# US 5,344,634 A · Method of nitriding silicon

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- Number: US 5,344,634 A
- Document ID: US5344634A
- Status: Granted
- Kind: A
- Application number: 07/972,070
- Filed: 1992-11-03
- Granted: 1994-09-06
- Earliest claimed: 1990-07-24
- Assignees: Eaton Corporation
- Inventors: James P. Edler
- Web page: https://patentgrep.com/patent/US5344634A

## CPC

- C04B 35/591: obtained by reaction sintering
- 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

## Abstract

A process for nitriding materials containing silicon to form a silicon nitride material predominantly in the alpha phase is disclosed which includes nitriding the silicon-containing material by (a) heating the silicon-containing material in an atmosphere containing at least hydrogen in the temperature range of about 0.degree. C. to about 1420.degree. C. and (b) thereafter, nitriding the silicon-containing material by heating the material in a nitriding atmosphere containing at least nitrogen gas in the temperature range of from about 1000.degree. C. to about 1450.degree. C.

## Claims

### Claim 1

A process for nitriding materials containing silicon to form a silicon nitride material predominantly in the alpha-phase, comprising:
(a) heating the silicon-containing material in an atmosphere containing at least hydrogen to a first temperature in the temperature range of from about 0.degree. C. to about 1000.degree. C. and
(b) thereafter, continuously heating from the first temperature to a second temperature in the temperature range of from about 1000.degree. C. to about 1450.degree. C. and nitriding the silicon-containing material by subjecting the silicon-containing material to a nitriding atmosphere while continuously heating to the second temperature to effect nitriding, said nitriding atmosphere containing at least nitrogen gas.

### Claim 2

A method of nitriding a silicon-containing material, consisting essentially of the steps of:
(a) heating the silicon-containing material in an atmosphere containing at least hydrogen in a temperature range of from about 0.degree. C. to about 1000.degree. C. and
(b) thereafter, nitriding the silicon-containing material by heating in an atmosphere containing at least nitrogen in the temperature range of from about 1000.degree. C. to about 1450.degree. C.

### Claim 3 (depends on 2)

The method of claim 2, wherein the silicon-containing material includes silicon metal.

### Claim 4 (depends on 2)

The method of claim 2, wherein the heating in step (a) is performed in the temperature range of from about 20.degree. C. to about 1000.degree. C.

### Claim 5 (depends on 2)

The method of claim 2, wherein the heating step (a) is performed to a maximum temperature of from about 500.degree. C. to about 1000.degree. C.

### Claim 6 (depends on 2)

The method of claim 2, wherein the heating of the silicon-containing material in the atmosphere containing at least hydrogen is performed at a temperature greater than 200.degree. C.

### Claim 7 (depends on 2)

The method of claim 2, wherein the atmosphere containing at least hydrogen contains at least about 1 mole percent hydrogen.

### Claim 8 (depends on 2)

The method of claim 2, wherein the atmosphere containing at least hydrogen contains at least about 5 mole percent hydrogen.

### Claim 9 (depends on 2)

The method of claim 2, wherein the atmosphere containing at least hydrogen contains at least about 25 mole percent hydrogen.

### Claim 10 (depends on 2)

The method of claim 2, wherein the atmosphere containing at least hydrogen is 100% hydrogen.

### Claim 11 (depends on 2)

The method of claim 2, wherein the silicon-containing material has a minimum thickness of about 1/2 inch.

### Claim 12 (depends on 2)

The method of claim 2, wherein the silicon-containing material has a minimum thickness of about 1 inch.

### Claim 13 (depends on 1)

The method of claim 1, wherein the heating of the silicon-containing material in the atmosphere containing at least hydrogen is performed at a temperature greater than 200.degree. C.

### Claim 14 (depends on 1)

The method of claim 1, wherein the atmosphere containing at least hydrogen contains at least about 25 mole percent hydrogen.

### Claim 15 (depends on 1)

The method of claim 1, wherein the atmosphere containing at least hydrogen is 100% hydrogen.

### Claim 16 (depends on 1)

The method of claim 1, further comprising, prior to heating the silicon-containing material in an atmosphere containing at least hydrogen, the steps of:
admixing an organic binder with the silicon-containing material and
pressing the silicon-containing material-organic binder admix into a green body part, the organic binder being admixed at a level which provides the green body part with sufficient strength to allow machining without the need for partially nitriding or sintering the green body part.

### Claim 17 (depends on 2)

The method of claim 2, further comprising, prior to heating the silicon-containing material in an atmosphere containing at least hydrogen, the steps of:
admixing an organic binder with the silicon-containing material and
pressing the silicon-containing material-organic binder admix into a green body part, the organic binder being admixed at a level which provides the green body part with sufficient strength to allow machining without the need for partially nitriding or sintering the green body part.

### Claim 18

A method of nitriding a silicon-containing material, comprising the steps of:
(a) heating the silicon-containing material in an atmosphere containing at least hydrogen to a first temperature in the temperature range of from about 0.degree. C. to about 1000.degree. C. and
(b) thereafter, nitriding the silicon-containing material by heating in an atmosphere containing at least nitrogen in an atmosphere containing at least nitrogen in the temperature range of from about 1000.degree. C. to about 1450.degree. C.

### Claim 19

A method of nitriding silicon-containing material in powder form, comprising the steps of:
(a) heating the silicon-containing material in powder form in an atmosphere containing at least hydrogen in the temperature range of from about 0.degree. C. to about 1000.degree. C. and
(b) thereafter, nitriding the silicon-containing material in powder form by heating in an atmosphere containing at least nitrogen in the temperature range of from about 1000.degree. C. to about 1450.degree. C.

### Claim 20 (depends on 19)

The method of claim 19, wherein the heating of the silicon-containing material in the atmosphere containing at least hydrogen is performed at a temperature greater than 200.degree. C.

### Claim 21 (depends on 19)

The method of claim 19, wherein the atmosphere containing at least hydrogen contains at least about 25 mole percent hydrogen.

### Claim 22 (depends on 19)

The method of claim 19, wherein the atmosphere containing at least hydrogen is 100% hydrogen.
