Note: Descriptions are shown in the official language in which they were submitted.
P~S
BACKGROUND OF THE INVENTION
This invention relates to friction compositions, particularly
asbestos free friction compositions especially suitable for use as
disc brake pads or drum shoe lining in the automotive industry.
Because of its assumed chemical and biological inertness,
its temperatuxe resistance, its fibrous nature, and its possession
of approximately the appropria.te degree of hardness and coefficient
of friction with ferrous metals, asbestos has been used as a main-
stay of friction materials in industry in general and in particular
in the automotive industry. The composition of these materials
frequently included additives of various types to improve their
bonding characteristics, their noise generating potential, their
heat transfer ability, or even to reduce their costs. Among the
additives listecl in the prior art are ~inc oxicle alld calcium
carbonate used in percentages of less than 20~ in combination
with asbestos or even on occasion with other fibrous materials.
Applicant considers the following U. S. patents to be relevant
-2- ~.a~
6~
.i to his invention or to particularly pref~rred emboclimcnts thorcc)~.
Copies thereof accompany this application.
2,078 r 617-Spokes disclosing the use of cashew nut oil in
friction surfaces such as brakes and clutches. The use of asbestos
is contemplated (col. 3, line 59).
2,158,337-Rasmussen describes a brake lining having a glass
fiber incorporated therein. The glass fiber may be used in place
of asbestos and is contemplated as the primary friction material.
2,165,140-Harvey discloses friction elements containing hexa-
10 methylene tetramine modified cashew nut oil, and phenolic resinsused with fillers in the usual proportions, such as zinc oxide,
carbon, barytes and rubber. Fibers other than asbestos may be
used.
3,526,306-Bentz et al., discloses a clutch facing which con-
tains glass filaments in combination with asbestos, phenolic resins,butadiene-acrylonitrile rubber, barytes and particulate cashew nut
oil.
3,850,874-Grazen et al., discloses a friction element contain-
ing a substitute material for the cashew nut oil particles of con-
ventional friction compositions.
3,857,811-Grazen et al., claims the composition of the sub-
stitute material used in the 3,850,874 patent.
3,297,599-Eschen discloses the use of calcium aluminate in
otherwise conventional brake compositions.
3,916,062-Dougherty discloses the use of molecular sieves in
otherwise conventional friction materials, and
4,002,592-Baskin discloses the use of spinels in low con-
centration as friction modifiers in otherwise conventional friction
compositions.
The compositions of this invention employ ~inc oxide and~or
calcium carbonate and materials with similar properties, as set
forth more fully hereinafter, in quantities greater than 20~ to
totally replace asbestos in friction compositions.
Replacement of asbestos has, of course, become desirable
from the standpoint of friction material manufacturers and of
~, 'rl
those wllo directly ha~ldle the Einishcd product ill pUt~ J il irl~o
the vcllicle in which it ls used bccausc o~ rcsE~lratory haz.lrcls
found to be associated with its use and the expense of health pre-
cautions llOW required for its safe handling.
SUMM~Y OF THE INVE~TION
The invention provides in a composition aspect a substantially
asbestos free friction material which comprises as essential in-
gredients:
a. a thermosetting resin;
b. cashew particles;
c. a structural integrity providing proportion of a
non-asbestos fiber; and
d. more than 20% by weight of a powdered inorganic
compound having a Moh's hardness rating greater
than 2.0 and less than 5.0 and capable of being
- subjected to temperatures of greater than about
425C without substantial chemical or physical
alteration.
The tangible embodiments of this composition aspect oE the
invention possess the inherent applied use characteristic of
being friction materials particularly suitable for fabrication
into disc brake pads for automotive use. The compositions possess
wear and braking qualities comparable to similar compositions con-
taining asbestos.
The invention also provides in a preferred aspect of this
composition aspect of the invention a friction composition which
comprises, in addition to the aforementioned essential ingredients,
barytes.
The invention also provides another preferred aspect of this
comuosition aspect of the invelltion which compriscs, in additio~
to the aforemelltioned essential ingrediell-ts, ru~er paL ticles.
The invention also provides in another preferred aspect of this
composition aspect of the invention a friction composition which
comprises, in addition to the aforementioned essential ingredients,
non-ferrous metal cllips.
11~`6~95
Thc invell~ioll Eurther providcs in anothcr ~)rc~errc(l asL~ecL
of this composition aspcct of the invention a friction composi-
tion which comprises, in addition to the aforementioned essential
ingredients, 1 to 15~ by weight of an unloaded molecular sieve.
Special mention is made of compositions of this composition
aspect of the invention wherein the powdered inorganic compound
is
1. Zinc oxide;
2. Calcium carbonate;
3. Zinc oxide and calcium carbonate in combination.
The invention also provides in a composition aspect an im-
proved friction composition suitable for use in brakes for auto-
motive vehicles wherein the improvement comprises replacing the
entire asbestos content of conventional automotive brake pad com-
positions with greater than 20~ by weight of the total pad con-
tents of a powdery inorganic material a Moh's hardness rating of
greater than 2.0 and less than 5.0 and capable of withstanding
temperatures of greater than about ~25~C without substan-tial
chemical or physical decomposition together with a minor proportion
of a non-asbestos fibrous material.
The invention also provides in a process aspect a process
for the manufacture of an asbestos free automotive brake shoe
which comprises fastening to a conventional brake shoe backing
plate, a friction pad formed from the asbestos free friction
compositions of this invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The compositions of the present invention may be prepared in
a fashion analogous to that employed for the preparation of known
prior art compositions from well-known commercially available
materials. The thermosetting resins generally known to be usc-
ful in the production o~ brake lining materials may be employed.
These include, for example, urea formaldehyde resins, cresol
resins, pheno:L formaldehyde resins, melamine formaldehyde resins,
alkyds, polysiloxanes and epoxy resins. The phenol formaldehyde
resins are preferred. The cashew particles are the conventiollal
q395
thermosettinq cashew nut resins commonly employed in ~abricatillc~
brake shoe pacls wllich are preferred. Other equivalent products
are known, such as those described in U. S. Patents 3,658,751,
3,850,874 ancl 3,857,811. As used herein and in the appended
claims the term cashew particles or cashew nut particles also
contemplates these known equivalent materials. The non-asbestos
fiber or fibrous material may be any- organic or inorganic fibrous
material which is capable of providing structural integrity to the
mixed uncured friction composition until,upon cure,it is fused into
a solid mass. The term will therefore include the degradation i)ro-
- ducts of those fibrous materials which do not survive the curing
process temperatures, approximately 160C, unaltered. Suitable
materials include,for example, fiberglass, mineral wool, silica
fibers, carbon fibers, boron fibers, and the like, cotton, rayon,
polyamide, polyester fibers and the like, as well as tungsten or
steel fibers and the like. While essentially any non-asbestos
fiber will suffice for structural integrity purposes during the
molding process, it will be apparent that for greater structural
integrity during use a fiber capable of withstanding the tempera-
tures generated immediately below the rotor stator in-terface will
be preferred. It ic a~pare~t that the majority of such materials
will be inorganic in nature. It has been found in the manufacture
of the disc brake pads of the invention that a mixture of longer
and shorter fiber lengths may be a convenience in processing
and may improve the integrity of the finished pad. The powdered
inorganic compound which is employed in a relatively high per-
centage of the composition to replace the asbestos may include
a number of materials such as zinc oxide, or calcium carbonate,
which have been normally considered as fillers when usecl in
small quantities in prior art asbestos containing brake com-
positions. E:ssentially any material known to have the necessary
hardness range and to be able to withstand the temperatures en-
countered immediately below the rotor stator interface during
braking may be employed. In addition to -the zinc oxide and
calcium carbc,nate already mentioned, other suitable inorganic
ri..l~s Ill.~y l)~ lL):l.iLi.~d l)y:
~ Jl~s~ 04)
Anhydrite (CaS04)
Apatite (CaF2.3Ca3P208)
Augite (CaMg(SiO3)2+(Mg, Fe)-(AlFe)2SiO6)
Barysilite (Pb3Si207)
Biotite ( (K,EI)2(Mg, Fe)2(Al, Fe)2(SiO4)3)
Bornite (FeS.2Cu2S.CuS)
Celestite (SrS04)
Chalcopyrite (CuFeS2)
- Chiolite (5NaF.3AlF3)
Clinochlorite (1I8Mg5A12Si301~)
Crocoite (PbCrO4)
Cryolite (Na3AlF6 or 3NaF.AlF3)
Cryolithionite (3NaF.3LiF.2AlF3)
Cuprite (Cu20)
Eulytite (3Sio2.2Bi203)
Ferberite (FeW04)
Forsterite (Mg2SiO4)
Galena (PbS)
Glauberite (Na2S04.CaS04)
Halite (NaCl)
Lanarkite (Pb2S.(S04) )
Laurionite (PbC12.Pb(OH)2)
Leadhillite (Pb(OH)2.PbS04.2PbC03)
Lepidolite (KLi[Al(OH, F)2]Al(SiO3)3)
Litharge (PbO)
Matlockite (PbO.PbC12)
Mendipite (2PbO.PbC12)
3 0 Mimc ti te ( 9I'bO . 3As205.PbC12)
Monetitc (IlCaI'04)
Nantokite (CuCl)
Parisite (CaO.2CeOF.3C02)
Phlogopite ((K,ll)3Mg3Al(Sio4)3 (+Na, Fe, F) )
Powellite (CaO.MoO3)
~1~6~3S
ryromor~ itc ( r~bcl2 311~3(I~1)2)
Pyrr~ll~ite (F~`5S62F~16S17 )
Scheelite (CalYo4)
Stolzite (PbO.WO3)
Strontianite (SrCO3)
Sylvite (KCl)
Thenardite (Na2SO4)
Triphylite-lithiophyllite (Li(Fe, Mn)PO4)
Vanadinite (9PbO.3V2O5.PbC12)
Villiaumite (NaF)
Witherite (BaO.CO2)
Wollastonite (CaSiO3)
Wulfeni-te (PbMoO4)
Xenotime (Y203 . P205 )
The powdery inorganic materials may be crystalline or amorphous
in structure as long as they fall within the hardness range for
their individual particles and are able to maintain stability with-
in the desired temperature range. The particle size of these
powdery materials is not particularly critical. The particle sizes
normally employed for powdery fillers in brake materials are satis-
factory but wide deviations therefrom will have no substantial
effect on performance. Particle sizes from 0.5 to 100 microns
may be used and a particular range of sizes may be employed at the
option of one skilled in the art -to facilitate ease of processing
and the attainment of a uniform product.
To prepare the compositions of the inventio.n, 10 to 30~ by
weight preferably about 15 to 20% by weight of the thermosetting
resin, 5 to 25% preferably about 10 to 15o cashew nut particles,
from 5 to 15% preferably 6 to 12 1/2 % of the non-asbestos fibers
and from 20 to 60o preferably about 25 to 35% of the inorganic
powder are blended in the usual fashion for manufacture of
friction materials. ~fter thorough blending the mixture may
then be placed into the appropri.ate molds ancl cured ullcler heat
and pressure in the usual fashion. If desired, after curing
and dcmoldincJ are completed, the pads may be trimmed of ally e~-
l~lç~¢)~
cess material l:o the exact shape desired by standard techniques
well-known to anyone in the art.
It is contemplated that the finished pads will then be
fastened onto standard brake shoe members by conventional means,
either by integral moldin~, riveting or bonding with a rubber
solvent based adhesive, as desired, for installation into con-
vention brake assemblies.
One skilled in the art will recognize that while the afore-
mentioned compositions represent basic compositions suitable for
use as a friction pad, various other additives co~nonly used in
known friction compositions may also be incorporated. Among
these are such typical additives as barytes which may be added
for their polishing action on the metal braking surface, rubber
particles which may be incorporated for their noise resistance,
metal chips optionally included for their additional friction
imparting ability, and molecular sieves, as illustrated in U. S.
Patent 3,916,062, which may be employed for their ability to
impart fade resistance. Such materials will be employed in con-
ventional proportions well recognized in the art.
One skilled in the art will also recognize that, in addition
to single powdered inorganic compou~ds, for replacement of the
asbestos fibers one may incorporate mixtures of two or more of
these compounds.
Amongst the additives which may be included in the basic
compositions are by weight:
from 3% to 10~ rubber particles,
from 10% to 30% barytes,
from 1.5% to 6% metal particles,
from 0.~% to 2% carbon black,
from 0.5~ to 5% hexamethylene tetramine, and
from 0.5% to 5% calcium carbonate.
B -9-
~1¢6~9S
In addition there may be present from 10~ to about 15
of an unloaded molecular sieve.
In accordance with a specific teaching of the present
concept the composition may comprise the following by weight:
from 29% to 32% calcium carbonate,
from 3.5~ to 4.0% fluffed fiberglas floc, average fiber
length from about 1/8 inch,
from 3.5 to 4.0% fluffed fiberglas floc, average fiber
length from 1/4 inch to 1/2 inch,
from 15% to :L8% thermosetting phenolic resin,
from 9% to 12% cashew nut particles,
. from 0.6 to 7.5% rubber particles,
from 17~ to 20% barytes,
from 2.5% to 4.0% zinc metal chips,
from 0.5% to 1.5~ carbon black,
from 1.0% to 2.0% hexamethylene tetramine, and
from 1.0% to 2.0% calcium aluminate.
To the above composition there may be added additionall~ from .,
3.0~ to 4.5% of an unloaded molecular sieve.
: As used herein and in the appended claims the expression
"without substantial chemical or physical alteration" means that
- substantially no change in the chemical structure of the compounds
occurs such as, for example, oxidation, reduction, or significant
loss of any particular element or elements in the molecular
formula, and that the crystalline structure, if any, or other
spatial arran~ement of the various atoms in a particular solid
is essentially unaltered,
The following Examples further illustrate the best mode
contemplated by the inventor for the practice of his invention.
-~a-
B
11~6~`~95
EX~MPLI~S 1 ~ND 2
Sample asbestos containing disc brake pads to be used as
controls in a series of comparative tests were prepared as
follows: .
A Patterson-Kelley blender equipped with a whirling agitator
is charged with asbestos, phenolic resin, cashew particles, rubber
particles, calcium aluminate, barytes, zinc chips, hexamethylene
tetramine, carbon black, and 3A molecular sieves in proportions
taught by U. S. Patent 3,916,062.
.
.
-10
r~
S "~
Tl~e b.l.eni~C!r is tUIIIblC~d l:or 30 secon~3s, aEter whicl~ e
~gitator is turned on and the mixer run for all a~kli~ionai 4.5
minutes. The mixer is then discharged into a container.
Disc brake pads are molded from the mixture by placing a
quantity in a mold and treating at 1200 psi with a 10 second
dwell time in the mold. The sample is then cured at 300F for
15 minutes at 4000 psi with degassing at the end of one minute
and at the end of 2.5 minutes. The resulting disc pads are then
ejected from the mold and allowed to cool.
The edges of the sample are then trimmed to remove excess
- material and the samples post-baked while under constraint in a
forming container to prevent swelling for a period of 8 hours.
The temperature is increased linearly over a period of 1.5 hours
to 400F and then held at that point for the remaining period.
1~ After cooling the samples are released from the cons-training form.
Example 1 represent asbestos pads prepared in the laboratory,
Example 2 represents identical pads prepared in a production plant.
The pads so fabricated are then fastened on appropriate metal
backing plates in conventional fashion and installed in a full size
1976 Mercury Sedan for road testing. The testing procedure follow-
ed lS a simulated drive on Whitehorse Mountain.
1. The effectiveness of the brakes is determined at 30 and
60 miles per hour (m.p~.h.) with 200F being the limit for the
hottest rotor or drum.
2. The brakes are cooled at 150F hottest rotor or drum and
the starting temperatures are recorded.
3. The recovery is checked by stopping 30-0 m.p.h. at 10
feet per sec in gear.
~. Three warm up stops 55-5 m.p.h., at 15 feet per sec in
gcar.
5. Seven snub stops 50-40 m.p.h., a-t 10 fect per sec2 in
gear and the temperature recorded.
6. The Eirst fade stop is conducted 55-0 m.p.h., at 15 feet
per sec in gear and the temperatures are recorded.
;q ~9~
7. Sevel~ more snub stops similar ~o thc ~irst ;et ar-~
performecl.
8. The second fade stop similar to the first is performed
and the temperatures are recorded.
9. Four more snub stops similar to the first set are per-
formed.
10. A third fade stop similar to the earlier two is performed.
11. Seven more snub stops similar to the first set are per-
formed.
12. A fourth fade stop similar to the earlier three is per-
- formed.
13. The vehicle is driven at 40 m.p.h. for 0.4 mile. The
maximum temperatures are recorded.
14. The vehicle is further driven at 40 m.p.h. and the
temperatures recorded 0.2 mile before the recovery stop.
lS. A recovery stop is performed 30-0 m.p.h. at 10 feet per
sec ln gear.
16. Items 14 and 15 are repeated until a total of eiyht re-
covery stops have been completed and the temperatures are recorded.
17. A fade stop check is then performed 55-0 m.p.h. at 15
feet per sec2 in year.
18. Steps 2 throuyh 17 inclusive are repeated for a total of
3 laps.
19. The effectiveness of the brakes is checked at 30 and
60 m.p.h. with 200F for the hottest rotor or drum.
20. The brakes are then inspected and wear measured.
The lininys are evaluated duriny the test for noise and
rubber banding or a scale of 10 no noise to 0 totally unacceptable,
and of course, for fade and stopping ability. At cornpletion of
the test the brakes are examined for pad wear and condition and
rotor condition. The results so obtainecl are sun~arized in Table
I.
11q~6~)~5
.
TAL31,~ I
.
r~x. l ~x. 2
_ _
Noise and Rubber None None
Banding
Lining Condition Dull Mottled Light Spewing
Light Spewing
Rotor Condition 70-85% Transfer of lleavy Texture
Material
Maximum Wear (in) 0.078 0.023
Test Evaluation Slightly over effective, Good performance,
all other phases of test good wear and rotor
satisfactory conditioning
.
~ -1.3-
t'
q ~S
EX~MI.'LI,.S 3 r.L'IIRU 6
Followinq a procedure analogous to that described in
Examples 1 and 2 the ingredients shown in Table II are formulated,
and cured into disc brake pads.
30 .
q~c~
T~ULE II
E~am~le No.
Quantity (p.b.w.)
In~redien _ 3 4 5 6
Zinc Oxide 40 40 40 40
Thermosetting Phenolic Resin23 23 23 23
Fiberglass 5 -- -- --
*Fiberglass (fluffed before -- 5 5 5
addition)
Cashew Nut Resin Particles 14 14 14 14
Calcium Aluminate 2 2 2 2
Barytes 15 15 15 15
Zinc Metal Chips 4 4 4 4
Hexamethylene Tetramine2 2 2 2
Carbon Black
3A Molecular Sieves 5 5 5 5
Rubber Particles 13.8 13.8 13.8 13.8
*Cut floc tumbled for a short period to render it fluffy.
All cures were at 300F for 15 minutes in the mold and then
for 8 hours at 400F for the post-cure conditioning.
When tested as described for Examples 1 and 2 the results
obtained are summarized in Table III.
_ 1 ~ _
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U~
a)ra ~ x ~
X
a a) o
~D ~ m ~ . I J
~) h C ) ~ S:
u~ 3
~ o
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~ ~ ~ ~ ~ I
l-- ~ o ~ O
.,,
~ U~ ~
U~
Q) ~5 ~ x
U ~
u~ ~ ~ o
-~1 ~ ~ c
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o ~ o I ~ o a~ o o
3 ~ O
E~ .
x
v~
a~
o ~ ~ ,1 Q E~
1~ -rt I ~ r~
~ f~ O R Q,
u~ ~ h ~v~
H
H H O 11~ 0 3o~ ~1 ~ U~
H ~ ~I R O o
~-1 ~ O ~ ~ O O ~I h ~ O 0 ~1
H
~ a~
u~ ~ ~ ~ 3~J
a) ~ ~ o ~ ~ o
O ~
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H ~ ~ R O o ~ ~ ~ R O ~a
o ~ ~ o o a.
U~ r~ CO H ~ ~ ~
U~ .IJ
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0 ~ r~ ~
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h
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~ X u~
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llSf~9S
EX~II'LI.~,S 7 AND R
Bra~e pads are formulated and cured as in the previous
E~amples. The proportions of the ingredients used are shown in
Table IV.
GO
`,.,? ~.1~6~)9S ~i@\
TABL,E IV
Example
IngredientsQuantity (p.b.w.)
Zinc Oxide 24 --
S Fiberglass (f:luffed) 5 5
Thermosetting Phenolic Resin 23 23
Cashew Nut Resin Particles14 14
Rubber Partic:Les 13.8 13.8
Calcium Aluminate 2 2
Barytes 31 55
Zinc Particles 4 4
Hexamethyiene Tetramine 2 2
Carbon Black
3A Molecular Sieves 5 5
- Cure and post-cure conditloning are as described for
: Examples 3-6.
Testing is as described for Examples 1 and 2. Results are
. summarized in Table V.
~ ~ .
-25
. ,,~
:
4~
T~13L~ V
Example
7 8
Noise and Rubber ll Instances 13 Instances
Banding Squealing Rubber Banding
Worst rating 7 Worst rating 7
3 Instances
Squealing
Worst rating 8
Lining Condition Heavy Cracks Heavy Cracks
Rotor Condition Light Score 50~ Polish
50~ ~ieavy Texture
- Maximum Wear (in) .041 .150
Test Evaluation Slow recovery, some Poor pad strenyth,
noise, light rotor high wear, frequent
score banding, high com-
pressability
--19--
( )C~S
E~A~IPLFS ~ TIIR[J 13
.
Brake pacls are formulatecl and cured as in the previous
Examples. The f ormulations are given in Table VI.
TA~I.l. VI
Example
Quantity (p.b.w.)
Ingredient 9 10 11 ].2 13
Zinc Oxide 27.5 27.5 27.527.5 27.5
Fiberglass (fluffed) 5 5 5 5 5
Thermosetting Phenolic Resin23 18 23 23 23
Cashew Nut Resin Particles 14 14 14 14 14
Rubber Particles 13.8 13.8 19 19 14
Calcium Alumi:nate 2 2 2 2 2
Barytes 27.5 27.5 27.527.5 27.5
Zinc Metal Chips 4 4 4 4 4
Hexamethylene Tetramine 2 2 2 2 2
Carbon Black
3A Molecular Sieves 5 5 5 ~ S 5
Chunky Graphite ---- ---- ---- ---- 2
Pads are cured and conditioned as described for Examples 3
thru 6 and tested as described for Examples 1 and 2. The results
are summarized in Table VII.
.
11t16;~9~
~n
a).,l ~
h h O
O
, ~ ~ O ~
r`~ I I I h
~, , , I I ~ a) ~
n ~ rv O
h
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a) ,l rn
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r4
o a~
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I I I I~ ~ ~
u7 ~ a~ o
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E~ ~a ~ Il,
`;
~, ~
. ~ ~ I a) ~,
O ~ ~ ~a
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~ I X rJ r
a) ~ I O ~ ~ ~ ~ R.
~a ~a ~ D rn E~
h a) ~ ~1 o O ~1 ~a
~ ~ ~ ~ m E~ u ~ ~
~a
~D
rn ~
rV 1~ 1 ~ X h h
o ~rl 3 ,1 0 ~a O O
~ rv R. ~a
H Ord ~ la ~ h :~ h~ o o ~a a
H ~1 .~ rn ~ ~ ~a ~ ~a ra h h 3 a)
u~ ~ ~ Q) ~ h ~1 a) ~a I
~a ~ ~ ~a ~ ~ rn u~ v h
~: H rv ~r) ~ rV ~ h O
h ra ~ ~ o\ ra ~D rn ~ 3 ~ o r)
o ~v ~ o h ~v ra 0-~ v
. ~; ~ ~ u~ ~ ~- 1 ~ ~ E~ E~ rn ~:: ~ rn ~
~: .
h ~
rn ~ rn ~ ~ rV
. ~v ~ ~ rv O
U ~ ~ V h rl ~v
~ 0 ~ rn~ ~ ~: ~ h
o~ra ~ ~ h ~ 0 ~ O ~ ~
~1 h ~ ~ ~I rv E~ rl ra
rn ~ ra o ~ S~ ~a ~ rn
~ ~a ~ P, ~ o ~1 ~v
H rv rn ~ ~orv ~ h ~ rn r~
::5 h t~' dP o\ 1~ t) h 0 ~- 1 0
r~ r o ~ o o oX tv ~v O O h
rn ~ r Z rv
O
-,~ O ~ O
~ ~1 -~1
~ ~ h ~
ara
O
C~ o ra
~J ~ ~
tv t:: h ~;
rn 1 o rl ~
~ ~ ~ Xrn
O ~1 0 0~v
I;`X/~IPI,F.S 1'1 TllI~U 1~
Brake pads are formulated and cured as in the previous
Examples. The formulations are shown in Table VIII.
.
'
~"'"r '' !'~
11¢~6~
rr~BLI. VIII
Example
Quantity (p.b.w.)
Ingredien_ 14 15 16 17 18 l9
Zinc Oxide 27.5 5027.5 27.5 27.5 27.5
Fiberglass (fluffed) 10 5 5 S 10 10
Thermosetting Phenolic Resin 23 15 23 23 23 23
Cashew Nut Resin Particles14 14 14 14 14 14
Rubber Particles 14 13.8 14 14 14 14
Calcium Aluminate 2 2 2 2 2 2
Barytes 27.5 15 27.5 27.5 27.5 27.5
Zinc Metal Chips 4 4 4 4 4 4
Hexamethylene Tetramine 2 2 2 2 2 2
Carbon Black
3A Sieves 5 5 5 ~5 5 5
Cryolite --- --- 5 --- --- ---
:
. .
Cure and conditioning are as described for Examples 3 through
6 and testing is as described for Examples 1 and 2. Results are
summarized in Table IX.
' '
~ 25
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)~ C~
CO
U)
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aJ rl a) ~ aJ
O tJ~ ~J X ~ r~ rC h
~ 0 ~1 tn t~ O
cc ~ I h ~) a
~) I~~ Q ~ h ~ u~ u~
u~ h
co ~J h ~1 0
:~ h ~ o~ ~1 u~ o ~ ~
~t O (~ - L() ~) a) O a~) O
E-~ Q r~ h
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O G) r~t
3 X ~ ~ X
r` a) h
~i a) ~ (~ a) ~ a) h
~ u~ Q h
o ~ u~ r I h
z; ~ ~-rl Lr~ ~ rl h a) O
~ O ~
a) o ~ oa) (~ (I) a) Q-r~ a)
Q) ~ h ~ ~
Q~
~ CO
X U) ~
a
U -1 3 ~
~; ~-IJ a) ~t U~ ` h
td ~ tr~ rl u) a) U
~1 ~ ~1 ~ u~ td ~ r-j X ~ td
tn~1 a) ~ o
~: td ~ I td O a) u~
X H o U) S I ~ o ~ tn r~ ~t
,~ t~ ~I td JJ ~1
Lr~ ~ O ~ Lt~ o U~ ~ .C a o
. ~I tJ~ ~I td ~ t~
~ .
m
~ o~ l
E~ ~ ~a
~ r~ a) a).~: >t
t~ Q, U h b' h
a) ~ I ta 0 ~1 ~ tn o
U ~ 1~ 3 ~ '~ ~ o ~ ra ~ Q,~
~: ~ td a) .C h r~ ~1 0 t~l td U
t~ td - r~ ~ ~ ~ O ~I td
r-j .~ tJ) tn td td ~ In 4~
td -1~ ~ XtJ~ h ~ r:n
~: a) rn ~ U t~ td h 0 h rJ
H ,~ h ~ ~ ~ td o~ cr~ ~) .IJ td ~ t~
t~t O t~ l h O ~1 a) u~ tl) O td
r1 ~ U CO P~ ~ 3 h ~ u~
CO
u~
C) -r-l 3 !n
U t~ a) ~>t ~ h '~
r~ > rl ` t~) O
~r td ~ u) td ~ ~ tn,~: rd
td X ~ t:n ~n ~
~n ta ~ ~r~t ~ r~U~ h O a) O
C C) t n td tn ~
H r~ ~1 td ~ ~ O~o.~ ~ td r,^, U
~t O ~1) C r~ O O r-l ,C al td
cr~ tn 3 ~ r~ C~ td r~
h r. r~
U O r.rl r~
Q rl O O
Q ~J - rl r~
" ~ h J~
td
a
O r~ ~ ~
U O td
td ~ U
r~ ~ ~ r~
(l) r1 r~ ~ E.
~1~6~)~S
E.Y~1}']:,13S 20 'rlll~U 26
Brake pa~s are formulated and cured as in the previous
experiments. The ormulations are shown in Table X.
;
:~:
.
t~S
.r~s.r.,l; x
Example
Quantity (p.b.w.)
Inyredient 20 21 22 23 24 25 26
Zinc Oxide 27.5 27.5 5027.5 45 5527.5
Fiberglass (fluffed) 7.5 7.5 5 5 5 5 7.5
Thermosetting Phenolic 23 23 15 23 15 15 23
Resin
Cashew Nut Resin 14 14 14 14 .4 14 14
Particles
- Rubber Particles 14 10 8.8 14 8.8 8.8 8
Calcium Aluminate 2 2 2 2 2 2 2
Barytes 27.5 27.5 1527.5 15 1527.5
Zinc Chips 4 4 4 4 4 4 4
Hexamethylene Tetramine 2 2 2 2 2 2 2
Carbon Black
3A Molecular Sieves 5 S 5 5 5 5 5
Cure and post-cure conditioning are as described for Examples
3-6. Testiny is as described for Examples 1 and 2. Results are yiven
in Table XI.
S
cn ~1
tn b' I h
a)~ ~ tu~
S~ h ~ rl a
I ~ ~5 n~
ln n~ n~
~1~ h tJ ,~
t) Q ~ ~ ~ rl tU ~1 Rl ~ tU
F~ ~l tl) ~ tu ~ tu a~ ~ a) o ~a tn
r~ 1~ t~ R, n~ 4~ ~ tU ~ tn
t~l~- ~J ~ ~ tn tn
m ~r~ ~n ~
nl I .-1 ~ "~o c~ ~n ~ S ~ a) a) ~n
,~ :~ tn n~ ~ rd ~
h r~ :~ a tu O O O tU ~ O.C a) ,~ ol
O ~ h .q ~ ~ -~
a~ .,J ;,
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: ~ ~ n~ O
ln ~rl (n
tU rl~ tn ~a ~
o ~ ~aJ x tu a
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t~ ~ r~ ~ rC h
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a tU-rl h n~ h O X
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.
,~
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o tU X (U tU'~J ~ O tU
t~l 1~ tU tl) tn h 41 h au s s
O ~ n~ 4~ tn ~ tn
Z r~-r~-r~ C ~ ~ tU ~)
tn u3 ~ ,~ tn x .:: tn h
tU oP ~ 3 tn ~a ~ '~ ~ RJ
o o o au h ~l na (U
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.
S
a
tn
rl
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tU
:r
tn
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. ~- ^ Z ~ ~ ~ Q
U~ .C ~ 5~ (11
a) a~ a) ~1 rl U~ O a
O ~ 3 ~a) ~ u~a
Q ~: C ~ U
E~ 10 O '~ 0 ~
~ ~ ~ V~ X
X u) rd ~ Q u~
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H ~ ~1 ~ o~ Lt~ J E~ Q
cr o a) ~ o ~ ~ o ~ ~ a
.' ~ H ~ a) ~
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. s ~ a) td
. ~ ~ ~ a~
~:
::
.. ~ ~ ~ a
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a) -,( ,~ u
O ~J) ~ 3 ~ o L~
a) o
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Q ~ a)
u~ ~ a) ,c
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H ~ U~ O ~ a) ~
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117 ~ O t)
~n
.~
a
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Q ~,1 0 ~ O O
Q
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rl rd (d O
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u o (a
o ~ ~
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o ~ ~1 o ~ a
z m
6~ ~9~
~XAMI'LES 27 TIIRU 29
Brake pads formulated and cured as in the prior Examples.
The formulations are shown in Table XII.
,
, .
. .
` 10
~: 15
~"
~. .
i,i :
~: ~
: 25
?
P~S
T~BL,~' XII
Example No.
Quantity_~p.b.w.)
Ingledient 27 28 29
Zinc Oxide 27.5 50 50
Fiberglass (Fluffed) 7.5 5 5
Thermosetting Phenolic Resin 23 15 18
Cashew Nut Resin Particles 14 14 14
Rubber Particles 10 3.8 8.8
- Calcium Aluminate 2 2 2
Barytes 27.5 15 15
Zinc Metal Chips 4 4 4
~; Hexamethylene Tetramine 2 2 2
Carbon Black
3A Molecular Sieves 5 5 ' --
~'
Cure and post-cure conditioning is as described for Examples
3-6. The pads so produced are mounted in the usual fashion on a
standard 1976 Mercury Sedan as in the prior Examples and tested
for fade resistance as follows:
1. 3 Successive stops are made 30-0 m.p.h. at 10 feet per
sec , in high gear, 190-200F one brake temperature maximum.
2. 10 stops to check fade are made 60-0 m.p.h. in high gear
with a 4 mile interval at 15 feet per sec and 140-150F one brake
temperature maximum for 1st stop.
3. The car is driven at 40 m.p.h. cooling speed for one mile
after the last fade stop.
4. 5 stops from 30 m.p.h. at 10 feet per sec2 in highest gear
are performed.
5. The brakes are then burnished by 35 stops from 40 m.p.h.
at 12 feet per sec2 with 250 1 brake temperature or 1 mile maximum
in gear.
6. Steps 1, 2 and 3 are then repeated.
7. The brakes are then checked for wear and condition.
The results are summarized in Table XIII.
~ ~ ~r~
11~6q.~
~BLI;: XIII
Example No.
27 28 29
Noise and Rubber 4 Instances 19 Instances
Banding rubber band- squealing
ing-worst worst rating 9
rating 9-4 in- 2 Instances
stances squeal- wire brush
ing-worst ra-ting wound-worst
: 9-1 Instances rating 9-3 in-
.: erratic brake stances-pinch
.: out squeal
`~ worst rating 9
.:
` Lining Condition Outboard broken Light spewing Med. spcwing
- Inboard cracked Light pitting Light pitting
Rotor Condition 30% Polish 70% Satin 50~ Satin
` 70~ Transfer 30% Polish 50~ Medium-
~- heavy transfer
. .
;: Maximum Wear (in) .252 .062 .100
.
:~ Test Evaluation 10 Stop fade OK
Pedal floored 9-
15-stop fade,
~: lining badly
broken and
cracked, test
POor
: .
-
` ' .
-32-
6~ V
~X~MPL~S 30 TIIRU 39
Brake pads are formulated and cured as in the previous
Examples. The formulations are shown in Table XIV.
:`
~ 20
:
cs~ o I If~ ~n~r co ~ n ~r ~ r-l ~n
(~ In I ~ r-l r-l ~ r-l
co o I Lnc~ ~rcO ~ In ~r ~ r-l Ln r~~
~ I n I r--lr~
ct~
I O I Ln m ~00 '::t' Ln ~r t~l r-l Ln
t~ Ln I r-l r-l ~ r-l I
C~
I O LnLn ~r~ ~ Ln ~r ~ ~ n
~) I L~ r-l r~ ~ r~l
_
. 3 Ln O I Ln Ln ~r O;) N Ln ~ N r-l O
O ~ ~ Ln I r~
~Z Q~ CO
aJ _
~ ~ ~r o I m Ln ~ ~ ~ Ln ~r ~ ~ Ln
X ~) ~ Ln I r-l r-l ~ r~l
~Ll 1~ Ot~
O;
n Ln In Ln ~r co ~ Ln ~ ~ r~l Ln
~1 ~I 01 r-1 r-1 r--l I
r
~> ~ o I Lnco ~rco ~ Ln~r ~ ,~ Ln ~1
H 1~1Ln I r-l r-l ~ r~l
X C~
~ r-l O I LnLn ~ I Ln~ ~ r-~ Ln
E-~ ~ Ln I ,-1 r~l ~1
CO
O In I LnLn ~r o ~ Ln~r ~ ~ Ln
r~ ~r I r-l r lr-l r-l I
~n ~n
a) a)
r1 ~ - rl
,~ h E~
~ O ~ ~ ~n
~ h
Lj~
4~ n ~ ~n a~ a
~) .~ Lnr~l~ rl
a) o ~ ;r~ ~ C~
_r~ '~ rl ~) ~ ~) U
(I)r~ tnI J ~ h ,~ r-l
a) ~ h~ ~n
r~ ZP~ U a
n ~ Lna) ~ ~ ~
~: O ~ ~ O:~ h ~ aJ ~ "
h ~a)QJr~ ~) F
U ~ QC) :~U Q~
r r l .naU~n Q ,~h ~ X h rd
t 1 C) ,tL~ [--~ C~ 1~ CJ 1~ N ~ C~
~1~61 ~;ltj
Tlle pads are cured and post-cure conclitioned as clescribed .in
Examples 3-6. Testing for l.xamples 30, 32-37 and 39 is as de-
scribed for E:xamples 1 and 2. Examples 31 and 38 are tested as
for Examples 6.
S The results are summarized in Table XV.
-25
11~'6~t~S
CO
~ ~ tn
a) 1 rl ~)
3 ~ u~
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u~ 1~ r~ ) r~
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U)
o
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r~
3 X
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tl~ ~ U~ O
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ll~S~iq~
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H ~1 H ~ ~o\ ~1 ~D
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o
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a) ~ . , 0~O
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X ~: . R 3 ~i,1~ 1
r ra ~::a) I ~' ~ I 1--
F~ U) (11 ai
~ s:: a) R ~ a) O
a~ H ~ R P~ 5~ ~ ~ o\ ~ ~
~¢ ~ ~ ) o o
. ~ h H U~
Ul
--~ X
O
~ 1 a
u~ ~ u) ra Q, ~-~
a)-rl a
t~ h t
Q
~ara
a) a) r~
a)
~ ~ ~ R ~n
H ~I H R o\ ~
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a) o ~ ,,
R ,1 0
R ~ ,
~a a
~a o ~ ~:
o
a~
rl o ~1
X
6q~
T~XI~MPI,~S 4 0 ~ U 4 8
Brake pads are formu1ated and cured as described in the
previous Examples. The formulations are as given in Table XVI.
n o co ~ co N I O ~ N ~1 n I I
N '~ ~ ~n ~r N ~ I I
o n n I ~r ~ N
3 I o Ln n I n ~ o~ N L ~ N ~1 n
o ~
a~
E ~ ~ o n ~ I n ~ co N n ~ ~ ~
X .~
~ ~- o I n I ~ ~r co N L ~ N ~ Ln
N
~ .
E~
o I ~ I n ~ c~ N n ~r N ~ LO r-l
o t~ o I n ~r co N ~ n
,_1
v
V
.,1 ~ ~1
~ O r~ E
a) O H ~ ~ ~ ,rVl ~ S C ,!~
r1 ~ h rl .1J _~ a) V ~a
rc~ C) r~ U~rr~
a) rc~ a ~ h
c ~) C~ 0 3 )~ ) c~ r
r~ -rl h rl E~ rl) c) r~ O O r~ r~
r o V V h ~ R V ~ V r~ ~ ~ C O
a ~ rl a) rr~ ~¢ ~ h
'` ~' ll~S6q'~
Cu2'e and post-cure condi.t:ioning are as described for r.Xampl('S
3-6. The pads are mounted in stanclard fashion on a 1976 r~ercury
full si.ze Station Wagon. The pads from Examples 40 through 44,
47 and 48 are tested as described for Examples 1 and 2. The pads
from Examples 45 and 46 are tested as described for Examples 27
through 29. The results are summarized in Table XVII.
- 25
ra ra
a~
F f~;
n ~
~rl r-l~ ln
3 1 rl rl
Q) O ~l ~I r~t
~r ~ n, ~: ~n ~ o
n rt ~
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~ ~a0~O 0~O ~
.t ~ ~n o o
a~
~ ~ ~t
rt rt ( )
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v~ ~ a) o
L!~ ~ I rt ' h
r~ o ~n
.~
U~ rt Ull ~ U)
H ~ ~ ~ 0\ o~ ~
rt ~ a) ~rl ~ Ln h
r~t ~ U~ ~ r't ~ S ~ I~ E~
.'
.
O ~ O ~ rt b~O ~n S~
Z U~. r1 h
O.~1rt ,C rt a)~ rt ln ~.) ,~
a) ~ 1 3 ~ n u~
r-t ~~ ,LI ~ O ~ ~ R ~~ ~ rt rl ~
~J 11~ O ~t U~ 111 h ~ O ~ .IJ ~-t a
~r~ ~ ~ r-t a) ~) h O c (~ O h
r~ ~n C ~ ~ U ~ ~ ~n O ~E~ ~1 rt U~ ~ E-l
X C U ~ n ~n c R ~n I
~t C ~ h r~ R h ~ ~ ~\ `~ \ ~
rt ~ I ~ h O :~ O~ a) rt I n O Ln O
H ~ Q~ ~n t~ ~n R 3 ~ h 3 ~ ~ t
~>
r-l
tl~ ~
1-l (1) U
m l ~ ~
~: tn tn h h
E~ ~ ) U tn
U ~ ~1 X 4-1
~ ~0 ~ ~u C tn
r-l ~ rt
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~ ~ ~ ra ~ ra \ \ ~
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n ,t ~n :~ rt
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rt (I) ~) C tn
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Z U ~> t~
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a) o ~ .rt
R rt O `~
R ~ rl
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ra O C
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u~ ~ ~rl r~
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oo ~ U ~ rd ~
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v a) ~ o ~ o
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æ
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X
o ~ ,~ a
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tJ~ o o
U~ ~ O
H a) r~~ ~ ~R ~ I
H U r~ I r-l - r~
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X ~D t~ ~ h a~ tJ` I O ~ h ';r
. ~ ~ ~, ~ ra
u~ X ~ a
~1
~ H ~I h~ ~J 0 0 ri ~a 0\ ~a ~r
r~; . (U O~ r~ h h ~ O O O
r-l 3 ~ Q
~ ra
r-l a) ~ r~
tJl I I ~) rrJ ~ h
u~ o a
(JJ rl ~ \ Q .IL) ~1
1) r--l ~ rl r~l rl ~) ~
r-l ~i3 I h ~J R ~ r~ ~
h a~ I O (1~ r~
~r~ ~ Q~ a h r~
U~ rl X ~) G) ~ O U~
s~: ~ rn~ ~ r-l r~ rr)
H ~ h~ ~ r~ O~r~ ra o\ o\ r.o
a) o~) r~ h h ~ t~5 r~ I~ )
~3 r~~ 3. 1~ Q, ~ ) ~1 (1-l Q r-l L( ) r.~o -
h ~ _
CJ O ~ ~ rl
Q rl 0
rl
~5 r~ ~) h
~a r~
~a
ra o
o
r~
a) rl ~ h E~
V~ ra r~ ~ rl
r~ ~ ~ ~) X
O r~] rl O , 1
rr~ .:1 r~'
X~MPLE~S ~9 THRU 51
Bra~e pads are formulated and cured as in the prior Examples.
The formulat:ions are given in Table XVIII.
,
6~ S t~
TABL~ XVIII
Example No.
Quantity (p.b.w.)
``5 Ingredient 49 50 51
.
Zinc Oxide -- 10 20
Calcium Fluoride -- 35 25
Fiberglass (fluffed) 5 12.5 12.5
Calcium Carbonate 40 -- --
Thermosetting Phenolic Resin 15 15 15
- Cashew Nut Resin Particles 14 14 14
Rubber Particles 8.8 8.8 8.8
Calcium Aluminate 2 2 2
Barytes 15 15 15
Clay 10 -- --
- Zinc Metal Chips 4 4 4
llexamethylene Tetramine2 2 2
` Carbon Black
~ 20 Pads are cured and post-cure conditioned as described in
~~ Examples 3-6. Testing is on a full size 1976 Mercury Sedan as
described for Examples 1 and 2. Results are shown in Table XIX.
- 25
.
T~BL~ XIX
Example No.
49 50 51
Noise and Rubber 7 Instances 1 Instance 2 Instances
Banding squealing wire brush left pull
worst rating 9 sound rating worst ra-ting 1
1 Instance 9-9 Instances 1 Instance
pinch out xubber band- squealing
squeal-rating ing-worst rating 9
9-l instance rating 7-2
left pull instances
rating 1 squealing
worst rating 9
Lining Condition Med. heavy Med. heavy Med. heavy
pitting-med. pitting-surface pitting and
spewing and cracks
cracks
Rotor Condition 40% Polish 25~ Satin 40% Satin
~ 60~ Satin 75% Polish 60~ Polish
; Maximum Wear (in) .062 .025 .029
~ .
~ , .
~ -45-
E~11'IIE 52
Brake pads are formulated and cured as in the prior Examples.
The ingredients are:
Ingredient ~uantity (p.b.w.)
Calcium Carbonate 40
Fiberglass (fluffed, 1/8 in.)* 5
Fiberglass (fluffed, 1/2 in.)* 5
Thermosetting Phenolic Resin - 22
Cashew Particles 14
Rubber Particles 8.~
Barytes 25
Zinc Metal Chips 4
Carbon Black
Hexamethylene Tetramine 2
Molecular Sieve 5
Calcium Aluminate 2
*Average fiber length
After cure and post-cure conditioning as described in
Examples 3 to 6, the pads are tested on a full size 1976 Mercury
Sedan in a modified procedure analogous to that described for
Examples 27 through 29. In this test the fade stops in step 2
are increased to 20, and step 5 is omitted. The results are as
follows:
Noise and Rubber Banding 3 Instances rubber banding, 1
instance wire brush on second
series of fade stops, 13 in-
stances smoke and odor, 2 light,
2 heavy and 4 instances 1st series
Lining Condition Pads were very ligl~t sur~ace
cracked
Maximum Wear (in) .041
Comments Substantial improvement over
previous ~ormulations
-~6-
~1~6~9S
L~-~r~ s 53 - ~
Com~ound the in~redients shown in T~ble XX in a fashion
analogous to t:hat described in the prior examples.
-47-
q~9S
co ~r
n
~r
~ .
.
. . ~ ~r
`~' Z ~ LO
~` ~ _
. ~ ~
~ ~ .~ U~ ~
: X ~ U~
~` O'
~r ~
U~
"~-
N
:. ~ ~
X . ~r
,_~
m
:: .
:
.
~ ~ ~ .
-1 3
S
S
a) ~ o ~H
O I ~ h S~-rl q) vl ul o
~ x ~ o a) a
$ 1 h
1 o a) o
h ~ 3
O ~1 ~ .1 ~ s ~ ~ o u~ a)
O h O ~J O ~10 a) ~:: ` O ~ ~1 ~1
1 s ~1 s :~ ~s
a) ~ a) ha) h ~ X ~1 ~1 ~ ~ S
S :~ S O ~ O S ~
11(36~
C~ ~
~a
[~ o u~ u~ u~
u~ ~;r
co ~a -a
O Q ~3 o u~ m~r co u~ ~ u~
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