized sheet steel in
an acidic aqueous solution containing the constituents of
film having an adhesion promoting function and the
constituents of film having a rolling lubricating
function, which may be provided as desired, or by
subjecting the galvanized sheet steel to a cathode
electrolytic treatment in the aqueous solution. In the
dipping treatment, the pH of the interface increases when
Zn goes into solution, and resultantly the film consti-
tuents precipitate as hydroxides or oxides. The dissolved
Zn and other plating layer components also get mixed in
the film. An oxidation-reduction reaction may also be
used. The dissolution of Zn is an oxidation and, in
correspondence thereto, metal ions of oxidized type
precipitate as insoluble oxides of reduced type. Both
anions of oxoacids, such as phosphoric acid etc., and
oxide colloids can also be precipitated by pH increase at
the interface. The cathode electrolytic treatment have
the effect of promoting the pH increase at the interface.
Attempts to control the interfacial reaction by regulation
of water film thickness, as spraying treatment, coating
treatment, etc. may also be used in the present invention.
Firstly, the first aspect of the present
invention is described below.
As one embodiment of the first aspect of the
2046288
- 14 -
1 present invention, mention may be made of a zinc-base
galvanized sheet steel having an inorganic covering layer
formed on the surface thereof, said covering layer being
composed of 1-500 mg/m2, in terms of the weight of
metallic elements, of the oxides of at least one metallic
element selected from the group consisting of Mn, Mo, Co,
Ni, Ca and P.
Hereunder, description will be made with refer-
ence to Mn as the example.
In order to impart a press working lubricity to
a plated sheet steel, it is effective to form a hard film
on the surface of the plated sheet steel. Though the
electrolytic chromate treatment and the iron-zinc alloy
plating are effective in this respect, the former fails to
form a phosphate film, whereas the latter requires a large
amount of plating, resulting in increase in cost.
To solve such problems, it is necessary to
provide a hard film, namely an oxide film, which dissolves
in the phosphating liquid and can form a phosphate film
and, at the same time, does not adversely affect the
phosphating treatment even when the film components
dissolve out into the phosphating liquid.
From such a viewpoint, the present inventors
have found that the above-mentioned need can be met by
forming Mn oxide film on the zinc-base galvanized sheet
steel surface. The Mn oxide film, similarly to chromate
2046 288
- 15 -
1 film, is of a glass-like structure and, at the time of
press forming, suppresses the galling of plating with the
die and enhances sliding property. Further, since it
dissolves in the phosphating liquid, it permits formation
of the phosphate film unlike the chromate film. Moreover,
since Mn is one of the components of the phosphate film,
no adverse effect results even when the Mn oxide film
dissolves out into the phosphating liquid.
Though the structure of the Mn oxide fil~;is not
definitely clear, the present inventors estimate that it
is an amorphous macromolecular structure composed mainly
of a network formed of Mn-O bonds partly substituted with
such groups as -OH, C03, P04, etc., and further with
metals supplied from plating.
Since the film is an oxide film it does not
dissolve in the steps of washing with oil and oil ,
removing, so that it neither undergoes lowering of the
lubricating property due to these steps nor adversely
affects other process steps.
The adhesive property and the film forming
property of the present film can be effectively improved
by addition of inorganic acids such as phosphoric acid,
boric acid, sulfuric acid, nitric acid, hydrochloric acid,
etc., and the salts thereof.
The present film may contain as impurities
substances contained in the treating bath and the
plating. Such impurities may be Zn, A1, Cr, Co, Ni, Pb,
204fi 288
- 16 -
1 Sn, Cu, Ti, Si, B, N, S, P, C1, K, Na, Mg, Ca, Ba, In, C,
Fe, V, W, Mo, etc.
Now, description will be given of the range of
the amount of the film of the present invention.
The amount of the present film must be at least
mg/m2 in terms of Mn to attain a good press-formability,
but when the film amount exceeds 500 mg/m2 it causes
insufficient film formation in the phosphating treatment.
An appropriate film amount, therefore, is not less than 5
mg/m2 and not more than 500 mg/m2 in terms of Mn.
Exactly the same applies in the cases of Mo, Co,
Ni and Ca as in the case of Mn. When the film is formed
by using P oxides, the film must contain 1 mg/m2 or more
(in terms of P) of P oxides, but when the film amount
exceeds 500 mg/m2 the film becomes crystalline, result-
ing in decreased lubricity and lowered press-formability
and causing insufficient film formation in the phosphating
treatment. An appropriate film amount, therefore, is not
less than 1 mg/m2 and not more than 500 mg/m2,
preferably not more than 200 mg/m2.
Hy forming such films in such amounts, it is
recognized that the lubricity is enhanced and the
press-formability is improved.
Thus, the press-formability and the phosphat-
ability are improved by forming a P oxide film on
zinc-base galvanized sheet steel simultaneously.
Such oxide film may be prepared, for example, by
2046 288
- 17 -
1 dipping the galvanized sheet steel in an aqueous solution
of pH 2-6 containing 5-60 g/!L of sodium phosphate, by an
electrolytic treatment in said aqueous solution with the
galvanized sheet steel used as the cathode or the anode,
or by spraying said aqueous solution onto the galvanized
sheet steel.
The adhesive property, etc. of the oxide film
can be favorably improved by adding to said aqueous
solution 1-10 g/!L of at least one etching agent. for
example, sulfuric acid, nitric acid, perchloric acid,
phosphoric acid, etc.
When an oxide film is thus formed on the
galvanized sheet steel surface, part of the plating layer
and of the alloy metals in the plating layer get mixed
into the oxide film as other oxides.
In this case, boric acid may also be present
together. The range of film amount for such a case is
described below.
The amount of the oxide film must be at least 1
mg/m2 in terms of P to attain a good press-formability,
but when the film amount exceeds 500 mg/m2 it causes
insufficient film formation in the phosphating treatment.
An appropriate film amount of P oxide, therefore, is not
less than 1 mg/m2 and not more than 500 mg/m2,
preferably 1-200 mg/m2, in terms of P.
The film amount of boron oxide is preferably
1,000 mg/m2 or less, more preferably 200 mg/m2 or less, in
terms of boron. When the amount exceeds 1,000 mg/m2 it
206 288
- 18 -
1 may deteriorate the phosphatability. The lower limit of
the amount is not critical, as far as it exists.
When boric acid is incorporated into the
above-mentioned oxide film, the film must be formed such
that the total amount of boric acid and phosphoric acid is
not more than 1,000 mg/m2 in terms of P and boron. An
amount exceeding 1,000 mg/m2 is not preferable because
it may deteriorate the phosphatability. The lower limit
is 1 mg/m2. Preferably, the total amount is 200 mg/m2
or less.
The oxide film as mentioned above can be formed
with certainty, for example, by dipping the above-
mentioned zinc-base galvanized sheet steel in an aqueous
solution of pH 2-6 containing 1-60 g/Q of sodium
phosphate, 1-60 g/!L of sodium borate, and an etching aid
agent such as sulfuric acid, by spraying the aqueous
solution onto the sheet steel, or by an electrolytic
treatment in the aqueous solution with the sheet steel
used as the cathode or the anode.
When the oxide film is thus formed, part of the
plating layer and of the alloy metals in the plating layer
get mixed into the oxide film as other oxides.
Although the structure of the film formed of P
oxide, or P oxide and boric acid, is not definitely clear,
it can be estimated that it is an amorphous macromolecular
structure composed mainly of a network formed of P-O bonds
and B-O bonds partly substituted with such groups as -OH,
2046 288
- 19 -
1 C03, etc. and further with metals supplied from plating.
When Mn oxide is used, if necessary and desired,
phosphoric acid and/or boric acid and, as occasion
demands, further at least one oxide selected from the
group consisting of Mo oxide, W oxide and V oxide may be
used in addition to Mn oxide, in a total amount of 1,000
mg/m2 or less (respectively in terms of the weight of
metals) to form a film.
When phosphoric acid alone is used together, the
amount thereof to be incorporated is not more than 1,000
mg/m2 (exclusive of 0). At such amounts, the film
property of Mn oxide is improved. An amount larger than
1,000 mg/m2 is unfavorable since it may deteriorate the
phosphatability. The lower limit of the amount is not
critical. The amount is preferably 200 mg/m2 or less.
In the case of boric acid, too, the amount
thereof to be incorporated is not more than 1,000 mg/m2,
preferably not more than 200 mg/m2, in terms of boron.
An amount larger than 1,000 mg/m2 is unfavorable since
it may deteriorate the phosphatability. The lower limit
of the amount is not critical.
When both boric acid and phosphoric acid are
incorporated, the film is formed such that the total
amount of boric acid and phosphoric acid is not more than
1,000 mg/m2 (in terms of P and boron). An amount larger
than 1,000 mg/m2 is unfavorable because it may deteriorate
the phosphatability. The lower limit of the amount is not
2046 288
- 20 -
1 critical, but a preferable total amount is not more than
200 mg/m2.
When phosphoric acid and at least one ozide
selected from Mo oxide, W oxide and V ozide are used, the
amount (when two or more thereof is used, the total
amount; the same applies hereinafter) is preferably 1,000
mg/m2 or less, more preferably 200 mg/m2 or less, in
terms of P, Mo, W and V, respectively. An amount larger
than 1,000 mg/m2 is unfavorable because it may ._-_
deteriorate the phosphatability. The lower limit of the
amount is not critical.
The aqueous solution used in forming the oxide
film described above may contain, for example, from 1
g/Q to the solubility limit of potassium permanganate,
1-60 g/!L of phosphoric acid and 1-60 g/Q of at least
one compound selected, as described, from molybdic acid,
tungstic acid, vanadic acid, and the salts thereof. The
solution may further contain an etching aid agent, such as
sulfuric acid etc.
The desired ozide film can be formed with
certainty by dipping the above-mentioned zinc-base
galvanized sheet steel in such an aqueous solution, by
spraying the aqueous solution onto the galvanized sheet
steel, or by an electrolytic treatment in the aqueous
solution with the sheet steel used as the cathode or the
anode.
Next, description will be given below of a
case wherein an inorganic covering layer having both an
. 2046 288
- 21 -
1 adhesion promoting function and a rolling lubricating
function is provided by incorporating an oxoacid or the
like into the above-mentioned inorganic covering layer.
The film amount of the inorganic covering layer
having both an adhesion promoting function and a rolling
lubricating function is suitably 2-1,000 mg/m2 when the
above-mentioned inorganic compounds including metals are
calculated in terms of the weight of metallic elements.
When the amount is less than 2 mg/m2 a distinct
lubricating effect cannot be recognized, whereas when the
amount exceeds 1,000 mg/m2, it gives rise to a risk for
the film to peel off in the form of lumps and further it
may adversely affect the film formation in the phosphating
treatment. In another embodiment for forming a covering
layer having both an adhesion promoting function and a
rolling lubricating function, wherein an amorphous
structure film composed mainly of metal oxides and/or
hydroxides and an oxoacid and/or metal oxide colloid film
are formed, the film amounts of the two films are both
suitably 1-500 mg/m2 in terms of metallic elements,
respectively. When the respective amounts are both less
than 1 mg/m2 no distinct lubricating effect is recogni-
zable, whereas when the respective amounts are both larger
than 500 mg/m2 there appears a risk for the films to
peel off in the form of lumps and further the film
formation in the phosphating treatment may be adversely
of fected .
When the amorphous structure film composed
l~r
',
r... 2046 288
- 22 -
1 mainly of metal oxides and/or hydroxides and the oxoacid
and/or metal oxide colloid film are deposited by an
interfacial chemical reaction as in the dipping method or
the cathode electrolytic treatment mentioned above, the
films are in general formed as a mixed film. However, it
is also possible to form the film with gradient functions
such that the adhesion promoting function is stronger at
the interface with zinc plating and the rolling lubri-
Gating function is stronger at the surface of the .film.
In this manner, though no marked effect is observed in the
lubricating property indicated by friction coefficient. an
effect is obtained of increasing the critical face
pressure, at which galling takes place when a high face
pressure is applied to the local part of galvanized sheet
steel as in press-forming a hardly processable part.
Thus, the so-called press forming load range can be
selected widely, which makes the die design easy and the
press operation stable in practice. This is of great
advantage.
The method for forming a gradient function type
film comprises, by making use of the difference in
solubility products of the metal oxides, etc., controlling
the ion concentrations at the interface by regulating the
ion concentrations of respective components, flow rate,
solution temperature and, in the case of electrolytic
treatment, the current density, etc. In the case of Mn-
and P-containing films, for example, when the treating
solution is incorporated with potassium permanganate,
2046 288
- 23 -
1 phosphoric acid, and sulfuric acid and then made to react
with galvanized sheet steel, firstly, as Zn dissolves out,
Mn oxide having the smallest solubility product will
precipitate. The pH at the interface at this time does
not rise rapidly owing to the presence of sulfuric acid,
and next Mn phosphate and/or Zn phosphate will
precipitate with delay. The film thus formed was analyzed
in the thickness direction by glow discharge spectroscopy
and the result is shown in Fig. 5. It can be seer.~_that a
gradient function type film was formed wherein the surface
layer is rich in P and the lower layer is rich in Mn. The
Figure shows a spectroscopic analysis chart in the thick-
ness direction of an amorphous oxide-base film of total
content of Mn of 8 mg/m2 and P of 5 mg/m2 formed with
gradient functions on electrogalvanized sheet steel. The
portion of the chart corresponding to a film thickness of
7 nm or more and a sputtering time of about 0.4 seconds or
more represents the zinc plating layer.
The desired oxide-base film as described above
can be formed, for example, by dipping the above-mentioned
zinc-base galvanized sheet steel in an aqueous solution
containing 50-800 g/Q, respectively, of calcium nitrate,
nickel nitrate, cobalt nitrate and ammonium molybdate,
5-60 g/SL of phosphoric acid and further an etching
auxiliary (such as sulfuric acid, etc.), by spraying the
aqueous solution onto the galvanized sheet steel, or by an
electrolytic treatment in the aqueous solution with the
sheet steel used as the cathode.
r
.~ ' 2046 288
- 24 -
1 The above-mentioned acidic aqueous solution may
further contain at least one zinc dissolution promoting
agent selected from the N03 ion, N02 ion, C103 ion,
F ion and H202.
Said layer may be formed by contacting zinc-base
galvanized sheet steel with an acidic aqueous solution of
a pH of 5 or less which contains ions of at least one
metal selected from Mn, Mo, Co, Ni, Ca, Cr, V, W, Ti, A1
and Zn and further contains at least one oxide colloid of
an element selected from Si, A1 and Ti, or by subjecting
the sheet steel to a cathode electrolysis in said solution.
According to the process of the present inven-
tion, a novel film which works through a working mechanism
utterly different from those in the previous processes is
formed on zinc-base galvanized sheet steel. That is, on
the surface of zinc-base plating are formed a film
composed mainly of 1-500 mg/m2 (in terms of metallic
elements) of inorganic oxide and/or inorganic hydroxides
and having an adhesion promoting function and, if
necessary and desired, a film composed mainly of 1-500
mg/m2 (in terms of metallic elements) of oxoacid and/or
metal oxide colloids and having a rolling lubricating
function.
The film to which has been imparted the two
functions mentioned above has an amorphous structure
composed mainly of metal-oxygen bonds, wherein the film
structure having the adhesion promoting function and the
film structure having the rolling lubricating function are
_1
2046 288
- 25 -
1 present mingling with each other via ozygen bonds and
cannot be separated as individual layer structures. They
can only be discriminated as such functions at the time of
press working.
The second aspect of the present invention, that
is, a process for producing a galvanized sheet steel
excellent in press-formability and phosphatability will be
described below.
Thus, the second aspect of the present invention
relates to a process for producing a zinc-base galvanized
sheet steel excellent in press-formability and phosphat-
ability which comprises forming on the plating layer
surface 2-1,000 mg/m2 (in terms of metallic elements) of
an inorganic covering layer having an adhesion promoting
function, through which the covering layer sticks fast to
the plating layer surface and maintains covering in
pursuance of its deformation at the time of press working,
together with a rolling lubricating function that works
between the die and the plating layer, by contacting the
galvanized sheet steel with an acidic aqueous solution of
a pH of 5 or less which contains ions of at least one
metal selected from Mn, Mo, Co, Ni, Ca, Cr, V, W, Ti, A1
and Zn and/or phosphate ions and, if necessary and
desired, further contains one or two ogoacids of P and/or
B, or by subjecting the sheet steel to a cathode
electrolysis in said acidic aqueous solution.
In practicing the above-mentioned process, a
A-
;.
-T 2046 288
- 26 -
1 more favorable result is obtained when the covering layer
is formed with a function gradient such that the adhesion
promoting function is stronger at the interface with the
plating layer and the rolling lubricating function is
stronger at the covering layer surface.
In press working, the amorphous metal-oxygen
bond structure deforms in pursuance of the newly developed
surface of the deforming zinc plating layer and sticks
fast to zinc via oxygen bonds to prevent the adhes~_on of
zinc to the die. On the other hand, part of the film is
broken into the form of powders, which then exert the
rolling lubricating function on the sliding face with the
die. This is conceivably the reason why the film of the
present invention exhibits a striking lubricity in spite
of being an extremely thin inorganic film.
As described before, in the case of an
electrogalvanized sheet steel having an amorphous oxide-
base film comprising 8 mg/m2 of Mn and 5 mg/m2 of P
formed thereon, only zinc plating crystals can be observed
and the thin surface film cannot be seen at all, as is
apparent from Fig. 1. When the surface is subjected to
electron probe microanalysis. the presence of Mn and P can
be confirmed as shown in Fig. 2. From Fig. 3, which shows
the surface condition examined with an electron microscope
after the surface has been subjected to a draw bead
sliding test, it will be apparent that the zinc plating
surface has been rubbed by the bead part of the die,
leaving not a trace of original zinc crystals. Although
l~
1
2046 288
- 27 -
1 the test conditions are such that the rupture of sheet
would take place in an untreated electrogalvanized sheet
steel, the galvanized sheet steel having the film of the
present invention formed on the surface maintains a good
lubricating condition, the friction coefficient being
0.17. From Fig. 4, which shows an electron probe micro-
analysis chart of the present sheet steel after being subjected
to a draw bead sliding test, it will be apparent that
although the amounts of Mn and P present in the film are
both lower than those before the sliding test, no rift is
observed in the film and the film remains approximately
uniformly. This conceivably shows that the film is
reconstructed even when a new zinc surface develops as the
result of sliding. With respect to the Mn/P ratio, it can
be seen that P has decreased to a relatively larger extent
as compared with the ratio before the sliding. It can be
considered that P in the film was selectively broken into
the form of powders and as such contributed to rolling
lubrication.
It can be considered that in a film having an
adhesion promoting function, the function comes mainly
from an amorphous structure comprising mainly oxides
and/or hydroxides of metals such as Mn, Mo, Co, Ni, Ca,
Cr, V, W, Ti, A1, Zn, etc., while, in a film having a
rolling lubricating function, the function comes mainly
from a structure wherein colloids formed of oxoacids
comprising P, B etc. and/or oxides comprising Si, A1, Ti
etc. are bonded to the above-mentioned amorphous structure
~
,
2046 288 ~ '
._.
- 28 -
1 via oxygen bonds. However, in the film forming reaction,
the constituents of the film are precipitated as a
harmonious whole from an aqueous solution by making use of
the pH increase at the interface, and hence the working
function cannot be discriminated strictly. Accordingly,
it is more reasonable to consider that a part of the film
carries the adhesion promoting function and another part
carries the rolling lubricating function.
The constituents of the film mentioned move are
all inorganic substances, so that no extra load is put on
the degreasing liquid used after press working. Since the
constituents dissolve with decrease in pH at the time of
phosphating treatment, the phosphate film can be formed in
a normal manner.
The film formation can be performed with
certainty by dipping zinc-base galvanized sheet steel in
an acidic aqueous solution of a pH of 5 or less that
contains ions of at least one metal selected from Mn, Mo,
Co, Ni, Ca, Cr, V, W, Ti, A1 and Zn, which are to become
the constituents of film having an adhesion promoting
function, and contains oxoacids of P and/or B, which are
to become the constituents of film having a rolling
lubricating function, or by a cathode electrolytic
treatment of the galvanized sheet steel in said aqueous
solution. As to metallic ions, Mn is vatted to industrial
advantage in the form of permanganate (Mn04 ), which
also offers the advantage of promoting the dissolution of
zinc by making use of the oxidizing power of Mn04 ions,
2046 288
- 29 -
1 Mo, W and V may be vatted stably in the form of molybdate
(Mo04 2), tungstate (W04 2) and vanadate (V04-3),
respectively, or the poly salts thereof. Cr is preferably
used as Cr3+. Cr, Ti and A1 can be dissolved in an
acidic medium of a pH of 2 or less. These metal ions can
be used in concentrations from 1 g/Q to their solubility
limits. The oxoacids of P and B are used respectively in
the form of phosphoric acid and boric acid, or the salts
thereof. The pH of the solution is preferably 5 or less.
When it exceeds 5, the reaction does not proceed
practically: Though the pH of the solution may be
adjusted also with phosphoric acid or boric acid, it is
advantageous as the means for controlling the film amount
and the film constituent ratio independently from each
other to regulate the pH by adding an acid which does not
participate in film formation, for example, sulfuric acid,
hydrochloric acid, nitric acid, acetic acid, perchloric
acid, etc.
As another mode of film formation, it is also
possible to dip zinc-base galvanized sheet steel in an
acidic aqueous solution of a pH of 5 or less that contains
ions of at least one metal selected from Mn, Mo, Co, Ni,
Ca, Cr, V, W, Ti, A1 and Zn, which are to become the
constituents of film having an adhesion promoting
function, and contains, as desired, colloids of the oxide
of at least one element selected from Si, A1 and Ti, which
are to become the constituents of film having a rolling
.~
2046 288
- 30 -
1 lubricating function, or to subject the sheet steel to
cathode electrolytic treatment in the aqueous solution.
As such oxide colloids, Si02, A1203 or Ti02 colloids
having a particle diameter of 0.1 um or less are added
to the acidic aqueous solution, whereby they are dispersed
stably owing to the electrostatic force of the OH group
present on the surface. The total concentration of the
oxide colloids is preferably 60 g/Q or less. The pH of
the solution may be adjusted, besides with phosphoric acid
and boric acid, also with sulfuric acid, hydrochloric
acid, nitric acid, acetic acid, perchloric~acid, etc.
In the dipping, at the time of the dissolution
of Zn, the pH at the interface increases and resultantly
the metal ions change into hydroxides or oxides and
precipitate. When the oxoacids of P and B are present,
they are taken into the amorphous network of metal-oxygen
bonds via oxygen bonds. The oxide colloids also
precipitate as the pH increases and enter the network of
oxygen bonds. The oxide colloids act as the rolling
lubricating function type, one reason for which can be
estimated that the colloids distribute themselves in the
form of clusters in the film. Dissolved zinc and other
plating layer components also get mixed in the film. An
oxidation-reduction reaction may also be used. The
dissolution of Zn is an oxidation and, in correspondence
thereto, metal ions of oxidized type precipitate as
insoluble oxides of reduced type. Permanganate salts
mentioned above represent one of such examples.
-~ 2046288
- 31 -
1 The film forming reaction is of a self passiva-
tion type; that is, when all the surface of zinc-base
plating has been covered, the reaction reaches completion
automatically. The treating time necessary to completion
of the covering is as short as 0.1 second for fast
reactions, and generally a time of 1 minute or less is
sufficient. The treatment can be easily performed at a
treating liquid temperature of from room temperature to so°C.
The film amount can be controlled with the amount of
undercoat zinc dissolved, because if the dissolution of
zinc is regarded as an anodic reaction, the deposition of
film is a corresponding cathodic reaction. Therefore, increase in
the free acid concentration, in other w6rds decrease in
pH, will increase the amount of film. It is also
effective in controlling the film amount to regulate the
thickness of water film furnished to the zinc-base
galvanized sheet steel. surface and thereby to promote the
increase of pH by spraying treatment, coating treatment,
etc.
Cathodic electrolytic treatment has an effect of
promoting a pH increase at the interface and increasing
the film amount. An applied current density of 10 A/dm2
or less is sufficient. A current density exceeding 10
A/dm2 is unfavorable because it promotes the deposition
of metals to deteriorate the lubricating property or gives
a film amount exceeding 1,000 mg/m2 even in a short time
of treatment.
It is also effective in controlling the film
2046 288 ~ '
- 32 -
1 amount to add to the above-mentioned treating liquid a
dissolution promoting agent for zinc-base undercoat
plating. As the dissolution promoting agent, there may
be used one, or two or more, of the N03 ion, NOZ ion,
C103 ion, F ion and H202. The amount of these dissolu-
tion promoting agents to be added is 10 g/Q or less.
The zinc base galvanized sheet steel is
subjected to a contacting treatment with the treating
liquid as dipping, spraying, coating, etc. or to a__;
cathodically electrolytic treatment, then washed with
water and dried; if necessary, it is coated with a rust
preventive oil to prepare for subsequent working steps.
The amount of film having an adhesion promoting
function together with a rolling lubricating function is
suitably 2-1,000 mg/m2 in terms of metals. When the
amount is less than 2 mg/m2 a distinct lubricating
effect is not recognizable, whereas when it is larger than
1,000 mg/m2 it gives rise to a risk for the film to peel
off in the form of lumps and further it may adversely
affect the film formation in the phosphating treatment.
In one mode of forming a covering layer having an adhesion
promoting function together with a rolling lubricating
function wherein an amorphous structure film composed
mainly of metal oxides and/or hydroxides and an oxoacid
and/or metal oxide colloid film are formed, the amounts of
two films are both suitably 1-500 mg/m2 in terms of
metals. At an amount less than 1 mg/m2 no distinct
lubricating effect is recognizable. whereas at an amount
it
2046 288
- 33 -
1 larger than 500 mg/m2 there arises a risk for the film
to peel off in the form of lumps and further the film
formation in the phosphating treatment may be adversely
affected.
When the amorphous structure film composed
mainly of metal oxides and/or hydroxides and the oxoacid
and/or metal oxide colloid film are deposited by an
interfacial chemical reaction as in the dipping method or
in the cathodically electrolytic treatment mentioned
above, the films are in general formed as a mixed film.
However, it is also possible to form the film with
function gradient such that the adhesion promoting
function is stronger at the interface with zinc plating
and the rolling lubricating function is stronger at the
surface of the film. In this manner, though no marked
effect is observed in the lubricating property indicated
by frictional coefficient, an effect is obtained of
increasing the critical face pressure, at which galling
takes place when a high face pressure is applied locally
to galvanized sheet steel as in press forming a hardly
processable part. Thus, the so-called press forming load
range can be selected widely, which makes the die design
easy and the press operation stable in practice. This is
of great advantage.
The method for forming a gradient function-type
film comprises, by making use of the difference in
solubility products of the metal oxide, etc., controlling
the ion concentrations at the interface by regulating the
r"
_ 2046 288
- 34 -
1 ion concentrations of respective components, flow rate,
solution temperature and, in the case of electrolytic
treatment, the current density, etc. A particularly
effective method is to use a solution composition wherein
the total molar concentration of oxoacids is higher than
that of metal ions. Thus, in a film deposition reaction,
the deposition takes place successively, in principle,
with the precipitate having the smallest solubility
product deposited preferentially as the pH at the
interface increases; but, actually, since the reaction is
generally rapid, the film tends to deposit as a mixed
film. In the above-mentioned method, however, use is
made, after the film formation, of a substitution
precipitation reaction which takes place accompanying the
redissolution reaction caused by acids. When the total
molar concentration of oxoacids is higher than that of
metal ions at the interface after the film formation, the
metal oxides and/or hydroxides dissolve and are
substituted with oxoacids of P, B, etc.
The third aspect and the fourth aspect of the
present invention, that is, a zinc-base galvanized sheet
steel excellent in weldability, press-formability and
phosphatability and a process for producing such sheet
steel are described below.
The zinc-base galvanized sheet steel excellent
in weldability, press-formability, and phosphatability
according to the present invention refers to a zinc-base
galvanized sheet steel which comprises zinc-base plated
2046 288
- 35 -
1 sheet steel, a film composed of 30-3,000 mg/m2 of Zn
oxide formed on the surface of the plating layer of said
sheet steel and further, as the upper layer, either an
inorganic covering layer containing at least 1-500 mg/m2
(in terms of the weight of metallic elements) of inorganic
oxides as metal oxides, etc. or an inorganic covering
layer containing 3-500 mg/m2 of Zn oxide together with
5-500 mg/m2 of Mn oxide (respectively in terms of the
weight of metallic element) and, if necessary and desired,
further containing 1,000 mg/m2 or less (in terms of the
weight of elements) of oxides of P, B etc., respectively
formed on said film.
The process for producing said sheet steel
comprises forming zinc oxide on the surface of zinc-base
galvanized sheet steel, and then contacting the resulting
surface with an acidic aqueous solution of a pH of 5 or
less containing at least one member selected from the
group consisting of ions of metals including Mn, Mo, Co,
Ni, Ca, V, W, Ti and A1 and oxoacids containing P and B,
or subjecting it to a cathodic electrolysis in said
aqueous solution, thereby forming a film containing said
constituents on the zinc oxide layer.
The third and the fourth aspects are collec-
tively described in detail below.
First, description is given of the case wherein
Zn oxide and Mn oxide are used in combination.
As described above, the present inventors have
found that a satisfactory result can be obtained by
2046 288
- 36 -
1 forming a Mn oxide film on a zinc-base galvanized sheet
steel surface. The Mn oxide film, similarly to chromate
film, is of a glass-like structure and, at the time of
press working, suppress the galling of the plating with
the die and enhances sliding property. Further, since it
dissolves in the phosphating liquid, it can form the
phosphate film unlike the chromate film. Moreover, it
exerts no adverse effect on phosphating treatment even
when it dissolves out into the conversion treating liquid.
Although Zn oxide by itself can hardly give a
press sliding property-improved film in a wet method, the
present inventors have found that when Zn oxide is in the
form of mixed crystals with Mn oxide, the press sliding
property can be markedly improved and at the same time the
weldability can be also improved. Of course, Zn oxide
also permits the film formation in the phosphating
treatment and exerts no adverse effect even when it
dissolves out into the conversion treating liquid.
Though the structure of the oxides of Mn, Zn and
the like is not definitely clear, it can be estimated that
it is an amorphous macromolecular structure composed
mainly of a network formed of Mn-O, Zn-0 and, as occasion
demands, P-O and B-O bonds, and partly bonded with such
groups as -OH, C03, etc. and, further, substituted with
metals supplied from the plating.
Since the film is an oxide film, it does not
dissolve in the steps of washing with oil and degreasing,
2046 288
- 37 -
1 so that it neither undergoes lowering of the lubricating
property due to such steps, nor adversely affects the
other process steps.
The adhesive property and the film forming
property of the present film can be effectively improved
by addition of inorganic acids such as phosphoric acid,
boric acid, sulfuric acid, nitric acid, hydrochloric acid,
etc., and the salts thereof.
The present film may contain as impurities
substances contained in the treating bath and the
plating. Such impurities may be Zn, A1, Cr, Co, Mn, Pb,
Sn, Cu, Ti, Si, B, N, S, P, C1, K, Na, Mg, Ca, Ba, In, C,
Fe, V, W, Ni, etc.
Hereunder, description is given of the range of
film amount of the present invention.
The amount of the present film must be at least
5 mg/m2 of Mn oxide (in terms of Mn), but when the film
amount is larger than 500 mg/m2 it may cause insuf-
ficient film formation in the phosphating treatment.
An appropriate film amount, therefore, is not
less than 5 mg/m2 and not more than 500 mg/m2 in terms
of Mn.
To improve the adhesive property, film forming
property, etc. of such films, phosphoric acid and/or boric
acid may also be incorporated in the film. In this way,
it is recognized that the Mn-base oxide film structure
becomes more uniform, the film forming property is
2046 288
- 38 -
1 improved, the lubricity is improved to enhance the press-
formability, and the phosphatability is also improved.
Such oxide film can be prepared, for example, by
dipping zinc-base galvanized sheet steel in an aqueous
solution containing 1-70 g/Q of potassium permanganate,
5-60 g/SL of phosphoric acid or boric acid (when the two
acids are used together, respectively 5-60 g/Q) and
100-800 g/!L of zinc nitrate, by subjecting the galvanized
sheet steel to a cathode electrolytic treatment in said
aqueous solution, or by spraying the aqueous solution onto
the galvanized sheet steel, whereby Mn oxide, phosphoric
acid and Zn oxide are formed simultaneously.
When the oxide film is formed on the plated
sheet steel in the above-mentioned manner, the plating
layer and the alloy metals. etc. in the plating layer get
mixed into the oxide film as other oxides. The amount of
phosphoric acid and/or boric acid in the oxide film is
preferably not more than 1,000 mg/m2 (in terms of P
and/or B). An amount larger than 1,000 mg/m2 is
unpreferable because it may deteriorate the phosphat-
ability. The lower limit is not critical so long as
phosphoric acid is contained.
An etching agent, for example. at least one of
sulfuric acid, nitric acid, perchloric acid, etc. is
preferably added to the above-mentioned aqueous solution
in an amount of 1-10 g/Q to improve the adhesive
property, etc. of the film.
2A46 288
- 39 -
1 In the present invention, as described above, Zn
oxide is further incorporated in the film to improve the
weldability. The amount of such oxide film to be formed
is such that the Zn amount in the oxide film is 3-500
mg/m2 per one .side. When the amount is less than 3
mg/m2 no distinct effect is obtained, whereas when it is
larger than 500 mg/m2, the electric resistance increases
and the electrode tip tends to soften and deform,
resulting in a short tip life. Thus, in welding, etc.,
the plating metal fuses due to the heat of welding, and
then alloying of the metal with sheet steel proceeds. If
the plating metal in the fused state contacts directly
with the electrode tip, copper of the tip constituent and
zinc of the plating constituent react selectively to form
a hard and brittle copper-zinc alloy layer, resulting in
the wear of the tip and in a short life of electrode tip.
The plating metal in the fused state is
prevented, by the oxide film formed on the galvanized
sheet steel surface mentioned above, from contacting with
the tip, whereby the melt damage, etc. due to the direct
contact of the plating metal with the tip can be avoided;
further, the plating metal in the fused state alloys
itself with the iron of sheet steel mainly to form iron-
zinc alloy, which sticks to the head of the electrode tip
through cracks etc. in the oxide film or together with the
oxide film, and deposits there to form a protective metal
film for the tip; though the reason is not yet clear, the
protective film does not change its thickness, shape, etc.
2~~+6 288
- 40 -
1 through continued welding, thus ensuring a good welding at
all times and preventing the damage of the tip. The
electrode protecting metal referred to herein comprises
mainly an alloy of the plating metal with base iron and
usually contains, as average concentration, about 20-60%
by weight of Fe and about 40-80% by weight of Zn.
Alloys of higher Fe concentration are preferable in
general. In particular, the presence of local part of
high Zn concentration is unpreferable. The electrode
protecting metal may sometimes contain plating metal
components, sheet steel components such as Mn and S, and
electrode tip components such as Cu.
The electrode protecting metal film has an
effect of keeping the tip head in a convex form, so that
its presence permits welding to be performed at a lower
electric current at the same degree of softening and
damage of the tip. When the tip protecting film is
attached to the tip head surface to occupy 50% or more of
the surface area, the electrode tip life can be greatly
extended. Thus, an oxide film comprising mainly ZnO,
which acts to attach an electrode protecting metal, is .
formed on the zinc metal surface, and welding is performed
while the alloy of the plating metal with the sheet steel
formed by the heat of welding is being attached to the
electrode tip through the above-mentioned oxide film or
together with the oxide film, to form said electrode
protecting metal.
The same weldability improving effect is
;~.. ;
2046 288
- 41 -
1 observed also when the film is formed compositely with Mn
oxide and Zn oxide, as that obtainable with Zn oxide
mentioned above. This is presumably because Mn-Zn
composite oxide has an electric resistance not so much
increased.
Phosphoric acid does not adversely affect the
weldability when the content is 1,000 mg/m2 or less in
terms of P.
Thus. the press-formability and the weldability
of zinc-base galvanized sheet steel can both be improved
and also the phosphating treatment can be performed with a
satisfactory result when a film comprising mainly the
oxides of Mn and Zn and. as desired, P and/or B is formed
on the galvanized sheet steel.
Then, the formation of Zn0 film at a rate of
30-3,000 mg/m2 is described below.
Rust preventive sheet steel is generally in the
form of both side plated, single side plated or differ-
entially plated sheet steel, one and the other sides of
the last one being coated with platings different from
each other.
The present inventors have found that regardless
of the kinds of galvanized sheet steel, so long as the
plating comprises mainly Zn, an electrode protective metal
layer comprising mainly Fe and Zn can be formed at the
electrode tip head in spot welding and thereby the
electrode tip life can be greatly improved, by forming a
Zn0 film on the plated sheet steel.
2046 288
- 42 -
1 In the plated sheet steel of the prior art
mentioned above, it has been difficult to form an oxide
film comprising mainly Zn0 in a Zn0 amount of 30-3,000
mg/m2 (per one side), which is the amount regarded to be
effective in obtaining good weldability, in a stable
manner. The oxide film comprising mainly Zn oxide
referred to herein may contain in the oxides. besides ZnO,
for example the constituent elements contained in the
plating layer and such compounds as the oxides thereof.
Also it may take in, in an electrochemical treatment such
as anodization, the constituents contained in the treating
liquid or the compounds thereof.
The present inventors have found that by
contacting galvanized sheet steel with an acid-containing
aqueous oxidizing agent solution as the first method for
forming an oxide film comprising mainly ZnO, the oxide
film comprising mainly Zn0 can be easily formed in a Zn
amount of 30-3,000 mg/m2 (per one side) and a zinc-base
galvanized sheet steel excellent in weldability can be
provided thereby. The acid acts to dissolve the plating
layer surface to some extent, to furnish ions of Zn etc.
from the plating layer, and to elevate the pH of the
solution contacting the plating layer. The oxidizing
agent acts to oxidize Zn etc. in the bath at the plating
layer surface to form an oxide film comprising mainly Zn0
on the plating layer surface.
Incorporation of an oxidizing agent, for example
10-100 g/Q of HN03, in the aqueous solution makes it
2046 288
- 43 -
1 possible to oxidize Zn etc. thereby to form an oxide film
comprising mainly Zn0 on the plating layer surface. The
lower limit of HN03 was set at 10 g/Q because at still
lower concentrations oxidation hardly takes place,
resulting in failure of oxide film formation. The upper
limit of HN03 was set at 100 g/S~ because at concentrations
exceeding the value the effect as an oxidizing agent
reaches saturation, while the acid dissolves Zn and Fe,
particularly Fe of the alloy layer surface, to increase
the formation of Fe oxide and lowers the effect of
improving the tip life in spot welding.
The formation of surface film is promoted by
further adding, as an oxidizing agent, KMn04, Ca(C10)2,
K2Cr20~, NaC103, C102, KN03, NaN03, etc.
The contacting of sheet steel with the aqueous
solution of HN03 may be performed by any desired methods
including dipping and injection by spraying. After
dipping or injection by spraying, for example dry heating
gas may be blown against the sheet steel surface or the
sheet steel may be heated at below about 100°C. whereby
even a thinner solution is converted into a concentrated
solution by water evaporation and further the reaction
proceeds at elevated temperature, resulting in more
effective treatment.
The oxide film etc. thus formed by the oxide
film forming treatment comprises Zn0 as the main
component, oxides of Fe, and hydroxides of Zn and Fe,
which may be present singly or mingled with one another.
2046 288
- 44 -
1 The film may also contain impurities such as A1, etc.
With respect to characteristic properties as surface film,
an ozide film of high Zn0 content, which can cover the
surface uniformly and has a low film resistance, is
desirable.
To form an ozide film comprising mainly ZnO,
100-600 g/Q of Zn(N03)2 may be incorporated in the
solution as a supply source of Zn ions, which, at a pH of
the aqueous oxidizing agent solution of 4 or less,
contributes to the activation of the plating layer surface
and acts to furnish the Zn ions for forming ZnO.
The lower limit of Zn(N03)2 was set at 100
g/Q because at still lower concentrations the amount of
Zn ions on the alloy layer surface is insufficient to be
able to form oxide film. The upper limit was set at 600
g/!L because when the concentration is higher than that
value too much film is formed to increase the electric
resistance, which results in heat generation due to the
resistance between the sheet steel and the electrode tip,
causing deterioration of weldability due to the enlarge-
ment of the electrode tip diameter.
Into the treating bath, there may sometimes
dissolve out Fe and Zn in the plating and its, impurities
such as Mn, A1, P, Si etc. Among these, Zn ions are
preferably added to the bath beforehand because then Zn
ions need not be supplied by dissolving them out from the
plating layer and hence Zn0 can be deposited in a shorter
time. The elution of other impurities is desirably
fi.
2046 288
- 45 -
1 suppressed to as low an extent as possible. In
particular, Fe, when contained in a concentration higher
than 1 g/Q, forms Fe oxide and hydroxide on the surface
to cause yellowing of the surface and deteriorate the
product quality of the sheet steel surfacet at the same
time the oxide and hydroxide of Fe form an electrical
resistance film and lower the tip life in spot welding.
Accordingly, though the Fe ion concentration is not
specified in the present invention, it is desirably as low
as possible.
The oxide film comprising mainly Zn0 may be
formed by contacting galvanized sheet steel with an
aqueous oxidizing agent solution containing 100-600 g/Q
of Zn(N03)2 and 10-100 g/SL of HN03 at a bath temperature
of 30-80°C for 0.2-10 seconds.
The bath temperature of 30-80°C and its lower
limit of 30°C were selected to facilitate the oxidation of
Zn ions at the plating surface'. When the temperature is
lower than the limit, the reaction velocity is low and the
intended surface film is difficultly obtained. The upper
limit was selected at 80°C. because at higher temperatures
the reaction proceeds too far and the oxide film is formed
excessively, to lower the weldability. Though tempera-
tures higher than 80°C are not absolutely excluded if the
contact time is shortened correspondingly, the high
temperature corresponding to a short time can be regulated
with difficulty, so that the temperature is desirably 80°C
or less.
2046 288
- 46 -
1 Accordingly, the contact treating time in
dipping, spraying, etc. is selected in the range of 0.2-10
seconds though it may vary somewhat depending on the
balance with the line velocity. This is because when the
time is less than 0.2 second the oxide film is formed
insufficiently and the weldability is not improved,
whereas when the treating time is longer than 10 seconds
the oxide film is formed too much, resulting in poor
weldability.
As the second method, an oxide excellent in
weldability can be formed, for example. by subjecting
zinc-base galvanized sheet steel to an electrolytic
treatment in an aqueous solution containing 400 g/Q of
Zn(N03)2~6H20 and 1 g/!L of HN03 with the sheet steel used
as the cathode at a current density of 1-20 A/dm2 and
for a treating time of 0.5-10 seconds.
As the third method, the oxide film comprising
mainly Zn0 can be formed with certainty by performing an
alloying treatment and an oxide film forming treatment,
after melt dipping, electroplating or vapor deposition
plating. More specifically, the oxide film forming
reaction can be effectively performed, for example, by
adjusting an alloying furnace for producing alloyed fused
zinc-plated sheet steel so as to give a sheet temperature
of 300-600°C, passing the sheet steel through the furnace
at such a velocity that alloying is completed up to the
surface, and then subjecting the sheet steel to an
air-water treatment, wherein water and air are injected
204fi 288
- 47 -
1 with an air-water nozzle to secure the dew point of the
atmosphere. Further, the oxide film comprising mainly Zn0
can be formed with certainty by performing, after melt
dipping, electroplating or vapor deposition plating
conducted off line, an alloying treatment and an oxide
film forming treatment. These treatments may be performed
in the same manner as described above. Thus, the oxide
film comprising mainly Zn0 can be formed effectively and
with certainty.
The oxide film may be formed, besides by using
the above-mentioned air-water treatment, for example, by
injecting steam to the plating surface to form the oxide
film comprising mainly Zn0 or by performing, off line, a
heat treatment in a heating furnace in which the dew point
is adjusted to an oxidizing atmosphere, to form the oxide
film comprising mainly ZnO.
In the above-described manner, is formed
30-3.000 mg/m2 of an oxide film comprising mainly ZnO,
as an oxide excellent in weldability, on the surface of
zinc-base galvanized sheet steel, and further thereon can
be formed, as described below, a film comprising oxides
excellent in press-formability and phosphatability.
A good lubricity in press working may be
imparted, in principle, by a method according to the
second aspect of the present invention.
Thus, the lubricity may be imparted by forming
on the surface an oxide-base film comprising the oxide of
2046 288 r
- 48 -
1 at least one element selected from Mn, Mo, Co, Ni, Ca, W,
V, Ti, A1, P and B. The oxide film is of a glass-like
structure similar to chromate film and, at the time of
press working, suppresses the galling of the plating with
the die and enhances the sliding property. Further, since
it dissolves in the phosphatizing liquid, it permits
formation of the phosphate film unlike the chromate film.
Moreover, since the oxide{s) is (are) among the components
of the phosphating film, no adverse effect results even
when the oxides) dissolve{s) out into the phosphating
liquid. As a preferred embodiment wherein two or more
oxides are used in combination, mention may be made of a
case wherein a film comprising 1-500 mg/m2 (in terms of
P or Zn), respectively, of phosphorus oxide and zinc oxide
is formed.
Though the structure of the oxide film is not
definitely clear, it can be estimated that it is an
amorphous macromolecular structure composed mainly of a
network formed of Mn-0 bonds, other metal-0 bonds, P-0
bonds, B-O bonds, Ti-O bonds, and A1-O bonds partly
substituted with such groups as -OH, C03 etc. and
further with metals supplied from the plating.
Since the film is an oxide film, it does not
dissolve in the steps of washing with oil and degreasing,
so that it neither undergoes lowering of the lubricating
property nor adversely affects other process steps.
To improve the adhesive property and the film
~G_
2046 288
- 49 - w
1 forming property of the oxide film, as desired, at least
one colloid selected from colloidal Si02, colloidal
Ti02 and colloidal A1203 may be incorporated in the
film in an amount of not more than 500 mg/m2 (in terms
of Si02, Ti02 and/or A1203). In this manner, the structure
of the oxide film becomes more uniform, and the film form-
ing property, press-formability and phosphatability can be
improved.
Such oxide film can be formed with certainty by
dipping zinc-base galvanized sheet steel in an aqueous
solution of a pH of 5 or less containing ions of at least
one metal selected from Mn, Mo, Co, Ni, Ca, V, W, Ti, A1
etc. and at least one oxoacid that contain P or B, by
spraying the aqueous solution onto the galvanized sheet
steel, or by subjecting the sheet steel to a cathodically
electrolytic treatment in the aqueous solution. In these
treatments, zinc of the plating metal or, in the case of
zinc alloy plating, zinc and alloy elements (metals). and
impurities in the aqueous solution get mixed in the film
as other oxides.
Hereunder, description is given of the range of
amount of the film of the present invention.
The amount of the oxide film must be at least 1
mg/m2 in terms of metal to attain a good press-form-
ability, but when the film amount exceeds 500 mg/m2 it
causes insufficient film formation in the phosphating
conversion. An appropriate film amount, therefore, is
~3
2046 288
- 50 -
1 1-500 mg/m2, preferably 1-200 mg/m2, in terms of
metal. When two or more metal oxides are used, the
respective amounts may be selected in the above-mentioned
range.
The total amount of the at least one colloid
selected from colloidal Si02, colloidal Ti02 and
colloidal A1203 is preferably not more than 500 mg/m2
(in terms of Si02, Ti02 and/or A1203), more preferably
not more than 200 mg/m2. When the amount exceeds_500
mg/m2 the phosphatability may be deteriorated. The lower
limit of the amount is 1 mg/m2.
Then, description is given of a treating bath
for forming the above-mentioned oxide film. As to metal
ions, Mn is vatted to industrial advantage in the form of
permanganate (Mn04 ), which also offers the advantage of
promoting the dissolution of zinc by making use of the
oxidizing power of Mn04 ions. Mo, W and V may be vatted
stably in the form of molybdate (Mn04 2), tungstate
(W04 2) and vanadate (V04 2), respectively, or the poly
salts thereof. Ti and A1 can be dissolved in an acidic
medium of a pH of 2 or less. These metal ions can be used
in concentrations from 1 g/Q to their solubility limits.
The oxoacids of P and B are used respectively in the form
of phosphoric acid and boric acid, or the salts thereof.
The pH of the solution is preferably not more than 5.
When it exceeds 5, the reaction does not proceed
practically. Though the pH of the solution may be
adjusted also with phosphoric acid or boric acid, it is
~A
i
2046 288
- 51 -
1 advantageous as the means for controlling the film amount
and the film constituent ratio independently from each
other to regulate the pH by adding an acid which does not
participate in film formation, for example, sulfuric acid,
hydrochloric acid, nitric acid, acetic acid and perchloric
acid.
Si02, Ti02 and A1203 may be added in the form of an
aqueous solution containing fine particles of respective
colloids, or as potassium silicofluoride, potassium:
titanium fluoride, etc. in an amount of 1-60 g/Q in
terms of solid.
The film forming reaction is of a self passiva-
tion type; that is, when all the surface of zinc-base
plating layer has been covered, the reaction reaches
completion automatically. The treating time necessary to
completion of the covering is as short as 0.1 second for
faster reactions, and generally a time of 1 minute or less
is sufficient. The treatment can be easily performed at a
treating liquid temperature of from room temperature to 80°C.
Though the film forming reaction begins with the dissolu-
tion of the zinc oxide layer, the reaction stops in a
short time because the pH at the interface rises
immediately to deposit and form a covering upper oxide
layer or hydroxide layer. Resultantly, almost all of the
lower zinc oxide layer is retained and thus a two-layer
film is formed. An increase in free acid concentration,
in other words decrease in pH, will increase the amount of
film. It is also effective in controlling the film amount
2046 288
- 52 -
1 to regulate the thickness of water film furnished to the
zinc-base galvanized sheet steel surface and thereby to
promote the increase of pH, by spraying treatment, coating
treatment, etc.
Cathodic electrolytic treatment has an
effect of promoting a pH increase at the interface and
increasing the film amount. An applied current density of
A/dm2 or less is sufficient. A current density
exceeding 10 A/dm2 is-unfavorable because it promotes
10 the deposition of metals to deteriorate the lubricating
property or yields a film amount exceeding 500 mg/m2
even in a short time of treatment.
The present invention is described in detail
below with reference to Examples and Comparative Examples,
which, however, in no way limit the present invention.
First, the kinds of the plated sheet steel used
and the methods of evaluating or determining the
phosphatability, the press-formability, the oxides, the
weldability and the Zn0 film are described below.
(1) Kind of plated sheet steel
AS: Hot-dip galvannealed sheet steel (Fe: 10 wt.%,
Al: 0.25 wt%, balance: Zn),
EG: Electrogalvanized sheet steel,
GI: Hot-dip galvannealed sheet steel (Al: 0.3 wt.%,
Fe: 0.8 wt.%, Pb 0.1 wt.%, balance: Zn),
GG
2046 288
- 53 -
1 HA: Half-alloyed galvannealed sheet steel (Fe: 5 wt.%,
A1: 0.3 wt.%, balance: Zn),
The sheet steel used for all is a 0.8 mm thick conven-
tional sheet steel.
Zn/Zn-Cr: Double-layer electroplated sheet steel
with 2 g/m2 of zinc on the 10% Cr zinc alloy
layer.
(2) Phosphatability
The phosphating treatment was conducted by using
a commercially available phosphatizing liquid, SD 5000
(mfd. by Nippon Paint CO., LTD.), and after performing
degreasing and surface conditioning according to the manu-
facturer's instruction. The phosphate film was ezamined
by means of SEM (secondary electron beam image) and judged
as ~ when the film is uniformly formed, as ~ when it is
partly formed and as X when the film is not formed.
(3) Press-formability (friction coefficient)
Tests were made at several points between normal
loads of 100 and 600 kgf to measure pull-out loads under
the following conditions: test piece size: 17 mm by 300
mm, drawing speed: 500 mm/min., radius of square bead
shoulder: 1.0/3.3 mm, slide length: 200 mm, oil applica-
tion: ~~Noxrust"° 530F (mfd. by Parker Industries, INC.)
40.1 g/m2. The friction coefficient was determined from
the inclination between the normal load and the drawing
force.
2046 288
- 54 -
1 (4) Determination of oxides
The oxides were determined by GDS (glow
discharge spectroscopy) and ICAP (ion plasma emission
spectroscopy)
(5) Weldability
Welding test was conducted under the following
conditions:
1) Applied pressure: 250 kgf
2) Squeezed time: 40 hr.
3) Resistance welding time: 12 hr.
4) Retention time: 5 hr.
5) Welding current: 11 KA
6) Electrode Tip diameter: 5.0 cp (dome head types)
7) Electrode life end point judgement:
Judged by the number of weld spots up to
which a nugget diameter of 3.6 mm was secured at
85% of the welding current.
8) Electrode material: Cu-Cr (conventionally used)
Welding was conducted by placing plated
surfaces of two test specimens on the sides of
both electrodes.
(6) Determination of Zn0 film
The plating layer alone was dissolved with 5%
iodine methyl alcohol solution, and the extraction residue
was fused with a fusing mixture (boric acid: sodium
carbonate = 1 . 3). The resulting product was made into a
2046 288
- 55 -
1 solution with hydrochloric acid and analyzed by ICP to
determine the zinc amount, which was then calculated as
ZnO.
Example 1 and Comparative Example 1 (the case of
manganese oxide)
An Example of the present invention and a
Comparative Example are as shown in Table 1. The
treatment conditions for Run No. 1 of the present Example
were as follows: electrolysis was performed with sheet
steel to be treated used as the cathode and a Pt electrode
used as the anode in a solution containing 50 g/Q of
potassium permanganate, 10 g/Q of phosphoric acid, 3
g/!L of sulfuric acid and 5 g/Q of zinc carbonate at
30°C and at 7 A/dm2 for 1.5 seconds, and the sheet steel
was then washed with water and dried. The other samples
were prepared by regulating the concentrations of
potassium permanganate, phosphoric acid, sulfuric acid and
zinc carbonate, solution temperature, dipping time or
electrolysis amount. It is apparent from Table 1 that the
press-formability is markedly improved without deteriorat-
ing the phosphatability according to the process of the
present invention as compared with those in the
Comparative Example.
2046 288
- 56 -
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X046 288
- 57 -
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2046 288
- 58 -
1 Example II and Comparative Example II (the case of Mo)
An example of the present invention and a
Comparative Example are shown in Table 2. The treatment
conditions for Run No. 1 of the present Example were as
follows: electrolysis was performed in a solution contain-
ing 50 g/Q of ammonium molybdate and 10 g/SL of
phosphoric acid at 30°C with sheet steel to be treated
used as the cathode and a Pt electrode used as the anode
at 7 A/dm2 for 1.5 seconds, and the sheet steel was then
washed with water and dried. Other specimens were
prepared by varying the concentrations of ammonium
molybdate or phosphoric acid, in some specimens sulfuric
acid and zinc carbonate being further added to the
solution, and regulating the solution temperature, dipping
time and coulombic. As is apparent from Table 2,
according to the process of the present invention, the
press-formability is markedly improved without deterio-
rating the phosphatability as compared with those in
Comparative examples.
2046 288
- 59 -
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- 60 -
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2046 288
- 61 -
1 Example III and Comparative Example III (the case of Co)
An Example of the present invention and a
Comparative Example are shown in Table 3. The treatment
condition for Run No. 1 of the present Example were as
follows: electrolysis was performed in a solution contain-
ing 200 g/Q of cobalt nitrate, 150 g/Q of zinc nitrate
and 1 ml/Q of concentrated nitric acid at 30°C with
sheet steel to be treated used as the cathode and a Pt
electrode used as the anode at 7A/dm2 for 1.5 seconds,
and the sheet steel was then washed with water and dried.
Other specimens were prepared by regulating the concentra-
tions of cobalt nitrate, zinc nitrate and nitric acid, in
some specimens phosphoric acid, sulfuric acid and zinc
carbonate being further added to the solution, and
regulating the solution temperature and coulombic amount.
As is apparent from Table 3, according to the process of
the present invention, the press-formability is markedly
improved without deteriorating the phosphatability. as
compared with those in the Comparative Example.
yy
2046 288
- 62 -
~
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1 Example IV and Comparative Example IV (the case of Ni)
An Example of the present invention and a
Comparative Example are shown in Table 4. The treatment
conditions for Run No. 1 of the present Example were as
follows: electrolysis was performed in a solution contain-
ing 250 g/Q of nickel nitrate, 150 g/!L of zinc nitrate
and 1 ml/Q of concentrated nitric acid at 30°C with
sheet steel to be treated used as the cathode and a Pt
electrode used as the anode at 7A/dm2 for 1.5 seconds,
and the sheet steel was then washed with water and dried.
Other specimens were prepared by regulating the concentra-
tions of nickel nitrate, zinc nitrate and nitric acid, in
some specimens phosphoric acid, zinc nitrate and zinc
carbonate being further added to the solution, and
regulating the solution temperature and coulombic amount.
As is apparent from Table 4, according to the process of
the present invention, the press-formability is markedly
improved without deteriorating the phosphatability as
compared with those in the Comparative Example.
2046 288
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2046 288
- 67 -
1 Example V and Comparative Example (the case of Ca)
An Example of the present invention and a
Comparative Example are shown in Table 5. The treatment
conditions for Run No. 1 of the present Example were as
follows: electrolysis was performed in a solution contain-
ing 250 g/Q of calcium nitrate, 150 g/Q of zinc
nitrate and 1 ml/Q of concentrated nitric acid at 30°C
with sheet steel to be treated used as the cathode and a
Pt electrode used as the anode at 7A/dm2 for 1.5
seconds, and the sheet steel was then washed with water
and dried. Other specimens were prepared by regulating
the concentrations of calcium nitrate. zinc nitrate and
nitric acid; in some specimens phosphoric acid, sulfuric
acid and zinc carbonate being further added to the
solution, and regulating the solution temperature and
coulombic amount. As is apparent from Table 7, according
to the process of the present invention, the press-
formability is markedly improved without deteriorating the
phosphatability as compared with those in the comparative
Examples.
2046 288
- 68 -
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2046 288
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1 Example VI and Comparative Example VI (the case of
phosphorus oxide)
An Example of the present invention wherein
phosphorus oxide, or phosphorus oxide and boric acid, were
used respectively and a Comparative Example are shown in
Table 6(a) and Table 6(b). respectively.
2046 288
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2046 288
- 75 -
1 Example VII (a case wherein Mn oxide and other oxides are
used in combination)
An Example wherein a film of oxides of Mn and P
was formed is shown in Table 7(a), an Example wherein Mn,
boric acid and optionally phosphorus oxide were used is
shown in Table 7(b). and an Example wherein a film of
oxides of Mn and one or two selected from P, Mo, W and V
is shown in Table 7(c).
The oxide film shown in Table 7(a) was formed by
performing an electrolysis in a solution containing 50
g/SL potassium permanganate, 10 g/Q phosphoric acid, 3 g/SL
of sulfuric acid and 5 g/Q of zinc carbonate at 30°C with
sheet steel to be treated used as the cathode and a Pt
electrode used as the anode at 7 A/dm2 for 1.5 seconds,
followed by water washing and drying. Films in other Runs
were formed in the same manner but by regulating the
concentrations of potassium permanganate. phosphoric acid,
sulfuric acid and zinc carbonate, solution temperature and
dipping time. It is apparent from Table 7(a) that the
sheet steels of the present invention have a markedly
improved press-formability without deteriorating the
phosphatability as compared with those of Comparative
Example.
2046 288
- 76 -
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2046 288
- 82 -
1 Example VIII
An Example wherein an inorganic covering layer
having both functions of adhesion prevention and rolling
lubrication according to the present invention was
provided is shown in Table 8 along with a Comparative
Example.
The breaking critical load ratio was determined
in the following way.
In the draw bead test described before, the
normal load (i.e., pressing load) at which the drawing
force increases sharply was taken as the breaking critical
load, from which the breaking critical load ratio was
calculated by the following equation.
Breaking critical load ratio
Breaking critical load
Tensile strength x Sheet width x Sheet thickness
The amounts of the film having an adhesion
preventing function and the film having a rolling
lubricating function were expressed in terms of metal
amounts. The amounts of metals which had dissolved out
from the undercoat plating and deposited could not be
determined and hence are not indicated in the Table.
~A
2046 288
- 83 -
..
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2046 288
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2046 288
- 93 -
1 Example IX (Weldability improvement by combined use of Zn
oxide and Mn oxide)
An Example wherein a film was formed which
comprised 3-500 mg/m2 (as Zn) of Zn oxide, 5-500 mg/m2
(as Mn) of Mn oxide and, as desired, 1,000 mg/m2 or less
(as boron or phosphorus) of boric acid or phosphoric acid and
optionally other oxides and a comparative Example are shown
in Table 9(a), Table 9(b) and Table 9(c).
The amounts of the oxides were determined by GDS
(glow discharge spectroscopy) or ICAP (ion plasma emission
analysis).
~t A
.- 2046288 ~'
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2046 288 .~.
- 96 -
Table 9(b)
Plating Film formed
Run Plated i
ht
we
g
No. sheet (Top face/ Zn film Mn film P film
steel Bottom amount amount amount
face)
(9/m2) (m9/m2) (mg/m2) (mg/2)
1 EG 20/20 45 23 14
2 EG 40/40 10 7
3 EG 60/60 5 g 2
4 EG 60/60 20 24 14
5 EG 60/60 30 40 35
6 EG 60/60 180 87 100
Ex- 7 EG 60/60 95 130 550
ample 8 AS 60/60 470 453 800
9(b) 9 AS 30/60 300 130 70
10 AS 45/45 250 54 43
11 AS 60/60 50 28 32
12 GI 90/90 50 32 27
13 GI 120/120 50 34 28
14 HA 60/60 50 29 27
15 HA 100/100 50 34 27
1 EG 20/20 50 - _
2 EG 20/60 <1 64 44
Comp. 3 EG 60/60 Electro- 23(Cr) -
lytic
Ex- chromate
ample 4 AS 60/60 800 700 1300
9(b) 5 AS 45/45 50 880 300
6 AS 45/45 300 - 1500
7 HA 60/60 100 - _
8 GI 120/120 - - _
(to be cont'd)
2046 288
- 97 -
Table 9(b) (cont'd)
Run Phosphat- Press- Weldability
No. ability formability (Number
(Friction of spot)
coefficient)
1 0 0.106 6000
2 0 0.155 6000
3 0 0.155 6000
4 0 0.110 6000
5 0 0.114 6000
6 0 0.140 6000
Ex- 7 0 0.146 6000
ample 8 0 0.147 6000
g(b) g o 0.120 6000
10 0 0.100 6000
11 0 0.105 6000
12 0 0.115 6000
13 0 0.115 6000
14 0 0.116 6000
15 0 0.111 6000
1 0 0.948 6000
2 0 0.154 500
3 x 0.182 6000
Comp.
Ex-
ample 4 D 0.200 1000
9(b) 5 D 0.178 4000
6 p 0.382 1000
7 0 0.718 6000
g o 0.755 500
r:.-,
2046 288
_ 98 _
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2046 288
- 102 -
1 Example 10
An Example where on the surface of zinc-base
galvanized sheet steel was coated 30-3,000 mg/m2 (in
terms of Zn0) of an oxide and further thereon, as the
upper layer, was coated 1-500 mg/m2 (in terms of the
metal in the oxide) of at least one substance selected
from Mn oxide, P oxide, Mo oxide, Co oxide, Ni oxide, Ca
oxide, W oxide, and boric acid is shown in Table 10 along
with a Comparative Example.
The Zn0 film was formed by one of the following
three methods.
Dipping: The galvanized sheet steel was dipped
in an aqueous solution containing 400 g/!L of Zn(N03)2~6H20
and 70 g/Q of HN03 at 50°C for 1-10 seconds to form the
Zn0 film.
Electrolysis: Electrolysis was conducted in an
aqueous solution containing 400 g/!L of Zn(N03)2~6H20 and 1
g/Q of HN03 with the galvanized sheet steel used as the
cathode at a current density of 7 A/dm2 for 1-7 seconds to
form the Zn0 film.
Air-water spraying: Atomized water was injected
at a rate of 80-125 Q/min. to the surface of the galva-
nized sheet steel (at 500°C) which had been subjected to
alloying treatment, to form the Zn0 film.
The upper layer oxide films were formed as
follows.
The Mn oxide was formed by dipping the sheet
steel to be treated in a solution at 30°C containing 50
2046 288
- 103 -
1 g/Q of potassium permanganate, 10 g/Q of phosphoric acid,
3 g/Q of sulfuric acid and 5 g/Q of zinc carbonate or
conducting electrolysis in the solution with the sheet
steel to be treated used as the cathode and a Pt electrode
used as the anode at 7 A/dm2 for 1.5 seconds. followed
by water washing and drying.
The P oxide was formed by dipping the galvanized
sheet steel in an aqueous solution containing 50 g/!L of
potassium phosphate and 10 g/Q phosphoric acid or by an
electrolytic treatment (5-10 A/dm2, 1-1.5 seconds) in
the solution with the sheet steel used as the cathode or
the anode.
The Mo oxide was formed by dipping the sheet
steel to be treated in a solution (at 30°C) containing 50
g/!L of ammonium molybdate and 10 g/Q phosphoric acid
or conducting electrolysis in the solution with the sheet
steel used as the cathode and a Pt electrode used as the
anode at 7 A/dm2 for 1.5 seconds. followed by water
washing and drying. In other Runs the oxide was formed by
regulating the concentrations of ammonium molybdate and
phosphoric acid, in some runs further adding sulfuric acid
and zinc carbonate, and regulating the solution tempera-
ture, dipping time and coulombic amount.
The Co oxide was formed by conducting electro-
lysis in a solution containing 200 g/!t of cobalt nitrate,
150 g/Q zinc nitrate and 1 ml/SL of concentrated nitric
acid at 30°C with the sheet steel to be treated used as
the cathode and a Pt electrode used as the anode at 7
204fi 288
- 104 -
1 A/dm2 for 1.5 seconds, followed by water washing and
drying. In other Runs, the oxide was formed by regulating
the concentrations of cobalt nitrate, zinc nitrate and
nitric acid, further adding phosphoric acid, sulfuric acid
and zinc carbonate in some Runs, and regulating the
solution temperature and coulombic amount.
The Ni oxide was formed by conducting
electrolysis in a solution containing 250 g/Q of nickel
nitrate, 150 g/Q of zinc nitrate and 1 ml/Q of concent-
rated nitric acid at 30°C with the sheet steel to be
treated used as the cathode and a Pt electrode used as the
anode at 7 A/dm2 for 1.5 seconds, followed by water
washing and drying. In other Runs the oxide was formed by
regulating the concentrations of nickel nitrate. zinc
nitrate and nitric acid, adding further phosphoric acid,
sulfuric acid and zinc carbonate in some Runs, and
regulating the solution temperature and coulombic amount.
The Ca oxide was formed by conducting electro-
lysis in a solution containing 250 g/Q of calcium
nitrate and 1 ml/Q of concentrated nitric acid at 30°C
with the sheet steel to be treated used as the cathode and
a Pt electrode used as the anode at 7 A/dm2 for 1.5
seconds, followed by water washing and drying; and
further, regulating the concentrations of calcium nitrate
and nitric acid, adding further phosphoric acid, sulfuric
acid and zinc carbonate in some Runs, and regulating the
solution temperature and coulombic amount.
2046 288
- 105 -
1 The W oxide was formed by dipping the sheet
steel to be treated in a solution at 30°C containing 20
g/Q of ammonium tungstate and 10 g/Q of phosphoric
acid or conducting electrolysis in the solution with the
sheet~steel used as the cathode and a Pt electrode as the
anode at 7 A/dm2 for 1.5 seconds,' followed by water
washing and drying; and further, regulating the concent-
rations of ammonium tungstate and phosphoric acid, adding
further sulfuric acid and zinc carbonate in some Runs, and
regulating the solution temperature, dipping time and
coulombic amount.
The V oxide was formed by conducting electro-
lysis in an aqueous solution containing 30 g/Q of
ammonium vanadate and 10 g/!L of phosphoric acid at 30°C
with the sheet steel to be treated used as the cathode and
a Pt electrode used as the anode at 7 A/dmz for 1.5
seconds, followed by water washing and drying; and
further, regulating the concentrations of ammonium
vanadate and phosphoric acid, adding further sulfuric acid
and zinc carbonate in some Runs, and regulating the
solution temperature, electrolysis time and coulombic
amount.
The boron oxide was formed by conducting
electrolysis in an aqueous solution containing 50 g/Q of
boric acid with the zinc-base galvanized sheet steel used
as the cathode under electrolytic conditions of 7 A/dm2
and 1.5-7 seconds.
The Zn oxide was formed by an electrolytic
2046 288
- 106 -
1 treatment (5-10 A/dm2, 1.0-1.5 seconds) in an aqueous
solution containing 100-800 g/Q of zinc nitrate and 5-60
g/Q of phosphoric acid with the galvanized sheet steel
used as the cathode or the anode or a dipping treatment in
the solution, to form the oxide film.
The mixed oxide film was formed by preparing a
treating bath incorporated with respective appropriate
metal salts or acid described above.
2Q46 288
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2046 288
- 191 -
1 Ezample 11
An Example of the present invention wherein zinc
oxide was formed on the surface of zinc-base galvanized
sheet steel and further thereon, as the upper layer, was
formed a film comprising ozides by using an acidic aqueous
solution of a pH of 5 or less which contains at least one
member selected from ions of metals including Mn, Mo, Co,
Ni, Ca, V, W, Ti, and A1 and ogoacids containing P or B is
shown in Table 11 along with a Comparative Example.
The Zn0 film was formed by one of the following
three methods.
Dipping: The galvanized sheet steel was dipped
in an aqueous solution containing 400 g/SL Zn(N03)2~6H20
and 70 g/Q of HN03 at 50°C for 1-10 seconds to form the
Zn0 film.
Electrolysis: Electrolysis was conducted in an
aqueous solution containing 400 g/Q of Zn(N03)2~6H20 and 1
g/SL of HN03 with the galvanized sheet steel used as the
cathode at a current density of 7 A/dm2 for 1-7 seconds
to form the Zn0 film.
Air-water spraying: Atomized water was injected
at a rate of 80-125 Q/min. to the surface of the galva-
nized sheet steel (at 500°C) which had been subjected to
alloying treatment, to form the Zn0 film.
The upper layer oxide films were formed as
follows.
The Mn oxide was formed by dipping the sheet
steel to be treated in a solution at 30°C containing 50
fs A
t.
2046 288 _
- 192 -
1 g/Q of potassium permanganate. 10 g/Q of phosphoric acid,
3 g/Q sulfuric acid and 5 g/Q of zinc carbonate or
conducting electrolysis in the solution with the sheet
steel used as the cathode and a Pt electrode used as the
anode ~at 7 A/dm2 for 1.5 seconds, followed by water
washing and drying.
The P oxide was formed by dipping the zinc-base
galvanized sheet steel in an aqueous solution containing
50 g/Q of potassium phosphate and 10 g/Q of phosphoric
acid or by an electrolytic treatment (5-10 A/dm2, 1-1.5
seconds) in the solution with the sheet steel used as the
cathode or the anode.
The Mo oxide was formed by dipping the sheet
steel to be treated in a solution (at 30°C) containing 50
g/Q of ammonium molybdate and 10 g/Q of phosphoric
acid or conducting electrolysis in the solution with the
sheet steel used as the cathode and a Pt electrode used as
the anode at 7A/dm2 for 1.5 seconds, followed by water
washing and drying. In other Runs the oxide was formed by
regulating the concentrations of ammonium molybdate and
phosphoric acid, in some runs further adding sulfuric acid
and zinc carbonate, and regulating the solution
temperature, dipping time and coulombic amount.
The Co oxide was formed by conducting
electrolysis in a solution containing 200 g/Q of cobalt
nitrate, 150 g/!L of zinc nitrate and 1 ml/Q of concent-
rated nitric acid at 30°C with the sheet steel to be
treated used as the cathode and a Pt electrode used as the
2046 288 _
- 193 -
1 anode at 7A/dm2 for 1.5 seconds, followed by water
washing and drying. In other Runs, the oxide was formed
by regulating the concentrations of cobalt nitrate, zinc
nitrate and nitric acid, further adding phosphoric acid,
sulfuric acid and zinc carbonate in some Runs, and
regulating the solution temperature and coulombic amount.
The Ni oxide was formed by conducting
electrolysis in a solution containing 250 g/Q of nickel
nitrate, 150 g/Q of zinc nitrate and 1 ml/Q of concent-
rated nitric acid at 30°C with the sheet steel to be
treated used as the cathode and a Pt electrode used as the
anode at 7A/dm2 for 1.5 seconds, followed by water
washing and drying. In other Runs the oxide was formed by
regulating the concentrations of nickel nitrate. zinc
nitrate and nitric acid, adding further phosphoric acid,
sulfuric acid and zinc carbonate in some Runs, and
regulating the solution temperature and coulombic amount.
The Ca oxide was formed by conducting electro-
lysis in a solution containing 250 g/!~ of calcium
nitrate and 1 ml of concentrated nitric acid at 30°C with
the sheet steel to be treated used as the cathode and a Pt
electrode used as the anode at 7 A/dm2 for 1.5 seconds,
followed by water washing and drying; and further,
regulating the concentrations of calcium nitrate and
nitric acid, adding further phosphoric acid, sulfuric acid
and zinc carbonate in some Runs, and regulating the
2046 288
- 194 -
1 solution temperature and coulombic amount.
The W oxide was formed by dipping the sheet
steel to be treated in a solution (at 30°C) containing 20
g/Q of ammonium tungstate and 10 g/Q of phosphoric
acid or conducting electrolysis in the solution with the
sheet steel used as the cathode and a Pt electrode used as
the anode at 7 A/dm2 for 1.5 seconds, followed by water
washing and drying; and further, regulating the concent-
rations of ammonium tungstate and phosphoric acid, adding
further sulfuric acid and zinc carbonate in some Runs, and
regulating the solution concentration, dipping time and
coulombic amount.
The V oxide was formed by conducting electro-
lysis in an aqueous solution containing 30 g/SL of
ammonium vanadate and 10 g/Q of phosphoric acid,at 30°C
with the sheet steel to be treated used as the cathode and
a Pt electrode used as the anode at 7 A/dm2 for 1.5
seconds. followed by water washing and drying; and
further, regulating the concentrations of ammonium
vanadate and phosphoric acid, adding further sulfuric acid
and zinc carbonate in some Runs, and regulating the
solution temperature, electrolysis time and coulombic
amount.
The boron oxide was formed by conducting
electrolysis in an aqueous solution containing 50 g/Q of
boric acid with the zinc-base galvanized sheet steel used
as the cathode under the electrolytic conditions of 7
A/dm2 and 1.5-7 seconds.
2o4s 28a
- 195 -
1 The mined ozide film was formed by preparing a
treating bath incorporated with respective appropriate
metal salts or acids mentioned above.
2046 288
- 196 -
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DEMANDES OU BREVETS VO~UMINEUX
LA PRESENTS PARTIE DE C>=TTE DEMANDS OU CE BREVET
COMPREND PLUS D'UN TOME. - _-
CECI EST LE TOME ~ DE
NOTE: Pour Ies tomes additionels, veuiilez co~tacter !e Bureau canadien des
brevets
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THAN ONE VOLUME -
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