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1. WO1997041368 - CERMET POUR COMPOSANTS DE FREINS ET SA FABRICATION

Note: Texte fondé sur des processus automatiques de reconnaissance optique de caractères. Seule la version PDF a une valeur juridique

[ EN ]

CERAMIC METAL COMPOSITE BRAKE
COMPONENTS AND MANUFACTURE THEREOF
The present invention relates to brakes, and in particular to aircraft brakes, in which a ceramic matrix composite is at least a portion of a component in said brake.

Herein, a brake is a device for arresting the motion of a mechanism by friction, wherein the mechanism can be any wheeled vehicle such as a car, plane or train. A brake component is any component whose primary function is to cause the frictional force or transfer of said force to arrest the motion of a mechanism. Examples of the brake component include a torque tube, piston housing, rotor and stator, described hereinbelow. A friction element is a brake component in which at least a portion contacts another friction element causing a frictional force to be developed. Illustrative examples of a frictional element include a brake pad and a rotor or stator wherein the rotor or stator directly contact another friction element.

Because of the demands of flight, the materials used to construct aircraft brakes have to meet more stringent criteria compared to other vehicles such as automobiles. In an aircraft, there are three basic modes of brake operation: normal service (landing), rejected take off (RTO) and taxi stops and snubs (taxiing). Upon landing a commercial aircraft such as a Boeing 737, the brake parts which provide friction to arrest motion (friction element) typically heat up to a temperature of 600°C to 800°C. An RTO is the most severe brake operation, wherein the wear rate of the brake can be a thousand times or more greater than a landing and the temperature of the frictional material of the brake can easily exceed a temperature of 1000CC or more. After an RTO, the brake is scrapped because the conditions are so severe. Taxi snubs and stops occur when the plane taxis to and from the runway. A snub is when the plane does not come to a full stop. Because aircraft require large amounts of braking energy in short periods of time (that is, seconds), the friction element should have as large a specific heat as possible, wherein specific heat is the quantity of heat required for a one degree temperature change in a unit weight of material. Also, the friction element should have a low density to decrease aircraft weight and, subsequently, increase payload or decrease fuel consumption.

There are essentially two types of aircraft brakes in service today. The first type is a steel brake. The second type is a carbon/carbon composite brake. Each aircraft brake type has a brake assembly typically comprising a hydraulic piston assembly, torque tube, torque plate, integral wheel and alternating rotors and stators. The torque tube is typically made of steel or a titanium alloy. The wheel and hydraulic piston assembly are typically made of an aluminum alloy.

Typically, the aircraft brake assembly is configured as follows. The torque tube has grooves on the outer diameter running longitudinally the length of the tube to a flange. Typically, a backing plate (flat disk having an outer and inner diameter) is first slid onto the torque tube outer diameter until contacting the flange. The rotors and stators are then alternatingly slid onto the torque tube outer diameter. The rotors and stators are disks also having an inner and outer diameter. The rotors and the backing plate have no grooves on the inner diameter to engage the torque tube but have grooves or mounting means on the outer diameter to attach to the inner diameter of the wheel. The stators have grooves on the inner diameter which engage the torque tube. A pressure plate (a disk having inner diameter grooves engaging the torque tube) is then slid onto the torque tube. On top of the pressure plate is attached the hydraulic piston assembly which is connected to the torque tube by inner diameter grooves or by bolting to the torque tube. The above assembly is then slid over a landing strut axle and the torque tube is mounted to the landing strut at the hydraulic piston assembly end.

The wheel is attached to the backing plate and rotors of the above assembly. The wheel is typically attached by grooves on the inner diameter of the wheel which engage grooves on the outer diameter of the backing plate and rotors. The wheel is mounted to the axle by bearings and thrust nuts.

Functionally, the rotors spin with the wheel until application of the piston to the pressure plate, wherein the rotors contact the stators. Upon rotor-stator contact, torque is created by friction between the rotors and stators. The torque is transmitted to the landing strut via the torque tube, thus slowing the wheel and aircraft. The rotor-stator contact results in wear of the rotors and stators and also in significant heat generation. The stack of rotors and stators are commonly referred to as the heat sink because this is the part of the brake that absorbs energy, converts it to heat and then dissipates it to the atmosphere.

Steel brakes have pairs of rotors and stators, as described above, in which steel rotors (friction element) typically carry the brake pads and the stator is comprised of high-strength, high temperature steel. In a steel brake, the friction elements are the brake pads and stator. The brake pads which contact the stator are typically a metal matrix composite (MMC) wherein the matrix is copper or iron. The pads can be bonded to a rotor or stator by brazing, welding, riveting or direct diffusional bonding. The brake pads, typically, are in the form of segmented pads of some geometry such as trapezoids uniformly positioned around the face of the rotor or stator.

The second type of brake is a carbon/carbon composite brake. Carbon/carbon composite brakes have rotors, stators, backing plate and pressure plate made out of carbon/carbon composite. In this brake, the rotors and stators are the friction elements. Typically, a carbon/carbon composite is a composite of continuous carbon filaments embedded in a carbon matrix. The properties of the composite can vary widely depending on the processing and filament orientation.

As aircraft get ever bigger and faster, the amount of energy necessary to stop an aircraft during landing and RTO continues to increase. These two trends have
necessitated the decrease of weight wherever possible and required the brakes to handle ever increasing energy inputs into the heat sink of the brake. Loads have increased because the size of the wheels and, hence, brakes are limited (that is, by design and weight considerations). Because of weight, steel brakes, in general, are not used on larger commercial aircraft such as the Boeing 747.

Because carbon/carbon composites have a density of about a quarter of the density of steel, carbon/carbon composite brakes are generally used in high speed military aircraft and large commercial aircraft today. However, carbon/carbon composites have a specific heat (for example, J/K-g) that is only about two times greater than the specific heat of steel. Thus, a carbon/carbon composite brake would have to be at least twice the size of a steel brake if limited to the same temperature increase as a steel brake during a landing or RTO. Carbon/carbon composite brakes avoid this unacceptable increase in size by operating at significantly higher temperatures than steel brakes. The higher temperature at which a carbon/carbon composite brake can operate is limited by the ability of surrounding structures (for example, hydraulic piston assembly, wheel and tire) to withstand the temperature generated by the carbon/carbon heat sink and by the tendency of the
carbon/carbon composite to oxidize at higher temperatures which causes unacceptable wear.

The coefficient of friction (μ) of a friction material is desirably as great as possible. The coefficient is desirably as great as possible to minimize the load that is necessary to generate the frictional force (frictional force = μ x normal load) needed to stop a plane. Carbon/carbon composites tend to adsorb water, which decreases the coefficient of friction. The lowered coefficient of friction lasts until the brake has heated up sufficiently during braking to evaporate the water.

During braking, the coefficient of friction of a carbon/carbon composite friction material may vary by a factor of 3 or more causing a corresponding torque variation which can lead to undesirable vibration. Carbon/carbon composite also displays a static coefficient of friction that is less than the dynamic coefficient. This frictional behavior may cause problems during stopping due to the increased load necessary as the wheel slows down.

Two of the largest costs associated with aircraft brakes are the initial cost and the maintenance cost to repair and replace the friction material due to wear. The cost of replacement includes the non-flying time of the aircraft. Thus, the initial cost and wear rate of a brake friction material are two critical components in the costs of operating a plane, Because carbon/carbon composite requires long periods of time to make a component (up to three weeks), the cost of this material is quite high. Also, carbon/carbon composite generally displays significantly higher wear due to mechanical abrasion during taxiing versus landing brake operation. This phenomena is probably due in part to the low hardness of the composite.

It would be desirable to provide a brake component which has a low density, high specific heat, and good high temperature properties such as high flexure strength. In particular, and relative to steel and C/C brakes, it is desirable to provide a friction element having the aforementioned characteristics plus stable coefficient of friction and low wear in all modes of operation (that is, high hardness).

A first aspect of this invention is a brake component having at least 5 percent by volume of said brake component being a ceramic metal composite (CMC), the CMC having:

an interconnected crystalline ceramic phase and a noncontiguous metal phase dispersed within the interconnected ceramic phase,

a density of at most 6 g/cc,

a specific heat of at least 0.8 J/g°C and

a strength of at least 150 MPa at 900°C wherein at least 45 volume percent of the ceramic phase has a melting or decomposition temperature of at least
1400°C.

A second aspect of this invention is a brake having at least one friction element which has at least 5 percent by volume of the element being comprised of a ceramic metal composite (CMC), the CMC contacting upon braking a second friction element and having:

an interconnected crystalline ceramic phase and a noncontiguous metal phase dispersed within the interconnected ceramic phase,

a density of at most 6 g/cc,

a specific heat of at least 0.8 J/g°C,

an autogenous dynamic coefficient of friction of at least 0.4,

a hardness of at least 1000 Kg/mm2 and

a flexure strength of at least 150 MPa at 900°C

wherein at least 45 volume percent of the ceramic phase has a melting or decomposition temperature of at least 1400°C.

The brake component of this invention provides a brake component having a low density, high specific heat and desired high temperature properties such as strength. In particular, when the brake component is a friction element the present invention provides improved hardness (that is, less wear), high and stable coefficient of friction and the aforementioned characteristics.

The brake component of this invention can be any brake component such as a pressure plate, piston housing and brake piston. Preferably the brake component is a friction element. More preferably the brake component is a friction element wherein the CMC contacts a second friction element upon braking.

The brake component can be entirely composed of the ceramic metal composite (CMC) or partially composed of the CMC wherein the CMC comprises at least 5 percent by volume of the component. For example, said component may be a rotor or stator comprised entirely of the CMC. Alternatively, said component may be a rotor or stator which is partially comprised of said CMC. For example, the rotor or stator may have the grooves and material in close proximity to the grooves of the rotor or stator wherein said material has a higher toughness than the CMC, such as a metal or metal matrix composite. Preferably the CMC comprises at least 10 percent, more preferably 25 percent, and most preferably at least 50 percent by volume of the component.

The metal phase of the CMC may be a metal selected from the Periodic Table Groups 2, 4-1 1 , 13 and 14 and alloys thereof. Said groups conform to the new IUPAC notation as described on pages 1 -10 of the CRC Handbook of Chemistry and Physics 71 st Ed.. 1990-91 , incorporated herein by reference. Preferable metals include silicon, magnesium, aluminum, titanium, vanadium, chromium, iron, copper, nickel, cobalt, tantalum, tungsten, molybdenum, zirconium, niobum or mixtures and alloys thereof. More preferred metals are aluminum, silicon, titanium and magnesium or mixtures and alloys thereof.
Aluminum and alloys thereof are most preferred. Suitable aluminum alloys include aluminum containing one or more of Cu, Mg, Si, Mn, Cr and Zn. Al-Cu, Al-Mg, Al-Si, Al-Mn-Mg and Al-Cu-Mg-Cr-Zn aluminum alloys are more preferred. Examples of such alloys are 6061 alloy, 7075 alloy and 1350 alloy, all available from the Aluminum Company of America, Pittsburgh, Pennsylvania.

The ceramic phase of the CMC is crystalline, wherein at least 45 volume percent of said phase has a melting or decomposition temperature of at least 1400°C
Preferably at least 60 percent, more preferably at least 80 percent and most preferably at least 90 percent by volume of the ceramic phase has a melting or decomposition
temperature of at least 1400°C Preferably the decomposition temperature or melt temperature is at least 1500°C, more preferably at least 600°C and most preferably at least 1700DC The ceramic is desirably a bonde, oxide, carbide, nitride, sihcide or mixtures and combinations thereof. Combinations include, for example, borocarbides, oxynitndes, oxycarbides and carbonitndes. More preferred ceramics are SiC, B4C, Sι3N4, Al203, TiB2, SiB6, SιB4, AIN, ZrC, ZrB, a reaction product of at least two of said ceramics, or a reaction product of at least one of said ceramics and the metal. The most preferred ceramic is boron carbide.

Examples of CMC metal-ceramic combinations include B4C/AI, SiC/AI, AIN/AI,

TiBVAI, AI2OJAI, SiB/AI, Sι3N4/AI, SιC/Mgl SiC/Ti, SiC/Mg-AI, SiB/Ti, B4C/Nt, B4C/Tι, B4C/Cu, Aip/Mg, AI.O/1Ϊ, TiN/AI, TiC/AI, ZrB/AI, ZrC/AI, AIB12/AI, AIBVAI, AIB24C4/AI, AIB./Ti, AIB24C/Ti, TiN/Ti, TiC/Ti, ZrO/Ti, TiB7B4C/AI, SiC/TiB/AI, TiC/Mo/Co, ZrC/ZrC/ZrBJZr, TiB/Ni, TiBJCu, TiC/Mo/Ni, SiC/Mo, TiB/TiC/AI, TiB/TiC/Ti, WC/Co and WC/Co/Ni. The subscript "x" represents varying silicon bonde phases that can be formed within the part. More preferred combinations of a metal and ceramic include: B4C/AI, SiC/AI, SiBJAI, TiBVAI and SiC/Mg. Most preferably, the CMC is comprised of a chemically reactive system such as aluminum-boron carbide or aluminum alloy-boron carbide. In a chemically reactive system, the metal component can react with the ceramic during formation of the CMC resulting in a new ceramic phase being formed. Said new phase can modify properties such as hardness and high temperature strength of the composite. A most preferred chemically reactive .system is B4C/AI, wherein the metal phase is aluminum or alloy thereof, and the
interconnected ceramic phase is comprised of at least two ceramics selected from the group consisting of B4C, AIB., AI4BC, AI3B4aC.~ AIB12 and AIB24C4.

Herein, metal phase is considered to be noncontiguous when the individual regions of metal are neither touching nor connected throughout the CMC. The metal phase, consequently, is preferably at most 15 percent by weight of the CMC. The amount of metal is preferably within a range of from 2 to 8 wt. percent, based on total composite weight. Alternatively, the ceramic phase is preferably present in amounts between 85 percent to 98 percent by volume of the CMC. The dispersed noncontiguous metal phase is preferably comprised of metal regions in which the average equivalent diameter of the regions are at most 30, more preferably at most 10, and most preferably at most 5 microns and preferably at least 0.25, more preferably at least 0.5, and most preferably at least 1 micron. Preferably the largest metal region is at most 100, more preferably at most 75, and most preferably at most 50 microns in diameter. In addition, it is also preferred that the metal regions are predominately equiaxed and predominately situated at ceramic-ceramic grain triple points as opposed to elongated along ceramic grain boundaries as determined by optical quantitative stereology from a polished sample described by KJ. Kurzydtowski and B. Ralph, The Quantitative Description of the Microstructure of Materials. CRC Press, Boca Raton, 1995, relevant portions incorporated herein by reference.

Because air or voids have low specific heat and low thermal conductivity, the CMC preferably has a density of at least 90 percent, more preferably at least 95 percent and most preferably at least 98 percent of theoretical.

Since reduced weight is a critical factor in aircraft brakes, the CMC has a density of at most 6 g/cc, preferably at most 4 g/cc, and more preferably at most 3 g/cc. The CMC can have a density of 1.5 g/cc and still be useful as a brake component. A density lower than 1.5 g/cc may not be useful as a friction element, but said element having said density may be useful as a component which shields other components from excessive heat.

When the brake component is a friction element, the dynamic coefficient of friction of the CMC against itself (autogenous) is desirably at least 0.4 determined at a 1 pound load by a pin on disk method described by ASTM G-99 Standard and M. A. Moore, in Wear of Materials, pp. 673-687, Am. Soc. Eng., 1987, each incorporated herein by reference. The CMC coefficient of friction is preferably at least 0.8, more preferably at least 1.2, and most preferably at least 1.4 to preferably at most 5. In addition, the coefficient of friction of the CMC at a temperature of 1000°C desirably does not deviate more than plus or minus 50 percent, preferably not more than +/- 40 percent, more preferably not more than +/- 20 percent, and most preferably not more than +/- 10 percent from the room temperature coefficient of friction at a given load.

When the brake component is a friction element, the wear rate of the CMC as given by the scar diameter of the above described pin on disk method is desirably as small as possible. The sum diameter is preferably less than 2 mm, more preferably less than 1.5 mm, and most preferably less than 1 mm. To minimize wear, the CMC also desirably has a hardness of at least 1000 Kg/mm2. Preferably the hardness is at least 1200, more preferably at least 1400, and most preferably at least 1600 Kg/mm2 to preferably at most 5000 Kg/mm2 as determined by Vickers hardness at a load of 30 pounds.

The CMC preferably has a toughness of at least 5 MPam"2 so as to avoid catastrophic failure of the brake. More preferably the CMC toughness is at least 5.5, even more preferably at least 6 and most preferably at least 6.5 MPam1'2 to preferably at most 25 MPam"2 as determined by a Chevron Notch method described in Cheyron-Notched
Specimens: Testing and Stress Analysis. STP 855. pp. 177-192, Ed. J. H. Underwood et al., Amer. Soc. for Testing and Matl., PA, 1984., incorporated herein by reference.

To dissipate the heat generated during braking, both the CMC and the brake component containing the CMC preferably have a thermal conductivity of at least 10 W/m-K as determined by a laser flash method described in more detail by "Flash Method of
Determining Thermal Diffusivity, Heat Capacity, and Thermal Conductivity," in Journal of Applied Physics. W. J. Parker et al., 32, [9], pp. 1679-1684, incorporated herein by reference. More preferably said thermal conductivity is at least 15, even more preferably at least 20, and most preferably at least 25 W/m-K. However, the thermal conductivity should not be so great that other brake components such as an aluminum hydraulic piston housing are adversely affected. Thus, the CMC and brake component desirably have a thermal conductivity less than 150 W/m-K.

To absorb the frictionally generated heat during braking, the CMC has a specific heat of at least 0.8 J/g°C at room temperature as determined by differential scanning calorimetry. Preferably the specific heat is at least 0.9 and more preferably at least 1 J/g°C to preferably at most the maximum theoretically possible for a selected material. The specific heat also desirably increases as the temperature increases. For example, the specific heat at 1000°C is desirably at least double the specific heat at room temperature.

To minimize failure of a brake, the high temperature flexure strength of the CMC is at least 150 MPa at a temperature of 900°C as determined by ASTM C1161.
Preferably the strength at 900°C is at least 200 MPa, more preferably at least 300 MPa, and most preferably at least 400 MPa to preferably at most 1500 MPa.

The brake component can be made by any convenient or known method which results in said component containing the CMC, described herein. For example, the brake component may be a metal rotor which is fabricated by any convenient metal forming method such as casting, followed by machining, wherein brake pads comprised of the CMC, described herein, are subsequently bonded to said rotor (that is, the CMC is bonded to a metal substrate). The CMC can be bonded to said rotor by any convenient method such as brazing, welding, riveting and direct diffusional bonding. Alternatively, the brake component can be comprised entirely of the CMC.

The CMC portion of the brake component can be made by any convenient or known powdered metal or ceramic processing technique wherein a shaped body is formed followed by a consolidation technique(s) and, if desired, finishing the article to final shape. The ceramic and metal can be any metal or ceramic previously described. Two typical consolidation routes which can be used to form the CMC of this invention are (1 ) infiltrating a porous ceramic particulate body (greenware) with metal and (2) densifying a porous particulate body (greenware) containing metal and ceramic particulates. The infiltrated or densified body can then be finished (that is, machined) by techniques such as diamond grinding, laser machining and electro discharge machining. Said body can also be heat treated to alter the microstructure of the consolidated composite. Preferably the composite is made by infiltration.

The ceramic or metal powder typically has an average particle size by weight of at most 50 micrometers, preferably at most 15 micrometers, more preferably at most 10 microns, and most preferably at most 5 microns. The particles may be in the shape of platelets, rods or equiaxed grains. The particles of the ceramic powder desirably have a particle diameter within a range of 0.1 to 10 micrometers.

Suitable shaping methods to form greenware (that is, a porous body made up of particulates) for infiltrating or densifying include slip or pressure casting, pressing and plastic forming methods (for example, jiggering and extrusion). The shaping methods may include steps such as mixing of components such as ceramic powder, metal powder, dispersants, binders, and solvent and removing, if necessary, solvent and organic additives such as dispersants and binders after shaping of the greenware. Each of the above methods and steps are described in more detail in Introduction to the Principles of Ceramic
Processing. J. Reed, J. Wiley and Sons, N.Y., 1988, incorporated herein by reference.

The metal-ceramic particulate greenware can be densified into a substantially dense composite by techniques such as vacuum sintering, atmospheric pressure
(pressureless) sintering, pressure assisted sintering such as hot pressing, hot isostatic pressing and rapid omni directional compaction and combinations thereof, each pressure assisted technique is further described in Annu. Rev. Mater. Sci.. 1989, [19], C. A. Kelto, E. E. Timm and A. J. Pyzik, pp. 527-550, incorporated herein by reference. Substantially dense composite, herein, is a body having a density greater than 90 percent of theoretical.

The metal-ceramic particulate greenware is densified under conditions of time, atmosphere, temperature and pressure sufficient to density the greenware to a composite having a desired density. The temperature is typically greater than 75 percent of the melt temperature in degrees C of the metal but less than a temperature where substantial volatilization of the metal occurs. For example, the densification temperature for an aluminum-boron carbide system is preferably between 500°C to 1350DC. The time is desirably as short as possible. Preferably the time is at most 24 hours, more preferably at most 2 hours, and most .preferably at most 1 hour. The pressure is desirably ambient or atmospheric pressure. The atmosphere is desirably one that does not adversely affect the densification or chemistry of the CMC.

Preferably, the CMC is produced by infiltrating a porous ceramic body with a metal, thus forming a composite. Ceramic-metal combinations which may be suitable for infiltration are described herein. The infiltrated body may be further consolidated by techniques described hereinabove. More preferably the ceramic of the metal infiltrated ceramic also reacts with the metal, thus forming a new ceramic phase in the dense composite (that is, chemically reactive system). A preferred embodiment of a chemically reactive system is the infiltration of boron carbide with aluminum or alloy thereof, as described below, and in copending U.S. Patent Application Serial No. 08/289,967, filed August 12, 1994, incorporated herein by reference.

Infiltration involves forming a porous ceramic preform (that is, greenware) prepared from ceramic powder by a procedure described hereinabove, such as slip casting (that is, a dispersion of the ceramic powder in a liquid) or pressing (that is, applying pressure to powder in the absence of heat) and then infiltrating a liquid metal into the pores of said preform. Infiltration is the process in which a liquid metal fills the pores of preform in contact with the metal. The process preferably forms a uniformly dispersed and essentially fully dense ceramic-metal composite. Infiltration of the porous preform can be performed by any convenient method for infiltrating a metal into a preform body, such as vacuum infiltration, pressure infiltration and gravity/heat infiltration. Examples of infiltration are described by U.S. Patent Nos. 4,702,770 and 4,834,938, each incorporated herein by reference.

The temperature of infiltration is dependent on the metal to be infiltrated.
Infiltration is preferably performed at a temperature where the metal is molten but below a temperature at which the metal rapidly volatilizes. For example, when infiltrating aluminum or an alloy thereof into a porous ceramic preform, the temperature is preferably at most 1200°C, and more preferably at most 1100CC and preferably at least 750°C, and more preferably at least 900°C. The infiltration time can be any time sufficient to infiltrate the ceramic preform resulting in a desired CMC. The atmosphere can be any atmosphere which does not adversely affect the infiltration of metal or development of said CMC.

The preform may contain, in the case of chemically reactive systems, a ceramic filler material in an amount from 0.1 to 50 weight percent, based upon total preform weight. Filler is material which has no, or a significantly lower, reactivity with the infiltrating metal than a chemically reactive ceramic, such as boron carbide in the boron carbide-aluminum system. For example, when a boron carbide preform contains filler, the preform preferably contains from 70 to 95 wt. percent B4C and from 5 to 30 wt. percent ceramic filler. The percentages are based upon total preform weight. For example, in the boron carbide-aluminum system, the ceramic filler material can be titanium diboride, titanium carbide, silicon boride, aluminum oxide and silicon carbide.

When making, by infiltration, the most preferred CMC (boron carbide-aluminum system) of the brake component, the porous boron carbide preform is desirably baked at a temperature of at least 1400°C prior to infiltration. Baking should continue for at least 15 minutes, desirably at least 30 minutes, and preferably two hours or more.

The baked porous boron carbide preform is then infiltrated with aluminum or alloy thereof by any convenient method described hereinabove.

Ceramic-metal composites resulting from infiltration of baked B4C preforms, in which the metal has to infiltrate distances greater than 0.8 cm, have more uniform microstructures than infiltrated unbaked B4C preforms having the same metal infiltration distance. Although they have a more uniform microstructure, these ceramic-metal composites, because of residual unreacted metal, typically do not have the high temperature strength desired for this invention. In order to overcome this deficiency, the resulting composites (CMCs) typically are subjected to an additional (post-infiltration) heat treatment The infiltrated composite is heat treated at a temperature within a range of from 660°C to 1250°C, preferably from 660°C to 1100°C, and more preferably from 800°C to 950°C, in the presence of air or some other oxygen-containing atmosphere, for a time sufficient to allow slow reactions between residual unreacted metal and B4C or B-AI-C reaction products or both The reactions promote reduction of free (unreacted) metal and development of a uniform microstructure.

Post infiltration heat treating the boron carbide-aluminum composite outside the range of 660°C to 1250°C typically yields unsatisfactory results Temperatures of less than 660°C typically do not result in the residual metal being less than 15 wt percent, based on total composite weight or less. The residual metal is not reduced below 15 percent because the reaction kinetics are very slow Temperatures in excess of 1250°C generally lead to formation of undesirable amounts of aluminum carbide (AI4C3) which is hydrolytically unstable (that is, reacts with water) The aluminum carbide may adversely affect the coefficient of friction of the composite

The post-mf iltration heat treatment has a duration that typically ranges from 1 to 100 hours, desirably from 10 to 75 hours, and preferably from 25 to 75 hours A duration in excess of 100 hours increases production costs, but yields no substantial additional improvements in microstructure over those occurring at 100 hours

The boron carbide-aluminum composite described, hereinabove, typically has a bulk microstructure containing isolated B4C grains or clusters of B4C grains surrounded by a multiphase ceramic matrix, an Al203 surface layer and dispersed noncontiguous unreacted aluminum The ceramic phase comprises at least one of, preferably at least two of, aluminum bondes and aluminum borocarbides. The composite typically comprises from 40 to 75 wt. percent B4C grains, from 20 to 50 wt percent aluminum bondes and aluminum borocarbides and from 2 to 8 wt. percent aluminum or aluminum alloy, all percentages being based upon composite weight and totaling 100 percent. The aluminum bondes and aluminum borocarbides are selected from the group consisting of AIB24C4, AI3BC2, AI4BC, AIB2 and AIB12. The aluminum bondes and borocarbides are desirably AIB24C4 and AIB2, preferably with a ratio of AIB24C4/AIB2 that is within a range of from 10:1 to 1:5. The latter
.range is more preferably from 10:1 to 2:1.

When a ceramic filler material is present in the boron carbide-aluminum CMC, the filler typically is present in the CMC either as isolated grains or as part of the clusters of 5 B4C grains. The amount of ceramic filler material typically is between 1 to 25 volume
percent, based upon total composite volume.

Described below are methods to prepare a CMC useful in making the brake components and friction elements of this invention.

Method 1

10 B4C (ESK specification 1500, manufactured by Elektroschemeltzwerk Kempten of Munich, Germany) having an average particulate size of 3 micrometers in diameter) was dispersed in distilled water to form a suspension. The suspension was ultrasonically
agitated, then adjusted to a pH of 7 by addition of NH4OH and aged for 180 minutes before being cast on a plaster of Par mold to form a porous ceramic body (greenware) having a

15 ceramic content of 69 volume percent. The B4C greenware was dried for 24 hours at 105°C. The greenware sizes were 120 x 120 x 10 millimeters (mm) (thin tiles) and 120 x 120 x 16 mm (thick tiles).

Pieces of the greenware were used as is and after being baked at 1300°C for 120 minutes, baked at 1400°C for 120 minutes, baked at 1800°C for 60 minutes or baked at

20 2200°C for 60 minutes. All baking and sintering take place in a graphite element furnace.
The baked greenware pieces were then infiltrated with molten Al (a specification 1145 alloy, manufactured by Aluminum Company of America that was a commercial grade of Al,
comprising less than 0.55 percent alloying elements such as Si, Fe, Cu and Mn) under a vacuum of 100 millitorr (13.3 Pa) at 1180°C for 120 minutes to provide composite (boron

25 carbide-aluminum composite) pieces.

Composite pieces prepared from the thin tiles were all quite uniform from top to bottom even though some differences were noticeable. As such, the baking temperature does not have a significant impact upon microstructure.

Composite pieces prepared from the thick tiles have nonuniform
- 30 microstructures that varied from bottom (closest to infiltrating metal) to top (farthest from the infiltrating metal) in amount of B-AI-C phases and in phase morphology. The bottoms have a microstructure of equiaxed AIB2 and AI4BC with less than 2 volume percent free Al. The tops have a microstructure of AIB2 and AI4BC grains shaped like 50-100 micrometers long cigars in an Al matrix. The amount of free Al ranged between 5-15 vol. percent.

As shown in Table I, a post-infiltration heat treatment at 690°C in air for 50 hours provided an increase in hardness for ail composite pieces. The data in Table I also show that greenware baked at temperatures below 1800°C yields harder composites than composites made from greenware baked at temperatures above 1800°C. The greenware that was baked at 1400°C and 1700°C resulted in composites with uniform microstructures and high hardness values. The data in Table I further show that green B4C and B4C baked below 1400°C produced uniform and hard parts when limited to small sizes (<10 mm vertical metal flow). As vertical metal flow distances exceeded 10 mm in green (unbaked) B4C and B4C baked below 1400°C, hardness remained relatively high, but resulting parts exhibited nonuniform microstructures. In summary, Table I shows that the CMC of the present invention can be made by various routes. CMCs possessing the required hardness for a friction element in which the CMC contacts a second friction element upon braking (that is, at least 1000 Kg/mm2) can also be made by various routes and desirably the route includes a post infiltration heat treatment (last column of Table I).

Table I



*14.4 Kg load

Method 2

Pieces of greenware were prepared and infiltrated with or without baking, as in Method 1. Chemical analysis of the infiltrated greenware pieces were performed using an MBX-CAMECA microprobe, available from Cameca Co., France. Crystalline phases were identified by X-ray diffraction (XRD) with a Phillips diffractometer using CuKα radiation and a scan rate of 2° per minute. The amount of Al present in the infiltrated greenware (that is, before heat treatment) was estimated based upon differential scanning calorimetry (DSC). All of the greenware pieces were then heated from the melting point of Al (660°C) to 900°C over a period of one hour before 3 x 4 x 45 mm specimens from one-half of the pieces were subjected to Flexure Strength testing using a four-point bend test (ASTM C1161 ) at 900°C. The samples were maintained in air at that temperature for 15 minutes before they were broken. Upper and lower span dimensions were 20 and 40 mm, respectively, and the specimens were broken using a crosshead speed of 0.5 mm/min. Specimens from the other pieces were subjected to an additional heat treatment for 25 hours in air at 690°C before they were heated again to 900°C over a period of one hour and broken in Flexure Strength testing (Last column of Table II).

Table II - Phase Chemistry and Properties


means not measured; * not an example of this invention.

The data in Table II show that the heat treatment history of greenware prior to infiltration has a marked influence upon Flexure Strength of the resultant B4C/AI composites. The data show that the CMC according to this invention was possible without a heat treatment (for example, Examples A, B, C, F, G and H) but it was preferable to heat treat the composite to increase the high temperature strength. The data in Table II also show that the CMC described herein can be achieved by heat treating a sample which does not have the microstructure before heat treatment (for example, Examples D and E). The data also show, particularly for Samples A and G, that metal content alone does not determine strength at elevated temperatures before heat treatment. The strength at high temperature was also affected by ceramic phases formed during infiltration. Samples F, G and H have the highest flexure strength values prior to a post-infiltration heat treatment. This may be due to fast chemical reaction kinetics in conjunction with a sufficient amount of B4C. The data further show that the post-infiltration heat treatment generally leads to an increase in flexure strength.

Similar results are expected with other compositions and process conditions, ail of which are disclosed herein.

Method 3

Composite (B4C-AI) samples having respective initial B4C and Al contents of 75 volume percent and 25 volume percent were prepared by baking B4C greenware at 1300°C for 30 minutes and infiltrating the greenware with the same Al alloy as in Example 1 for 60 minutes at 1 150°C. The greenware, prior to infiltration, was in the form of tiles measuring 120 x 120 x 10 mm. After infiltration, the tiles were ground into 4 x 3 x 45 mm bars. The bars were divided into 4 groups. The first group (Group A) of samples were used as infiltrated, the second (Group B) was heat treated at 800°C in argon for 100 hours, the third (Group C) was heat treated in air at 800°C for 2 hours, the fourth (Group D) was heat treated in air at 800°C for 100 hours. The samples were all subjected to flexure strength testing as described in Example 2, save for changing the temperatures (Table III) at which samples were broken.

Table III



- means not measured

The data in Table III show that strength increased as a result of heat treatment (B, C and D compared to A). The data also show that heat treatment in air resulted in higher strength at high temperatures than heat treatment in inert atmospheres or no heat treatment (C and D compared to A and B).

Method 4

A boron carbide-aluminum composite was made by the same method as the method used to make the heat treated sample H in Table II. This sample was tested against itself by an unlubricated pin on disk method at varying loads. The pin on disk method used was described herein. The sample has a coefficient of friction of 1.8 at a load of 1 pound and a coefficient of friction of 1.7 at a load of 2 pounds. The wear scar diameter was 0.8 mm at a 1 pound load, 1.0 mm at a 2 pound load and 1.2 mm at a 3 pound load.