# US 5,708,956 A · Single step synthesis and densification of ceramic-ceramic and ceramic-metal composite materials

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- Number: US 5,708,956 A
- Document ID: US5708956A
- Status: Granted
- Kind: A
- Application number: 08/537,490
- Filed: 1995-10-02
- Granted: 1998-01-13
- Earliest claimed: 1995-10-02
- Assignees: The Dow Chemical Company
- Inventors: Stephen D. Dunmead; Michael J. Romanowski
- Web page: https://patentgrep.com/patent/US5708956A

## CPC

- C04B 35/6267: {Pyrolysis, carbonisation or auto-combustion reactions}
- C22C 29/00: Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides {(C22C26/00 takes precedence)}
- B22F 2999/00: Aspects linked to processes or compositions used in powder metallurgy
- C22C 1/057: with in situ formation of phases other than hard compounds by solid state reaction sintering, e.g. metal phase formed by reduction reaction
- C04B: LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE {(roofing granules E04D7/005)}; CERAMICS (devitrified glass-ceramics C03C10/00); REFRACTORIES; TREATMENT OF NATURAL STONE
- C22C: ALLOYS (treatment of alloys C21D, C22F)
- B22F: WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER (making alloys by powder metallurgy C22C); APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER

## Abstract

Ceramic-ceramic and ceramic-metal composite materials are disclosed which contain at least two ceramic phases and at least one metallic phase. At least one of these ceramic phases is a metal boride or mixture of metal borides and another of the ceramic phases is a metallic nitride, metallic carbide, or a mixture of metallic nitride and a metallic carbide. These composite materials may be made by a combustion synthesis process which includes the step of igniting a mixture of at least one element selected from titanium, zirconium, hafnium, vanadium, niobium, tantalum, chromium, molybdenum, tungsten, aluminum and silicon, or a combination of two or more thereof, at least one boron compound selected from boron nitride, boron carbide, or a combination thereof and an ignition temperature reducing amount of a metal selected from iron, cobalt, nickel, copper, aluminum, silicon, palladium, platinum, silver, gold, ruthenium, rhodium, osmium, and iridium, or a mixture of two or more thereof, provided that at least one of the aforementioned elements is different from at least one of the aforementioned metals. This process permits a high degree of control over the microstructure of the product and relatively low pressures are required to obtain high composite material density. A densified product having high density and a finely grained microstructure may be obtained by applying mechanical pressure during combustion synthesis. The composites have improved hardness, toughness, strength, resistance to wear, and resistance to catastrophic failure.

## Claims

### Claim 1

A process for making a multi-phase composite material by combustion synthesis which comprises:
(a) providing an ignitable mixture having a reduced ignition temperature by mixing (1) at least one element selected from the group consisting of titanium, zirconium, hafnium, vanadium, niobium, tantalum, chromium, molybdenum, tungsten, aluminum and silicon, and a mixture of two or more thereof (2) at least one of boron nitride and boron carbide, and (3) an ignition temperature reducing amount of a metal selected from the group consisting of iron, cobalt, nickel, copper, aluminum, silicon, palladium, platinum, silver, gold, ruthenium, rhodium, osmium, and iridium, or a mixture of two or more thereof, provided that at least one element is different from at least one metal, and
(b) igniting the mixture prepared in (a) to essentially completely react the at least one element selected from the group consisting of titanium, zirconium, molybdenum, tungsten, aluminum and silicon, and a mixture of two or more thereof with the at least one of boron nitride and boron carbide.

### Claim 2 (depends on 1)

The process according to claim 1 wherein the ignition temperature is within the range from about 1800.degree. C. to 1400.degree. C.

### Claim 3 (depends on 1)

The process according to claim 1 wherein the ignition temperature is within the range from about 900.degree. C. to about 1200.degree. C.

### Claim 4 (depends on 1)

The process according to claim 1 wherein the product produced by combustion synthesis initiated by step (b) is held at a temperature in the range from 1000.degree. C. to 2000.degree. C. for a time period from about 1 minute to about 2 hours following ignition.

### Claim 5 (depends on 1)

The process according to claim 1 wherein the product produced by combustion synthesis initiated by step (b) is held at a temperature in the range from about 1200.degree. C. to 1600.degree. C. for a time period from about 5 minutes to about 30 minutes following ignition.

### Claim 6 (depends on 1)

The process according to claim 1 comprising:
(c) applying mechanical pressure during the combustion synthesis initiated by ignition step (b).

### Claim 7 (depends on 6)

The process according to claim 6 wherein the pressure applied is in the range from about 5 MPa to about 55 MPa.

### Claim 8 (depends on 6)

The process according to claim 6 wherein the pressure applied is less than 30 MPa.

### Claim 9 (depends on 1)

The process according to claim 1 wherein at least one element of the ignitable mixture (a) is titanium or zirconium and the ignition temperature reducing amount of metal in step (a) comprises nickel.
