CA1148708A - Process for manufacturing a glass fiber friction article - Google Patents
Process for manufacturing a glass fiber friction articleInfo
- Publication number
- CA1148708A CA1148708A CA000333649A CA333649A CA1148708A CA 1148708 A CA1148708 A CA 1148708A CA 000333649 A CA000333649 A CA 000333649A CA 333649 A CA333649 A CA 333649A CA 1148708 A CA1148708 A CA 1148708A
- Authority
- CA
- Canada
- Prior art keywords
- composition
- friction
- blending
- minutes
- briquettes
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- 239000003365 glass fiber Substances 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 157
- 239000000463 material Substances 0.000 claims abstract description 42
- 238000002156 mixing Methods 0.000 claims abstract description 38
- 239000002783 friction material Substances 0.000 claims abstract description 37
- 239000003607 modifier Substances 0.000 claims abstract description 19
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 12
- 239000005011 phenolic resin Substances 0.000 claims abstract description 12
- 239000004615 ingredient Substances 0.000 claims description 16
- 239000004484 Briquette Substances 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 239000011230 binding agent Substances 0.000 claims 9
- 238000000465 moulding Methods 0.000 claims 4
- 238000007731 hot pressing Methods 0.000 claims 1
- 238000003825 pressing Methods 0.000 claims 1
- 229920005989 resin Polymers 0.000 abstract description 4
- 239000011347 resin Substances 0.000 abstract description 4
- 229920001187 thermosetting polymer Polymers 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 description 26
- 239000010425 asbestos Substances 0.000 description 22
- 229910052895 riebeckite Inorganic materials 0.000 description 22
- 239000000835 fiber Substances 0.000 description 20
- 239000011521 glass Substances 0.000 description 12
- 239000002245 particle Substances 0.000 description 6
- 229910001018 Cast iron Inorganic materials 0.000 description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000002557 mineral fiber Substances 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 244000226021 Anacardium occidentale Species 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 235000020226 cashew nut Nutrition 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 235000014571 nuts Nutrition 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000001627 detrimental effect Effects 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000012943 effectiveness check Methods 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000008240 homogeneous mixture Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000004816 latex Substances 0.000 description 2
- 229920000126 latex Polymers 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 238000004513 sizing Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 241000950314 Figura Species 0.000 description 1
- 229910001260 Pt alloy Inorganic materials 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- 235000012255 calcium oxide Nutrition 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000010459 dolomite Substances 0.000 description 1
- 229910000514 dolomite Inorganic materials 0.000 description 1
- 238000007580 dry-mixing Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000011152 fibreglass Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 231100000206 health hazard Toxicity 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- -1 ltmestone Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 230000013011 mating Effects 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000006060 molten glass Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16D—COUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
- F16D69/00—Friction linings; Attachment thereof; Selection of coacting friction substances or surfaces
- F16D69/02—Composition of linings ; Methods of manufacturing
- F16D69/025—Compositions based on an organic binder
- F16D69/026—Compositions based on an organic binder containing fibres
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Medicinal Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Polymers & Plastics (AREA)
- General Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Braking Arrangements (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
- Casting Or Compression Moulding Of Plastics Or The Like (AREA)
- Moulding By Coating Moulds (AREA)
Abstract
ABSTRACT OF THE DISCLOSURE
A process of manufacturing a composition of materials reinforced with glass fibers for use as a friction material article requires the blending of a mixture of glass fibers, friction modifiers and a thermosetting phenolic resin until the individual filaments that make up the glass fiber bundles are separated and are uniformly distributed throughout the mixture to produce a bulk density of between 0.1 - 0.6 gm/cc-3.
Thereafter, the mixture is placed in a mold to form briquettes. The briquettes are hot pressed to establish a preselected density and shape before curing the thermosetting resin which thereafter holds the filaments and friction modifiers in a fixed relationship.
A process of manufacturing a composition of materials reinforced with glass fibers for use as a friction material article requires the blending of a mixture of glass fibers, friction modifiers and a thermosetting phenolic resin until the individual filaments that make up the glass fiber bundles are separated and are uniformly distributed throughout the mixture to produce a bulk density of between 0.1 - 0.6 gm/cc-3.
Thereafter, the mixture is placed in a mold to form briquettes. The briquettes are hot pressed to establish a preselected density and shape before curing the thermosetting resin which thereafter holds the filaments and friction modifiers in a fixed relationship.
Description
` - 1148708 BACI~G~OUND OF TIIE INVENTION
Organic friction material compositions currently used in clutch and brake linings of vehicles must be capable of withstanding the severe operating temperatures and dynamic . pressures experienced during repeated applications. To pre-':`.
vent a deterioration in performance and physical degradation during such applications, the linings are normally reinforced by asbestos fibers randomly dispersed throughout a resin matrix. However, recent medical evidence indicates that asbestos fibers can cause health hazards for people exposed thereto during the manufacture of clutch and brake linings.
Unfortunately, because of the presence of fine diameter asbestos fiber during the manufacture of brake lining using asbestos fiber, a portion of the asbestos often becomes air-borne in quantities that exceed the exposure standard of ~ .
asbestos fiber in the United States as controlled by the - Occupational Safety and Health Act of 1970. Furthermore, mechanics relining the automotive brakes are also exposed to some quantity of asbestos from the linings.
In an effort to reduce the environmental contamination by the asbestos fiber and thereby continue the manufacturing of asbestos based organic friction linings, a water slurry process disclosed in Canadian Patent No. 1,105,214 (issued July 21, 1981) has been evaluated. The water slurry can be transmitted throughout a manufacturing facility without contaminating the surrounding environment with asbestos fibers. However, before the friction ma~erial can be cured, the water in the slurry must be removed in order to be assured that any resulting lining has essentially the same operating characteristics as a lining made from a dry mix. Unfortunately, this process adds considerable cost to the manufacturing cost of a brake or c~utch lining, and does not ~ecessarily solve emission problems during finishing and inspection.
. - 2 -~ B ~
dm~
~1~8708 ` In a effort to use readily available materials and the san~
manufacturing facilities, as currently available, it has been suggested that glass and/or mineral fibers be used in place of at least a portion of the asbestos fillers. U.S. Patent 3,967,037 discloses several lining con-positions utilizing glass fiber in place of asbestos. Fr~n experimentation, it has been determined such lining compositions in normal operational , . I
conditions produce brake noise, severe rotor scoring and wear, and poor frlction material life when the lining is mated with a cast-iron rotor or - drum.
In an effort to stabilize the coefficient of friction while reducing both sooring and wear on a corresponding cast iron drum or rotor, Canadian Patent Application 328,221, filed May 24, 1979, discloses a c~nposition of material for a friction lining having carbon and/or graphite particles therein which modify any detrimental effects that glass fibers in a composition of materials may have on a corresponding mating surface.
SUMMARY OF T~E INVE~C~
We have discovered that the detrimental effects caused by glass fibers in a friction material can be reduced by the separation of the individual bundles of glass fibers in the process of manufacturing the friction material.
In this process, dry ingredients including a thermosetting phenolic resin, friction modifiers and glass fibers are mixed together to form a oomposition of materials. me composition of materials is blended until a bulk density of between 0.1 -0.6 gm/cc is achieved through the separation of the individual filaments that make up the glass fibers. me blended composition of material is thereafter formed into briquettes. me briquettes t are hot pressed to a predetermuned density and shape. mereafter the pre-fo~med briquettes are cured in an oven to set the phenolic resin and hold ; the filaments and friction modifiers in a fixed position. The cured briq~lettes are thereafter ground to a desired thickness to produce a friction ~terial.
It is an object of this invention to provide a method of manufacturing ~m~ 3 -37~3 .i a friction material from a composition of materials including glass fibers ;.
` wherein the individual filaments are separated and thereafter uniformly distributed throughout the composition of materials.
, i It is a further object of this invention to modify the bulk density ~; of a composition of material during processing through the separation of glass fibers in a blending process.
It is another object of this invention to provide a composition ,~
of material for use as a friction material with filaments from glass fibers ~ to establish a substantially uniform coefficient of friction between 25~-65~ F.
'~ 10 These and other objects should be apparent from reading this specification while viewing the drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
Figure 1 is a table showing the components incorporated into the composition of material for making a friction lining according to the principlesof this invention;
Figure 2 is a graph comparing friction versus temperature of a typical asbestos based friction material and glass f;ber based friction materials;
Figure 3 is a graph comparing wear versus temperature of a typ;cal asbestos based friction material and glass based friction materials;
,~ 20 Figure 4 is a table showing friction stability, friction level, pad and rotor wear of a typical asbestos based friction material and glass based friction materials;
Figure 5 is a graph showing the fade and recovery of a typical asbestos based friction material and glass fiber based friction materials;
Figure 6 is a table comparing vehicle test data of a typical asbestos based friction material and glass fiber based friction materials;
~-~ Figure 7 is a graph illustrating pad and rotor wear of a test vehicle associated with a typical asbestos based friction material and glass fiber based friction materials;
Figura 8 is a photograph showing the effect of various blending times '~'' ~ 8708 on ~lass fiber;
Figure 9 is a photomicrograph magnified 20 times ; showing a glass fiber before and after blending for 10 minutes;
- F1gure 10 is a graph comparing friction versus temperature of glass fiber based friction materials made .. . .
according to the principles of this invention; and Figure 11 is a graph comparinq wear versus temperature of glass fiber based friction materials made .~ .
according to the principles of this invention.
- Figures 10 and 11 are found on the third page of .,, drawings along with Figure 7.
DETAILED DESCRIPTION OF TIIE INVENTION
1 , .
In order to evaluate the friction material disclosed by this invention, a typical asbestos friction material A
`, `1 ~
disclosed in Figure 1, was formulated and characterized to : - establish a standard or base for illustratinq an acceptable `~ coefficient of friction and rate of wear for a brake lining . ~ ..
~j of an automobile. Figure 1 also illustrates the modifi-,~
ri~J 20 cations associated with the composition of materials made ` according to this invention.
The ingredients in the composition of material A
were processed into brake friction material in the r, ~; following manner.
;~..
Asbestos fiber, zinc powder, organic modifiers (two parts of cashew nut powder and one part rubber scrap), ; inorganic modifier ~barytes), and dry phenolic resin in the . . .
weight percentages shown in Figure 1 were dry mixed : together for about 30 minutes until a homogenous mixture was -` 30 created. Thereafter, this homogenous mixture was placed in .....
`.`! a mold and compacted into briquettes. The briquettes were 1, , j .
! then transferred to a press station and individually com-. i .
I dm:J~/ 5 , ..~.
. ,- , ' -. .
. '' .
` 3L~87~8 ~. ~
, : pressed at about 6,000 pounds per square inch to establish i. a predetermined shape and density, while the temperature of the briquette was raised to about 275F. The 275F
temperature caused the phenolic resin to flow throughout the ~ mixture and establish a matrix for holding the other ,~ ingredients in a fixed position. Thereafter, the ' briquette as transferred to a curing oven having a temperature .
. of about 500F to further ., . .``
,; I
. .
.`~ ' ' . .
, ' .
., .
~ ~ dm~ Sa - `
~' ' .
376~3 set the phenolic resin. The rubbing surface of the cured briquette was then ground to a spe~ific size corresponding to a brake pad. Thereafter, a portion of the pad was tested on a Chase-type sample dynamometer. This test ` consists in making 40 applications of 20 second duration with a l-inch square sample of friction material against a cast-iron drum rotating at ~25 rpm (40 mph). After a burnish sequence, tests are made at 250 F, 350F, 450 F, 550F, 650 F, and 250 F (re-run). The controlled output torque was held at 350 in-lbs for the tests.
The sample dynamometer data in Figure 2 gives the 250 F, 350 F, 450 F, 550F and 650 F steady state friction ievels and the data in Figure 3 gives the 250 F, 350 F, 450 F, 550 F and 650F wear values.
~he coefficient of friction of composition A was measured and indicated as curve 100 in Figure 2 while the wear of the brake pads experienced at the various temperatures was calculated and illustrated by curve 102 in Figure 3. It should be noted that the wear rate of composition A is acceptable below 350 F. However, when vehicles equ;pped with such brakes are repeatedly applied, the thermal energy generated rapidly increases above 450 F where the wear rate reaches an undesirable level.
Because of the stopping requTrement standards established by the Department of Transportation in FMVSS 105-75, the maximum operating temperature generated in bringing a vehicle to a stop during repeated panic stop conditions often reaches 450F. Thus, typical standard asbestos organic friction lin;ngs, while producing acceptable coefficients of friction, are damaged since the wear rate increases exponentially above 350 F as shown in F;gure 3.
:
- A brake pad of composition A was mated with a caltper and rotor assembly of a full brake and installed on an inertial dynamoMeter. The inertial dynamometer procedure combined performance and wear versus temperature testing with emphasis placed on friction change wtth Increased duty usage.
The test procedure Included the following: pre-burnish effectiveness checks (at 30, 60, and 80 mph with 0.4, 0.6, and 0.7G deceleration, respectively) '7~8 with an initial pad temperature of 200F; 200 burnish stops (40 mph at 12 ft/sec. from 250F initial pad temperature); post-burnish effPctiveness (at 30, 60 and 80 mph with 0.4, 0.6 and 0.7G deceleration, respectively) followed by 3 SAE-type fade and recovery checks to 450 , 600 and 700 F, and a ftnal effectiveness check (at 30, 60 and ~0 mph with 0.4, o.6 and 0.7G deceleration).
The friction level and friction stability of composition A
as indicated by line pressure required to make 3 successive stops from 60 mph at 0.7G deceleration is shown by the table in Figure 4. The pad and rotor wear data are also included.
The fade characteristics of composition A is shown by lines lOô, 110, and 112 and the recovery characteristics is shown by lines 114, 116 and 118 in Figure 5.
Because of the superior frictional characteristics and high tensile strength of glass fibers over other fiberous materials suitable for friction materials, it was decided to modify composition A through the substitution of glass fiber and metal oxide particles to produce a glass fiber based composition of material B shown in Figure 1.
The glass fiber which is known in the industry as Type E is made by heating raw materials, such as s;lica sand, ltmestone, dolomite, clay, boric acid, soda ash and other minor ingredients in a h;gh-temperature furnace in a direct melt process to produce glass. The glass flows to forehearths in the bottom of the tank furnace. The glass flows through numerous holes or orifices located in platinum alloy bushings or spinnerettes to produce filaments of molten glass. The filaments, which can range in number from 20 to 2,000, are gathered together as a thread or strand and attached to a rotating drum which turns a.
a speed up to 75,000 rpm to produce a glass fiber. Thereafter, the glass . :~
;~; fiber is treated with a silanizing or sizing agent, such as a silane, to ~", ~`~ improve the resin-to-fiber adhesion. Thereafter, the continuous fiber is cut into lengths which may vary from 250-10,000 microns.
3 The composition of ma~erial ~ shown in Fisure 1 was compounded in ''''' ... .
. . .
:'~
: ~ :
~$ /~
the same manner as composition A and processed into a brake pad. The bra~e pad of composition B was installed in the Chase-type sample aynamometer and a friction wear test was performed. The coefficient of friction of composition B is illustrated by curve 104 in Figure 2 and the wear rate by curve lOS
in Figure 3. As shown in Figure 2 the coefficient of friction of composition B is substantially equivalent to ~he coefficient of friction of composition A.
However, the wear rate as shown in Figure 3 is unacceptable for use as a friction material.
Since the coefficient of friction as shown in Figure 2 of composition C is substantially stable above 450 F, it was decided to evaluate the modifications for composition B which would reduce the wear rate. Thus, it was decided to remove the abrasive metal oxide particles through a substitution of cashew nut dust particles and a non-abrasive mineral particle (barytes) to the mixture to produce composition C shown in Figure 1.
The processed mineral fiber in composition C is made up of a composi~ion consisting of silica, alumina, calcia, magnesia and other oxides. The fiber diameters may vary from 1-15 microns and the fiber lengths may vary from 40-1,000 microns. During the manufacture of these fibers, the surface thereof is treated with a silanizing agent to improve the resin-to-fiber adheston.
The composition of material C was compounded and processed into disc brake pads. The wear and friction level as measured on the inertial dynamometer of composition C is shown in Figure 4. The fade characteristics ; of composition C are illustrated by curves 120, 122 and 124 while the recovery characteristics are illustrated by curves 126, 128 and 130 in ; Figure 5. From comparing the friction and wear data of composition C with composition A, it is apparent that composition C is superior to composition A.
Thereafter, a test vehicle was equipped with friction material pads made of compositions A and C and test data obtained therefrom to further evaluate the glass fiber composition C. The test vehicle was a station wagon having a weight of 5,C00 lbs.GVW. Except for burni,h, reburnish and 7~3 light/heavy duty cycle operations, the performance data was obtained with only the front di;c brakes functioning. Noise rating was determined with ` light brake applications (20-150 psi line pressure) at slow speed (5-30- mph) in a quiet area (such as an inactive parking structure) for the best noise amplification and detection. In each noise search, the windows were open and the radio and heat/air conditioner fan were turned off to provide a low noise background.
The performance data of composition C and that of composition A is presented in Figure 6. The first four sets of effectiveness data were obtained with an initial pad temperature at 150F before each brake application.
Applications were made at 10, 30 and 60 mph, with 10 or 15 ft/sec.2 decelerationas specified. The fifth effectiveness data were obtained in the same manner, except that the initial pad temperature was kept at 300F. The first effective-ness test measures the effective line pressures at various speeds before the pads were subject to burnish; the second, post burnish and before the fades;
the third, post 450F and 600F fades; the fourth, post 700 F fade.
It is clear from the data in Figure 6 that compositions C and A
have comparable friction levels at the start of the test. However, the asbestos-free composition C has better friction stability than the typical asbestos based composition A as indicated by the smaller frictional level change and by the lack of friction increase with use which leads to brake burnup and friction instability.
After the series of tests reported in the table of Figure 6, the pads and rotors were measured for wear. The right front pad and rotor wear and the left front pad and rotor wear for compositions A and C are illustrated by lines RF and LF, respectively in Figure 7. From viewing Figure 7 it should be evident that the pad wear resistance of composition C is clearly superior to composition A. The rotor wears of the A and C
are comparable (0.0000 and 0~0001 inches, respectively~.
3 ~n order to further evaluate the family of composition of materials that include glass fiber as the strengthening ngredient, composition C was modified by removing the carbon particles and reducing the phenolic resin content while increasing the glass fiber and mineral fiber to produce composi-` tion D shown in Figure 1.
The friction and wear data of composition D generated from theChase-type sample dynamometer are shown by curves 105 and 107 in Figures 2 and 3, respectively.
The results of the inertial dynamometer test of composition D are i shown in Figure 4.
Thereafter, composition D was procéssed into brake pads and placed on the test vehicle. The results of the vehicle brake test for , . .
composition D are illustrated in Figure 6. When the data shown in the -~` table of Figure 6 is compared, it is evident that the glass flber reinforce-ment and cashew nut powder friction dust mod;fied compositions of both compositions C and D have better friction stability and less pad wear than - composition A.
In attempting to duplicate the data for compos;tion D sho~n in the table of Figure 6, different data values were obtained using the same ~ .
weight percentages for the material shown in Figure I for composition of material D. In attempting to explain the different data generation with ~, ~ the same material, it was determined that slight variations could occur in '~4 the blending of the dry ingredients from one batch to another. On in-vestigation it was observed that the bulk dens;ty of the compositlon varied with increased blending time. This change in bulk density was attributed to the ~ separation of the filaments that made up the glass fibers.
- To evaluate the effect of the glass fibers on blendtng time, six samples of glass fibers each weighing 10 grams were evaluated. Five samples ~; were successively placed in a mixer and hlended for times varying from I m;nJt2 to 10 minutes. The five samples after blending were removed from the mixer and placed in piles adjacer.t the test sample designated XF-10 as shown by the ', . ~ --10--., .,.,,~
7~
photograph in Figure 8. As shown in Figure 8, the glass fibers expanded by separation in almost a direct proportion to the blending time in the mixer.
To substantiate the speculation that substantially the entire bundles of filaments that make up glass fiber separated, SEM photo micrographs (20 x) shown in Figure 9 were taken of the glass fiber in sample XF-I0 and the glass `~ fiber after 10 minutes of blending. As shown in Figure 9, the individual filaments after blending are randomly dispersed without any definite orientation as compared to the tight knit bundles of the glass fiber in the original material.
To determine the optimum effect of`the expansion or opening of the bundles of filaments of glass fiber on a friction lining, a series of tests were performed on composition D made by a process of manufacturing wherein the blending times were varied. In the first composition designated D-l, the dry ingredients were placed in a mixer and blended for a time period of 5 minutes. At the end of 5 minutes, the composition of material had a bulk dens;ty of about 0.46 gm/cc . The material was transferred to a briquette mold and brjquettes ` were made from composition D-l. These individual briquettes were transported ; to a press and compacted with a force of about 6000 psi to a predetermined density while at the same time the temperature was raised to 275 F to allow the phenolic resin to flow throughout the mixture and hold the other ingredients in a fixed position. Thereafter, the indtvidual briquettes were transterred to a curing oven having a temperature of about 500 F to set the phenol;c resin. The individual briquettes of composition D-l were ground to a specific size brake pad and thereafter when tested by the Chase-type sample dynamometer ,'~J, procedure described above with respect to composition A produced a coefficient of friction illustrated by line 130 in Figure 10 and a wear rate illustrated by line 132 in Figure 11.
` Thereafter, a second composition designated D-2 ~as placed in a mixer and blended for a time period of 10 minutes. At the end of lD minutes, , , composition D-2 had a bulk density of about 0.25 gm/cc . This blended material , . ~
. ; - 1 1 -'',' .
, .
:
was processed into brake pads in the same manner as composi.ion D-l and when tested on the Chase-type sample dynamometer produced a coefficient of friction illustrated by line 134 in Figure 10 and a wear rate illustrated by line 136 in Figure 11.
~` A third composition designated D-3 was placed in a mixer and blended ` for a time period of 15 minutes. At the end of 15 minutes, composition D-3 had a bulk density of about 0.20 gm/cc 3. This blended material was similarly . =, , .
processed into brake pads and when tested on the Chase-type sample dynamometer produced a coefficient of friction illustrated by line 138 in Figure 10 ; ~. ...
and a wear rate illustrated by line 140 in Figure 11.
, ~:
From the test data generated by compositions D-l, D-2 and D-3, ~-~; it was discovered that a coefficient of friction for friction lining utilizing glass fiber is enhanced wilen the blending time in the manufacturing ~` process is limited to between 5-15 minutes.
~` in order to ;nsure that the tngredients are uniformly distributed throughout the resulting brake pad, it was decided to pre-blend 'he ingredients prior to adding the glass fibers to the mixture.
~; Therefore, the friction modifiers and phenolic resln ~ere placed in a . ., ~ mixer and pre-blended for 5 minutes before the glass fibers in composition D
- i
Organic friction material compositions currently used in clutch and brake linings of vehicles must be capable of withstanding the severe operating temperatures and dynamic . pressures experienced during repeated applications. To pre-':`.
vent a deterioration in performance and physical degradation during such applications, the linings are normally reinforced by asbestos fibers randomly dispersed throughout a resin matrix. However, recent medical evidence indicates that asbestos fibers can cause health hazards for people exposed thereto during the manufacture of clutch and brake linings.
Unfortunately, because of the presence of fine diameter asbestos fiber during the manufacture of brake lining using asbestos fiber, a portion of the asbestos often becomes air-borne in quantities that exceed the exposure standard of ~ .
asbestos fiber in the United States as controlled by the - Occupational Safety and Health Act of 1970. Furthermore, mechanics relining the automotive brakes are also exposed to some quantity of asbestos from the linings.
In an effort to reduce the environmental contamination by the asbestos fiber and thereby continue the manufacturing of asbestos based organic friction linings, a water slurry process disclosed in Canadian Patent No. 1,105,214 (issued July 21, 1981) has been evaluated. The water slurry can be transmitted throughout a manufacturing facility without contaminating the surrounding environment with asbestos fibers. However, before the friction ma~erial can be cured, the water in the slurry must be removed in order to be assured that any resulting lining has essentially the same operating characteristics as a lining made from a dry mix. Unfortunately, this process adds considerable cost to the manufacturing cost of a brake or c~utch lining, and does not ~ecessarily solve emission problems during finishing and inspection.
. - 2 -~ B ~
dm~
~1~8708 ` In a effort to use readily available materials and the san~
manufacturing facilities, as currently available, it has been suggested that glass and/or mineral fibers be used in place of at least a portion of the asbestos fillers. U.S. Patent 3,967,037 discloses several lining con-positions utilizing glass fiber in place of asbestos. Fr~n experimentation, it has been determined such lining compositions in normal operational , . I
conditions produce brake noise, severe rotor scoring and wear, and poor frlction material life when the lining is mated with a cast-iron rotor or - drum.
In an effort to stabilize the coefficient of friction while reducing both sooring and wear on a corresponding cast iron drum or rotor, Canadian Patent Application 328,221, filed May 24, 1979, discloses a c~nposition of material for a friction lining having carbon and/or graphite particles therein which modify any detrimental effects that glass fibers in a composition of materials may have on a corresponding mating surface.
SUMMARY OF T~E INVE~C~
We have discovered that the detrimental effects caused by glass fibers in a friction material can be reduced by the separation of the individual bundles of glass fibers in the process of manufacturing the friction material.
In this process, dry ingredients including a thermosetting phenolic resin, friction modifiers and glass fibers are mixed together to form a oomposition of materials. me composition of materials is blended until a bulk density of between 0.1 -0.6 gm/cc is achieved through the separation of the individual filaments that make up the glass fibers. me blended composition of material is thereafter formed into briquettes. me briquettes t are hot pressed to a predetermuned density and shape. mereafter the pre-fo~med briquettes are cured in an oven to set the phenolic resin and hold ; the filaments and friction modifiers in a fixed position. The cured briq~lettes are thereafter ground to a desired thickness to produce a friction ~terial.
It is an object of this invention to provide a method of manufacturing ~m~ 3 -37~3 .i a friction material from a composition of materials including glass fibers ;.
` wherein the individual filaments are separated and thereafter uniformly distributed throughout the composition of materials.
, i It is a further object of this invention to modify the bulk density ~; of a composition of material during processing through the separation of glass fibers in a blending process.
It is another object of this invention to provide a composition ,~
of material for use as a friction material with filaments from glass fibers ~ to establish a substantially uniform coefficient of friction between 25~-65~ F.
'~ 10 These and other objects should be apparent from reading this specification while viewing the drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
Figure 1 is a table showing the components incorporated into the composition of material for making a friction lining according to the principlesof this invention;
Figure 2 is a graph comparing friction versus temperature of a typical asbestos based friction material and glass f;ber based friction materials;
Figure 3 is a graph comparing wear versus temperature of a typ;cal asbestos based friction material and glass based friction materials;
,~ 20 Figure 4 is a table showing friction stability, friction level, pad and rotor wear of a typical asbestos based friction material and glass based friction materials;
Figure 5 is a graph showing the fade and recovery of a typical asbestos based friction material and glass fiber based friction materials;
Figure 6 is a table comparing vehicle test data of a typical asbestos based friction material and glass fiber based friction materials;
~-~ Figure 7 is a graph illustrating pad and rotor wear of a test vehicle associated with a typical asbestos based friction material and glass fiber based friction materials;
Figura 8 is a photograph showing the effect of various blending times '~'' ~ 8708 on ~lass fiber;
Figure 9 is a photomicrograph magnified 20 times ; showing a glass fiber before and after blending for 10 minutes;
- F1gure 10 is a graph comparing friction versus temperature of glass fiber based friction materials made .. . .
according to the principles of this invention; and Figure 11 is a graph comparinq wear versus temperature of glass fiber based friction materials made .~ .
according to the principles of this invention.
- Figures 10 and 11 are found on the third page of .,, drawings along with Figure 7.
DETAILED DESCRIPTION OF TIIE INVENTION
1 , .
In order to evaluate the friction material disclosed by this invention, a typical asbestos friction material A
`, `1 ~
disclosed in Figure 1, was formulated and characterized to : - establish a standard or base for illustratinq an acceptable `~ coefficient of friction and rate of wear for a brake lining . ~ ..
~j of an automobile. Figure 1 also illustrates the modifi-,~
ri~J 20 cations associated with the composition of materials made ` according to this invention.
The ingredients in the composition of material A
were processed into brake friction material in the r, ~; following manner.
;~..
Asbestos fiber, zinc powder, organic modifiers (two parts of cashew nut powder and one part rubber scrap), ; inorganic modifier ~barytes), and dry phenolic resin in the . . .
weight percentages shown in Figure 1 were dry mixed : together for about 30 minutes until a homogenous mixture was -` 30 created. Thereafter, this homogenous mixture was placed in .....
`.`! a mold and compacted into briquettes. The briquettes were 1, , j .
! then transferred to a press station and individually com-. i .
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, : pressed at about 6,000 pounds per square inch to establish i. a predetermined shape and density, while the temperature of the briquette was raised to about 275F. The 275F
temperature caused the phenolic resin to flow throughout the ~ mixture and establish a matrix for holding the other ,~ ingredients in a fixed position. Thereafter, the ' briquette as transferred to a curing oven having a temperature .
. of about 500F to further ., . .``
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376~3 set the phenolic resin. The rubbing surface of the cured briquette was then ground to a spe~ific size corresponding to a brake pad. Thereafter, a portion of the pad was tested on a Chase-type sample dynamometer. This test ` consists in making 40 applications of 20 second duration with a l-inch square sample of friction material against a cast-iron drum rotating at ~25 rpm (40 mph). After a burnish sequence, tests are made at 250 F, 350F, 450 F, 550F, 650 F, and 250 F (re-run). The controlled output torque was held at 350 in-lbs for the tests.
The sample dynamometer data in Figure 2 gives the 250 F, 350 F, 450 F, 550F and 650 F steady state friction ievels and the data in Figure 3 gives the 250 F, 350 F, 450 F, 550 F and 650F wear values.
~he coefficient of friction of composition A was measured and indicated as curve 100 in Figure 2 while the wear of the brake pads experienced at the various temperatures was calculated and illustrated by curve 102 in Figure 3. It should be noted that the wear rate of composition A is acceptable below 350 F. However, when vehicles equ;pped with such brakes are repeatedly applied, the thermal energy generated rapidly increases above 450 F where the wear rate reaches an undesirable level.
Because of the stopping requTrement standards established by the Department of Transportation in FMVSS 105-75, the maximum operating temperature generated in bringing a vehicle to a stop during repeated panic stop conditions often reaches 450F. Thus, typical standard asbestos organic friction lin;ngs, while producing acceptable coefficients of friction, are damaged since the wear rate increases exponentially above 350 F as shown in F;gure 3.
:
- A brake pad of composition A was mated with a caltper and rotor assembly of a full brake and installed on an inertial dynamoMeter. The inertial dynamometer procedure combined performance and wear versus temperature testing with emphasis placed on friction change wtth Increased duty usage.
The test procedure Included the following: pre-burnish effectiveness checks (at 30, 60, and 80 mph with 0.4, 0.6, and 0.7G deceleration, respectively) '7~8 with an initial pad temperature of 200F; 200 burnish stops (40 mph at 12 ft/sec. from 250F initial pad temperature); post-burnish effPctiveness (at 30, 60 and 80 mph with 0.4, 0.6 and 0.7G deceleration, respectively) followed by 3 SAE-type fade and recovery checks to 450 , 600 and 700 F, and a ftnal effectiveness check (at 30, 60 and ~0 mph with 0.4, o.6 and 0.7G deceleration).
The friction level and friction stability of composition A
as indicated by line pressure required to make 3 successive stops from 60 mph at 0.7G deceleration is shown by the table in Figure 4. The pad and rotor wear data are also included.
The fade characteristics of composition A is shown by lines lOô, 110, and 112 and the recovery characteristics is shown by lines 114, 116 and 118 in Figure 5.
Because of the superior frictional characteristics and high tensile strength of glass fibers over other fiberous materials suitable for friction materials, it was decided to modify composition A through the substitution of glass fiber and metal oxide particles to produce a glass fiber based composition of material B shown in Figure 1.
The glass fiber which is known in the industry as Type E is made by heating raw materials, such as s;lica sand, ltmestone, dolomite, clay, boric acid, soda ash and other minor ingredients in a h;gh-temperature furnace in a direct melt process to produce glass. The glass flows to forehearths in the bottom of the tank furnace. The glass flows through numerous holes or orifices located in platinum alloy bushings or spinnerettes to produce filaments of molten glass. The filaments, which can range in number from 20 to 2,000, are gathered together as a thread or strand and attached to a rotating drum which turns a.
a speed up to 75,000 rpm to produce a glass fiber. Thereafter, the glass . :~
;~; fiber is treated with a silanizing or sizing agent, such as a silane, to ~", ~`~ improve the resin-to-fiber adhesion. Thereafter, the continuous fiber is cut into lengths which may vary from 250-10,000 microns.
3 The composition of ma~erial ~ shown in Fisure 1 was compounded in ''''' ... .
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the same manner as composition A and processed into a brake pad. The bra~e pad of composition B was installed in the Chase-type sample aynamometer and a friction wear test was performed. The coefficient of friction of composition B is illustrated by curve 104 in Figure 2 and the wear rate by curve lOS
in Figure 3. As shown in Figure 2 the coefficient of friction of composition B is substantially equivalent to ~he coefficient of friction of composition A.
However, the wear rate as shown in Figure 3 is unacceptable for use as a friction material.
Since the coefficient of friction as shown in Figure 2 of composition C is substantially stable above 450 F, it was decided to evaluate the modifications for composition B which would reduce the wear rate. Thus, it was decided to remove the abrasive metal oxide particles through a substitution of cashew nut dust particles and a non-abrasive mineral particle (barytes) to the mixture to produce composition C shown in Figure 1.
The processed mineral fiber in composition C is made up of a composi~ion consisting of silica, alumina, calcia, magnesia and other oxides. The fiber diameters may vary from 1-15 microns and the fiber lengths may vary from 40-1,000 microns. During the manufacture of these fibers, the surface thereof is treated with a silanizing agent to improve the resin-to-fiber adheston.
The composition of material C was compounded and processed into disc brake pads. The wear and friction level as measured on the inertial dynamometer of composition C is shown in Figure 4. The fade characteristics ; of composition C are illustrated by curves 120, 122 and 124 while the recovery characteristics are illustrated by curves 126, 128 and 130 in ; Figure 5. From comparing the friction and wear data of composition C with composition A, it is apparent that composition C is superior to composition A.
Thereafter, a test vehicle was equipped with friction material pads made of compositions A and C and test data obtained therefrom to further evaluate the glass fiber composition C. The test vehicle was a station wagon having a weight of 5,C00 lbs.GVW. Except for burni,h, reburnish and 7~3 light/heavy duty cycle operations, the performance data was obtained with only the front di;c brakes functioning. Noise rating was determined with ` light brake applications (20-150 psi line pressure) at slow speed (5-30- mph) in a quiet area (such as an inactive parking structure) for the best noise amplification and detection. In each noise search, the windows were open and the radio and heat/air conditioner fan were turned off to provide a low noise background.
The performance data of composition C and that of composition A is presented in Figure 6. The first four sets of effectiveness data were obtained with an initial pad temperature at 150F before each brake application.
Applications were made at 10, 30 and 60 mph, with 10 or 15 ft/sec.2 decelerationas specified. The fifth effectiveness data were obtained in the same manner, except that the initial pad temperature was kept at 300F. The first effective-ness test measures the effective line pressures at various speeds before the pads were subject to burnish; the second, post burnish and before the fades;
the third, post 450F and 600F fades; the fourth, post 700 F fade.
It is clear from the data in Figure 6 that compositions C and A
have comparable friction levels at the start of the test. However, the asbestos-free composition C has better friction stability than the typical asbestos based composition A as indicated by the smaller frictional level change and by the lack of friction increase with use which leads to brake burnup and friction instability.
After the series of tests reported in the table of Figure 6, the pads and rotors were measured for wear. The right front pad and rotor wear and the left front pad and rotor wear for compositions A and C are illustrated by lines RF and LF, respectively in Figure 7. From viewing Figure 7 it should be evident that the pad wear resistance of composition C is clearly superior to composition A. The rotor wears of the A and C
are comparable (0.0000 and 0~0001 inches, respectively~.
3 ~n order to further evaluate the family of composition of materials that include glass fiber as the strengthening ngredient, composition C was modified by removing the carbon particles and reducing the phenolic resin content while increasing the glass fiber and mineral fiber to produce composi-` tion D shown in Figure 1.
The friction and wear data of composition D generated from theChase-type sample dynamometer are shown by curves 105 and 107 in Figures 2 and 3, respectively.
The results of the inertial dynamometer test of composition D are i shown in Figure 4.
Thereafter, composition D was procéssed into brake pads and placed on the test vehicle. The results of the vehicle brake test for , . .
composition D are illustrated in Figure 6. When the data shown in the -~` table of Figure 6 is compared, it is evident that the glass flber reinforce-ment and cashew nut powder friction dust mod;fied compositions of both compositions C and D have better friction stability and less pad wear than - composition A.
In attempting to duplicate the data for compos;tion D sho~n in the table of Figure 6, different data values were obtained using the same ~ .
weight percentages for the material shown in Figure I for composition of material D. In attempting to explain the different data generation with ~, ~ the same material, it was determined that slight variations could occur in '~4 the blending of the dry ingredients from one batch to another. On in-vestigation it was observed that the bulk dens;ty of the compositlon varied with increased blending time. This change in bulk density was attributed to the ~ separation of the filaments that made up the glass fibers.
- To evaluate the effect of the glass fibers on blendtng time, six samples of glass fibers each weighing 10 grams were evaluated. Five samples ~; were successively placed in a mixer and hlended for times varying from I m;nJt2 to 10 minutes. The five samples after blending were removed from the mixer and placed in piles adjacer.t the test sample designated XF-10 as shown by the ', . ~ --10--., .,.,,~
7~
photograph in Figure 8. As shown in Figure 8, the glass fibers expanded by separation in almost a direct proportion to the blending time in the mixer.
To substantiate the speculation that substantially the entire bundles of filaments that make up glass fiber separated, SEM photo micrographs (20 x) shown in Figure 9 were taken of the glass fiber in sample XF-I0 and the glass `~ fiber after 10 minutes of blending. As shown in Figure 9, the individual filaments after blending are randomly dispersed without any definite orientation as compared to the tight knit bundles of the glass fiber in the original material.
To determine the optimum effect of`the expansion or opening of the bundles of filaments of glass fiber on a friction lining, a series of tests were performed on composition D made by a process of manufacturing wherein the blending times were varied. In the first composition designated D-l, the dry ingredients were placed in a mixer and blended for a time period of 5 minutes. At the end of 5 minutes, the composition of material had a bulk dens;ty of about 0.46 gm/cc . The material was transferred to a briquette mold and brjquettes ` were made from composition D-l. These individual briquettes were transported ; to a press and compacted with a force of about 6000 psi to a predetermined density while at the same time the temperature was raised to 275 F to allow the phenolic resin to flow throughout the mixture and hold the other ingredients in a fixed position. Thereafter, the indtvidual briquettes were transterred to a curing oven having a temperature of about 500 F to set the phenol;c resin. The individual briquettes of composition D-l were ground to a specific size brake pad and thereafter when tested by the Chase-type sample dynamometer ,'~J, procedure described above with respect to composition A produced a coefficient of friction illustrated by line 130 in Figure 10 and a wear rate illustrated by line 132 in Figure 11.
` Thereafter, a second composition designated D-2 ~as placed in a mixer and blended for a time period of 10 minutes. At the end of lD minutes, , , composition D-2 had a bulk density of about 0.25 gm/cc . This blended material , . ~
. ; - 1 1 -'',' .
, .
:
was processed into brake pads in the same manner as composi.ion D-l and when tested on the Chase-type sample dynamometer produced a coefficient of friction illustrated by line 134 in Figure 10 and a wear rate illustrated by line 136 in Figure 11.
~` A third composition designated D-3 was placed in a mixer and blended ` for a time period of 15 minutes. At the end of 15 minutes, composition D-3 had a bulk density of about 0.20 gm/cc 3. This blended material was similarly . =, , .
processed into brake pads and when tested on the Chase-type sample dynamometer produced a coefficient of friction illustrated by line 138 in Figure 10 ; ~. ...
and a wear rate illustrated by line 140 in Figure 11.
, ~:
From the test data generated by compositions D-l, D-2 and D-3, ~-~; it was discovered that a coefficient of friction for friction lining utilizing glass fiber is enhanced wilen the blending time in the manufacturing ~` process is limited to between 5-15 minutes.
~` in order to ;nsure that the tngredients are uniformly distributed throughout the resulting brake pad, it was decided to pre-blend 'he ingredients prior to adding the glass fibers to the mixture.
~; Therefore, the friction modifiers and phenolic resln ~ere placed in a . ., ~ mixer and pre-blended for 5 minutes before the glass fibers in composition D
- i
2~ were added to produce a composition designated as D-4. This composition D-4 was ~, further blended for 5 minutes to expand or separate the filaments ;n the glass fiber. At the end of this time period (5 minutes pre-blend and 5 minutes blend with glass fiber) composition D-4 had a bulk density of about 0.45 gm/cc ~ Thereafter, when composition D-4 was processed into a brake pad and tested on Y~ the Chase-type sample dynamometer, a coefficient of friction illustrated by line 142 in Figure 10 was produced and a wear rate illustrated by line 144 in Figure 1} was achieved.
;` A fifth composition designated D-5 ~as produced by pre-blending th3 ~` friction modifiers and resin for 5 ~inutes before adding the glass fiber and thereafter blending the composition for an additional 10 minutes for a total .~, . ~ / A 12 . ,~ , .
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blend time of 15 minwtes. At the end of 15 minutes, composition D-5 had a bulk density of about 0.26 gm/cc 3. Thereafter, composition D-5 was processed into a brake pad and tested on the Chase-type sample dynamometer. Composition ~- D-5 produced a coefficient of friction illustrated by line 146 in Figure 10 and a wear rate illustrated by line 148 in Figure 11.
A sixth composition designated D-6 was produced by pre-blending the friction modifiers and phenolic resin for 5 minutes before adding the glass fiber. Thereafter, this mixture was blendèd for another 15 minutes for a total blend time of 20 minutes to produce a bulk density about 0.21 gm/cc 3.
Thereafter, composition D-6 was processed into a brake pad and when tested on the Chase-type sample dynamometer produced a coefficient of friction illustrated by line 150 in Figure 10 and a wear rate illustrated by line 152 in Figure 11.
,. ~
~ To substantiate the finding with respect to the expansion of the : . .
`~ individual filaments that make up the stands of glass ftber, a seventh , composition designated D-7 was made wherein a glass fiber identified as type E OCF405-AA-.13" was substituted for the original glass fiber OCF497-BB-.13".
The configuration of glass fibers in OCF405-M-.13" is the same as OCF497-B3-.13"
-, with the exception of the silanizing agent used as sizing for the bundle of filaments. The friction modifiers and phenolic res;n tn compositton D-7 were ~ 20 pre-blended for 5 minutes before the glass ftbers were added. Th;s mtxture :~ was blended for an additional 15 minutes for a total blend ttme of 20 minutes to produce a bulk density ;n the mixture of about 0.54 gm/cc 3.
Thereafter, this blended mixture was processed into a brake pad and tested on the Chase-type sample dynamometer. Composition D-7 when tested produced 3 coefficient of friction illustrated by line 154 in Figure 10 and a wear rate illustrated by line 156 tn Figure 11.
Another glass fiber identified as type E OCF636-DE-.13" was substi.uted for the glass fiber in composttton D to produce another composition !''. identified as composition D-8. This glass fiber has a d;ameter of approximately
;` A fifth composition designated D-5 ~as produced by pre-blending th3 ~` friction modifiers and resin for 5 ~inutes before adding the glass fiber and thereafter blending the composition for an additional 10 minutes for a total .~, . ~ / A 12 . ,~ , .
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blend time of 15 minwtes. At the end of 15 minutes, composition D-5 had a bulk density of about 0.26 gm/cc 3. Thereafter, composition D-5 was processed into a brake pad and tested on the Chase-type sample dynamometer. Composition ~- D-5 produced a coefficient of friction illustrated by line 146 in Figure 10 and a wear rate illustrated by line 148 in Figure 11.
A sixth composition designated D-6 was produced by pre-blending the friction modifiers and phenolic resin for 5 minutes before adding the glass fiber. Thereafter, this mixture was blendèd for another 15 minutes for a total blend time of 20 minutes to produce a bulk density about 0.21 gm/cc 3.
Thereafter, composition D-6 was processed into a brake pad and when tested on the Chase-type sample dynamometer produced a coefficient of friction illustrated by line 150 in Figure 10 and a wear rate illustrated by line 152 in Figure 11.
,. ~
~ To substantiate the finding with respect to the expansion of the : . .
`~ individual filaments that make up the stands of glass ftber, a seventh , composition designated D-7 was made wherein a glass fiber identified as type E OCF405-AA-.13" was substituted for the original glass fiber OCF497-BB-.13".
The configuration of glass fibers in OCF405-M-.13" is the same as OCF497-B3-.13"
-, with the exception of the silanizing agent used as sizing for the bundle of filaments. The friction modifiers and phenolic res;n tn compositton D-7 were ~ 20 pre-blended for 5 minutes before the glass ftbers were added. Th;s mtxture :~ was blended for an additional 15 minutes for a total blend ttme of 20 minutes to produce a bulk density ;n the mixture of about 0.54 gm/cc 3.
Thereafter, this blended mixture was processed into a brake pad and tested on the Chase-type sample dynamometer. Composition D-7 when tested produced 3 coefficient of friction illustrated by line 154 in Figure 10 and a wear rate illustrated by line 156 tn Figure 11.
Another glass fiber identified as type E OCF636-DE-.13" was substi.uted for the glass fiber in composttton D to produce another composition !''. identified as composition D-8. This glass fiber has a d;ameter of approximately
3 6 microns. The friction modifiers and phenolic resin in composition D-8 , s -13-:,~
, .
8~8 .~i .
~` were pre-blended for 5 minutes and the glass fiber OCF636-DE-.13" added and this mixture blended for another 15 minutes for a total blend time of 20 minutes.
; Composition D-8 had a bulk fiber density after 20 minutes of blending of about 0.07 gm~cc . Thereafter, composition D-8 was processed into a brake pad and when tested on the Chase-type sample dynamometer, produced a coefficient of friction illustrated by line 158 in Figure 10 and a wear rate illustrated by line 160 in Figure 11.
. In establishing the ranges for the ingredients in the family of glass fiber friction linings, the glass fiber in composition D was reduced and replaced by mineral fiber and an increase in the cashéw nut powder to produce composition E
~~ shown in Figure 1. Composition E was blended for a time period of about 5 ri minutes and thereafter processed into brake pads. When composition E was tested on the Chase-type sample dynamometer a coefficient of friction illustrated by line 170 and a wear rate illustrated by line 172 were produced.
Both friction and wear of composition E are acceptable.
-` To further substantiate our discovery that the opening of the glass fiber bundles stabilizes the coefficient of brake pads reinforced with glass fibers while proviting an acceptable wear rate, low noise and compatibility with a cast iron rotor or brake drum, composition D was further evaluated through -: 20 a vehicle test. A composition designated C 0005-1 was produced by pre-blending ~ the friction modifiers and phenolic res;n of compos;t;on D for 5 m;nutes before , . .
~ adding the glass f;bers and further blending for an additional 2 m;nutes.
~, Composit;on C 0005-1 was processed ;nto brake pads and installed on a veh;cle. The veh;cle was dr;ven 2,586 m;les in all kinds of traffic on the streets of Detroit, Michigan. Thereafter, the disc pads were evaluated.
The disc pads on the front axle of the vehicle had the following average pad wear: left front - ;nner 0.095 inches and outer û.078 inches; and rignt front - inner 0.099 inches and outer 0.061 inches. Both the left and right rotors had a maximum wear of 0.007 inches, which is considered unacceptable.
., ~ 3 During the road evaluation of composition C 0005-1 it was observed, noise ~.
~ -14-" '''' . ~ , 76~3 was created on substantially each brake application and the friction level was erratic. From the previous test generated on the inertial dynamometer it was assumed that the two minute blending time is insufficient to open the fiber bundles.
Therefore, a composition designated C 0005-2 was produced by pre-blending the friction modifiers and phenolic resin of composition D for five minutes before adding the glass fibers and further blending this mixture for an additional 7 minutes. Composition C 0005-2 was thereafter processad into brake pads and installed on the test vehicle. The vehicle was driven - 10 2,700 miles in all kinds of traffic on the streets of Detroit, Michigan.
Thereafter the disc pads on the front of the vehicle were removed for evaluation. The disc pads during this test were worn the following amounts:
" left front disc pad wear - inner pad 0.049 inches and outer pad 0.034 inches;
and right front disc pad wear - inner pad 0.03~ inches and outer pad 0.032 inches. The rotors were substantially free from any grooves and the wear rate measured a maximum of 0.001 inches which is acceptable. It was observed during the road test of composition C 0005-2 that the noise level generated during braking had decreased to a level considered acceptable. Thus, this test substantiated the results which were obtained through the inertial dynamcmeter testing that an optimum blending time for opening the glass fiber in composition D is about 10 minutes.
; To further evaluate the effect of the distribution of the filaments of glass fiber uniformly throughout a composition, milled fiber glass was substituted into composition D in place of the fiber bundles to produce ; composition F. Composition F was blended for 15 minutes to uniformly ~ distribute the filaments throughout the mixture. Composition F was processel ~ into a friction material and tested on the Chase-type sample dynamometer.
,. .
; Composition F has a coefficient of friction illustrated by curve 10~ in ,~
Figure 2 and a wear illustrated by curve 111 ;n Figure 3.
3 In order to reduce the dusty conditions associated with dry mixing, , ., ,~
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~ latex was substituted for rubber in the dry mixture of composition D to : produce a moist mixture identified as composition G. The latex aided in holding the composition together until the briquettes could be formed. A
friction material sample of composition G was tested on the sample dynamometer : and had a coefficient of friction illustrated by curve 113 in Figure 2 and a wear rate illustrated by curve 115 in Figure 3.
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, . . .
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, .
8~8 .~i .
~` were pre-blended for 5 minutes and the glass fiber OCF636-DE-.13" added and this mixture blended for another 15 minutes for a total blend time of 20 minutes.
; Composition D-8 had a bulk fiber density after 20 minutes of blending of about 0.07 gm~cc . Thereafter, composition D-8 was processed into a brake pad and when tested on the Chase-type sample dynamometer, produced a coefficient of friction illustrated by line 158 in Figure 10 and a wear rate illustrated by line 160 in Figure 11.
. In establishing the ranges for the ingredients in the family of glass fiber friction linings, the glass fiber in composition D was reduced and replaced by mineral fiber and an increase in the cashéw nut powder to produce composition E
~~ shown in Figure 1. Composition E was blended for a time period of about 5 ri minutes and thereafter processed into brake pads. When composition E was tested on the Chase-type sample dynamometer a coefficient of friction illustrated by line 170 and a wear rate illustrated by line 172 were produced.
Both friction and wear of composition E are acceptable.
-` To further substantiate our discovery that the opening of the glass fiber bundles stabilizes the coefficient of brake pads reinforced with glass fibers while proviting an acceptable wear rate, low noise and compatibility with a cast iron rotor or brake drum, composition D was further evaluated through -: 20 a vehicle test. A composition designated C 0005-1 was produced by pre-blending ~ the friction modifiers and phenolic res;n of compos;t;on D for 5 m;nutes before , . .
~ adding the glass f;bers and further blending for an additional 2 m;nutes.
~, Composit;on C 0005-1 was processed ;nto brake pads and installed on a veh;cle. The veh;cle was dr;ven 2,586 m;les in all kinds of traffic on the streets of Detroit, Michigan. Thereafter, the disc pads were evaluated.
The disc pads on the front axle of the vehicle had the following average pad wear: left front - ;nner 0.095 inches and outer û.078 inches; and rignt front - inner 0.099 inches and outer 0.061 inches. Both the left and right rotors had a maximum wear of 0.007 inches, which is considered unacceptable.
., ~ 3 During the road evaluation of composition C 0005-1 it was observed, noise ~.
~ -14-" '''' . ~ , 76~3 was created on substantially each brake application and the friction level was erratic. From the previous test generated on the inertial dynamometer it was assumed that the two minute blending time is insufficient to open the fiber bundles.
Therefore, a composition designated C 0005-2 was produced by pre-blending the friction modifiers and phenolic resin of composition D for five minutes before adding the glass fibers and further blending this mixture for an additional 7 minutes. Composition C 0005-2 was thereafter processad into brake pads and installed on the test vehicle. The vehicle was driven - 10 2,700 miles in all kinds of traffic on the streets of Detroit, Michigan.
Thereafter the disc pads on the front of the vehicle were removed for evaluation. The disc pads during this test were worn the following amounts:
" left front disc pad wear - inner pad 0.049 inches and outer pad 0.034 inches;
and right front disc pad wear - inner pad 0.03~ inches and outer pad 0.032 inches. The rotors were substantially free from any grooves and the wear rate measured a maximum of 0.001 inches which is acceptable. It was observed during the road test of composition C 0005-2 that the noise level generated during braking had decreased to a level considered acceptable. Thus, this test substantiated the results which were obtained through the inertial dynamcmeter testing that an optimum blending time for opening the glass fiber in composition D is about 10 minutes.
; To further evaluate the effect of the distribution of the filaments of glass fiber uniformly throughout a composition, milled fiber glass was substituted into composition D in place of the fiber bundles to produce ; composition F. Composition F was blended for 15 minutes to uniformly ~ distribute the filaments throughout the mixture. Composition F was processel ~ into a friction material and tested on the Chase-type sample dynamometer.
,. .
; Composition F has a coefficient of friction illustrated by curve 10~ in ,~
Figure 2 and a wear illustrated by curve 111 ;n Figure 3.
3 In order to reduce the dusty conditions associated with dry mixing, , ., ,~
,:
~ ` ~
'76~
~ latex was substituted for rubber in the dry mixture of composition D to : produce a moist mixture identified as composition G. The latex aided in holding the composition together until the briquettes could be formed. A
friction material sample of composition G was tested on the sample dynamometer : and had a coefficient of friction illustrated by curve 113 in Figure 2 and a wear rate illustrated by curve 115 in Figure 3.
~V
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, . . .
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"........................................................................ `.
.:
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:
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,` .` ` ~ ~
Claims (14)
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:
1. A process of manufacturing a friction material com-prising the steps of:
mixing together ingredients including a binder, friction modifiers and from 6-24% by weight of glass fibers to form a composition of materials;
blending the composition of materials together for a time period of more than S but less than 20 minutes to produce a bulk density therein of between .1 - .6gm/cc through the separation of the individual filaments that make up the glass fibers;
transferring the blended composition of materials to a mold;
applying pressure to the blended composition of materials in said mold to form a briquette; and curing said briquette at a temperature and under pressure to set said binder and thereby establish a desired shape and density for said friction material.
mixing together ingredients including a binder, friction modifiers and from 6-24% by weight of glass fibers to form a composition of materials;
blending the composition of materials together for a time period of more than S but less than 20 minutes to produce a bulk density therein of between .1 - .6gm/cc through the separation of the individual filaments that make up the glass fibers;
transferring the blended composition of materials to a mold;
applying pressure to the blended composition of materials in said mold to form a briquette; and curing said briquette at a temperature and under pressure to set said binder and thereby establish a desired shape and density for said friction material.
2. The process, as recited in claim 1 wherein said blending establishes a bulk density of approximately 0.25 gm/cc.
3. The process, as recited in claim 1, wherein said blending is achieved in approximately 10 minutes.
4. The product produced by the process recited in claim 2.
5. A process of manufacturing a friction material comprising the steps of:
mixing together ingredients including a binder and friction modifiers;
blending the dry ingredients together to create a uniform mixture;
adding from 6-24% by weight of glass fibers to the uniform mixture;
blending the glass fibers with the pre-blended dry ingredients to form a composition of material having a bulk density of between 0.1 - 0.6 gm/cc;
limiting the blending time of the composition of material to more than 5 but less than 20 minutes;
molding the composition of material to create briquettes; and curing the briquettes at a pressure and temperature to set said binder and thereby establish a desired density and shape for the friction material.
mixing together ingredients including a binder and friction modifiers;
blending the dry ingredients together to create a uniform mixture;
adding from 6-24% by weight of glass fibers to the uniform mixture;
blending the glass fibers with the pre-blended dry ingredients to form a composition of material having a bulk density of between 0.1 - 0.6 gm/cc;
limiting the blending time of the composition of material to more than 5 but less than 20 minutes;
molding the composition of material to create briquettes; and curing the briquettes at a pressure and temperature to set said binder and thereby establish a desired density and shape for the friction material.
6. The process, as recited in claim 5, the steps of blending of the composition of material is limited to about 10 minutes.
7. The process, as recited in claim 6, further including the step of:
limiting the preblending time of the dry ingredient to about 5 minutes.
limiting the preblending time of the dry ingredient to about 5 minutes.
8. The process, as recited in claim 7, wherein said blending causes the individual filaments that make up the glass fibers to separate and produce a bulk density of about 0.25 gm/cc in the composition of material before molding.
9. The process, as recited in claim 5, wherein said composition of material has a coefficient of friction of between 0.3 - 0.6 over a temperature range of from 250° -650°F.
10. In a process of manufacturing a composition of materials including the steps of blending a binder, friction modifiers and glass fibers together to create a uniform mixture, said glass fibers being from 6-24% by weight of said uniform mixture, transmitting the uniform mixture into a mold to form briquettes, hot pressing the briquettes to a desired shape, and curing the shaped briquettes in an oven to set the phenolic resin and hold the glass fibers and friction modifiers in a fixed relationship, the improvement when the individual filaments that make up the glass fibers are separated during the blending time period of more than 5 but less than 20 minutes to establish a bulk density in the uniform mixture of between 0.1 - 0.6 gm/cc.
11. In the process, as recited in claim 10, wherein said time period is about 10 minutes and the resulting bulk density is about 0.25 gm/cc.
12. A process of manufacturing a friction material comprising the steps of:
mixing together ingredients including a binder, friction modifiers and from 6-24% by weight of milled glass fiber to form a composition of materials;
blending the composition of materials together for a time period of more than 5 but less than 20 minutes to produce a bulk density of between 0.1 to 0.6 gm/cc;
molding the composition to create briquettes; and curing the briquettes at a pressure and temperature to set said binder and thereby establish a desired density and shape for the friction material.
mixing together ingredients including a binder, friction modifiers and from 6-24% by weight of milled glass fiber to form a composition of materials;
blending the composition of materials together for a time period of more than 5 but less than 20 minutes to produce a bulk density of between 0.1 to 0.6 gm/cc;
molding the composition to create briquettes; and curing the briquettes at a pressure and temperature to set said binder and thereby establish a desired density and shape for the friction material.
13. The product produced by the process recited in claim 12.
14. A process of manufacturing a friction material comprising the steps of:
mixing together ingredients including a binder, friction modifiers and from 6 to 24% by weight of mats of glass fiber filaments to form a composition of materials;
blending the composition of materials together to disperse the filaments throughout the composition and develop a bulk density therein of 0.1 to 0.6 gm/cc in a time period of between more than 5 but less than 20 minutes;
molding the composition to create briquettes therefrom; and curing the briquettes at a pressure and temperature to set the binder and thereby establish a desired density and shape for the friction material.
15. The product produced by the process recited in
14. A process of manufacturing a friction material comprising the steps of:
mixing together ingredients including a binder, friction modifiers and from 6 to 24% by weight of mats of glass fiber filaments to form a composition of materials;
blending the composition of materials together to disperse the filaments throughout the composition and develop a bulk density therein of 0.1 to 0.6 gm/cc in a time period of between more than 5 but less than 20 minutes;
molding the composition to create briquettes therefrom; and curing the briquettes at a pressure and temperature to set the binder and thereby establish a desired density and shape for the friction material.
15. The product produced by the process recited in
claim 14.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US93330178A | 1978-08-14 | 1978-08-14 | |
US933,301 | 1978-08-14 | ||
KR1019790002945A KR830001417B1 (en) | 1978-08-14 | 1979-08-29 | Process of manufacturing friction material of glass fiber |
Publications (1)
Publication Number | Publication Date |
---|---|
CA1148708A true CA1148708A (en) | 1983-06-28 |
Family
ID=26626608
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CA000333649A Expired CA1148708A (en) | 1978-08-14 | 1979-08-13 | Process for manufacturing a glass fiber friction article |
Country Status (13)
Country | Link |
---|---|
JP (1) | JPS5529580A (en) |
KR (1) | KR830001417B1 (en) |
AR (1) | AR218757A1 (en) |
AU (1) | AU528485B2 (en) |
BR (1) | BR7905267A (en) |
CA (1) | CA1148708A (en) |
DE (1) | DE2932647A1 (en) |
ES (1) | ES483360A1 (en) |
FR (1) | FR2433550A1 (en) |
GB (1) | GB2028350B (en) |
IT (1) | IT1195733B (en) |
SE (1) | SE440389B (en) |
YU (1) | YU40574B (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4920159A (en) * | 1987-12-28 | 1990-04-24 | Allies-Signal Inc. | Friction resistant composition |
Families Citing this family (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5776328A (en) * | 1980-10-29 | 1982-05-13 | Aisin Chem Co Ltd | Manufacturing method of clutch facing without asbestos |
DE3046696C2 (en) * | 1980-12-11 | 1984-11-22 | Rex Patent Graf von Rex GmbH & Co KG, 7170 Schwäbisch Hall | Process for the production of friction linings and friction linings |
DE19853159B4 (en) * | 1998-11-18 | 2005-04-14 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Process for producing friction linings |
KR100522254B1 (en) * | 2002-08-21 | 2005-10-18 | 백원두 | The method of manufacture the brake lining(or pad). |
CN105952826A (en) * | 2016-05-12 | 2016-09-21 | 苏州爱盟机械有限公司 | High-performance bicycle brake pad |
DE202018105384U1 (en) * | 2018-05-18 | 2019-08-20 | Rockwool International A/S | friction material |
Family Cites Families (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1453289A (en) * | 1973-11-01 | 1976-10-20 | Ivanov P M | Antifriction composition |
US3967037A (en) * | 1974-04-12 | 1976-06-29 | Owens-Corning Fiberglas Corporation | Friction material for brake linings and the like |
JPS5187549A (en) * | 1975-01-30 | 1976-07-31 | Asahi Ishiwata Kogyo Kk | MASATSUZAIRYO |
JPS5365277A (en) * | 1976-11-25 | 1978-06-10 | Sumitomo Electric Ind Ltd | Friction material for brake |
IT1105229B (en) * | 1977-07-07 | 1985-10-28 | Thiokol Corp | ASBESTOS-FREE FRICTION COMPOSITION PARTICULARLY USEFUL FOR DISC BRAKE PADS FOR VEHICLES |
-
1979
- 1979-07-30 GB GB7926467A patent/GB2028350B/en not_active Expired
- 1979-07-31 AU AU49387/79A patent/AU528485B2/en not_active Ceased
- 1979-08-07 YU YU1919/79A patent/YU40574B/en unknown
- 1979-08-09 SE SE7906685A patent/SE440389B/en not_active IP Right Cessation
- 1979-08-09 IT IT25007/79A patent/IT1195733B/en active
- 1979-08-11 DE DE19792932647 patent/DE2932647A1/en active Granted
- 1979-08-13 JP JP10391379A patent/JPS5529580A/en active Pending
- 1979-08-13 BR BR7905267A patent/BR7905267A/en unknown
- 1979-08-13 CA CA000333649A patent/CA1148708A/en not_active Expired
- 1979-08-13 ES ES483360A patent/ES483360A1/en not_active Expired
- 1979-08-14 AR AR277716A patent/AR218757A1/en active
- 1979-08-14 FR FR7920675A patent/FR2433550A1/en active Granted
- 1979-08-29 KR KR1019790002945A patent/KR830001417B1/en active
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4920159A (en) * | 1987-12-28 | 1990-04-24 | Allies-Signal Inc. | Friction resistant composition |
Also Published As
Publication number | Publication date |
---|---|
KR830001330A (en) | 1983-04-30 |
FR2433550A1 (en) | 1980-03-14 |
SE7906685L (en) | 1980-02-15 |
SE440389B (en) | 1985-07-29 |
DE2932647A1 (en) | 1980-03-06 |
JPS5529580A (en) | 1980-03-01 |
ES483360A1 (en) | 1980-04-01 |
AU528485B2 (en) | 1983-04-28 |
AU4938779A (en) | 1980-02-28 |
YU191979A (en) | 1983-02-28 |
IT7925007A0 (en) | 1979-08-09 |
GB2028350B (en) | 1982-10-27 |
KR830001417B1 (en) | 1983-07-25 |
YU40574B (en) | 1986-02-28 |
GB2028350A (en) | 1980-03-05 |
AR218757A1 (en) | 1980-06-30 |
IT1195733B (en) | 1988-10-27 |
BR7905267A (en) | 1980-07-08 |
FR2433550B1 (en) | 1983-12-23 |
DE2932647C2 (en) | 1989-07-27 |
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