# US 4,396,587 A · Method for manufacture of silicon nitride

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- Number: US 4,396,587 A
- Document ID: US4396587A
- Status: Granted
- Kind: A
- Application number: 06/294,027
- Filed: 1981-08-18
- Granted: 1983-08-02
- Earliest claimed: 1980-08-29
- Assignees: Asahi-Dow Limited
- Inventors: Masami Yamaguchi; Yoshirou Tajitsu; Yoshiharu Kitahama; Isamu Iwami
- Web page: https://patentgrep.com/patent/US4396587A

## CPC

- C01B 21/0685: {Preparation by carboreductive nitridation}
- C04B 35/584: based on silicon nitride
- C01P 2004/03: obtained by SEM
- C01P 2004/10: extending in one dimension, e.g. needle-like
- C01P 2004/62: Submicrometer sized, i.e. from 0.1-1 micrometer
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- 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
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

Silicon nitride of improved quality is obtained by using a liquid silicic acid or modified liquid silicic acid as a silicic substance and carbon in a powdered form, a precursor of carbon in a powdered form, or a precursor of carbon in the form of a solution as a carbonaceous substance, and thermally treating these raw materials in a non-oxidative atmosphere containing nitrogen. By this method, .alpha.-type silicon nitride can be easily obtained. Particularly, finely divided .alpha.-type silicon nitride suitable for use as the raw material for the production of high-strength sintered articles is also produced. .alpha.-type silicon nitride whiskers useful as a reinforcing material for ceramic and metallic articles is also obtained.

## Claims

### Claim 1

A method for the manufacture of silicon nitride having a particle diameter of at most 1.5 microns which comprises subjecting a homogeneous mixture of a liquid silicic acid or a modified liquid silicic acid with carbon in the form of powder or a solution to a heat treatment at a temperature of 1300.degree. C. to 1600.degree. C. in a non-oxidizing atmosphere containing nitrogen.

### Claim 2 (depends on 1)

A method according to claim 1, wherein the liquid silicic acid is a solution or sol of silicic acid obtained by neutralization or dealkalinization of an aqueous alkali silicate solution.

### Claim 3 (depends on 1)

A method according to claim 1, wherein the liquid silicic acid is a solution or sol of silicic acid obtained by hydrolysis of a hydrolyzable silicon compound.

### Claim 4 (depends on 1)

A method according to claim 1, wherein the carbon in the form of powder is a carbon black or an activated carbon.

### Claim 5 (depends on 2)

A method according to claim 2, wherein the carbon in the form of powder is a carbon black or activated carbon.

### Claim 6 (depends on 1)

A method according to claim 1, wherein the precursor of carbon is a carbohydrate or a derivative thereof, a protein substance or a derivative thereof, a vinyl polymer or a derivative thereof, a thermosetting resin, or a petroleum pitch.

### Claim 7 (depends on 2)

A method according to claim 2, wherein the precursor or carbon is a carbohydrate or a derivative thereof, a protein substance or a derivative thereof, a vinyl polymer or a derivative thereof, a thermosetting resin, or a petroleum pitch.

### Claim 8 (depends on 1)

A method according to claim 1, wherein the precursor of carbon is starch or a hydrolyzate thereof, cellulose, hemi-cellulose, hydroxyethyl cellulose, arginic acid, pectin, natural gum, dextrin, dextran, sucrose, maltose, glucose, gluten, casein, polyvinyl alcohol, polyacrylonitrile, polyvinyl chloride, polyvinylidene chloride, polyvinyl acetate, polybutadiene, phenol resin, urea resin, or petroleum pitch.

### Claim 9 (depends on 1)

A method accordiang to claim 1, wherein the precursor of carbon is starch, glucose, sucrose, alginic acid, casein, hydroxyethyl cellulose, or polyvinyl alcohol.

### Claim 10 (depends on 1)

A method according to claim 1, wherein the precursor of carbon is a carbohydrate or a derivative thereof.

### Claim 11 (depends on 1)

A method according to claim 1, wherein the precursor of carbon is starch or hydrolyzate thereof.

### Claim 12

A method for the manufacture of silicon nitride having a particle diameter of at most 1.5 microns which comprises forming a homogeneous mixture of a liquid silicic acid or a modified liquid silicic acid with carbon in the form of a powder or a precursor of carbon in the form of powder or a solution, precipitating the mixture, and heat treating the precipitate at a temperature of 1300.degree. C. to 1600.degree. C. in a non-oxidizing atmosphere containing nitrogen.

### Claim 13

A method for the manufacture of silicon nitride having a particle diameter of at most 1.5 microns which comprises forming a homogeneous mixture of a liquid silicic acid or a modified liquid silicic acid with carbon in the form of powder or a precursor of carbon in the form of powder or a solution, drying the mixture, and heat treating the dried mixture at a temperature of 1300.degree. C. to 1600.degree. C. in a non-oxidizing atmosphere containing nitrogen.

### Claim 14 (depends on 13)

A method according to claim 13, wherein the drying is performed by spray-drying.