Process for preparing fine powders of aluminum nitride

• US 5,151,260 A
• Filed: 12/19/1990
• Issued: 09/29/1992
• Est. Priority Date: 12/21/1989
• Status: Expired due to Fees

• Current Assignee: Temav SPA Venezia-Porto Marghera Italy
• Original Assignee: Temay SPA
• Inventors: Beaulardi, Leandro, Contursi, Luigi
• Primary Examiner(s): LANGEL, WAYNE A
• Application Number:
  US07/629,997
• Time in Patent Office: 650 Days
• Field of Search: 423/412, 423/625
• US Class Current: 423/412
• CPC Class Codes: C01B 21/0726 Preparation by carboreductive nitridation

Abstract

Disclosed is a process for preparing fine powders of aluminum nitride, by starting from an aqueous solution of an inorganic aluminum salt, characterized in that said process comprises the following steps:

(a) the anion of the inorganic salt of aluminum is at least partially removed by heating, with a colloidal solution of an aluminum compound being obtained;

(b) carbon powder is dispersed in said colloidal solution, with a suspension of an aluminum compound and carbon being obtained;

(c) said suspension is mixed with a carbohydrate, with a suspension being obtained of an aluminum compound and carbon in a solution which contains the carbohydrate;

(d) the suspension obtained from the (c) step is sprayed onto, or dropwise added to, an alkaline solution, with spherical bodies being obtained, which contain aluminum hydroxide and carbon;

(e) said spherical bodies are carbothermally reduced and nitrided at a temperature comprised within the range of from 1350° to 1650° C. for a time comprised within the range of from 1 to 24 hours, so that powders containing aluminum nitride are obtained;

(f) carbon is removed from said powders by a calcination carried out at a temperature comprised within the range of from 600° to 700° C., for a time comprised within the range of from 1 to 7 hours, under an oxygen-containing atmosphere.

Claims

1. Process for preparing fine powders of aluminum nitride, by starting from an aqueous solution of an inorganic aluminum salt, wherein said process comprises:

(a) removing the anion of the inorganic aluminum salt at least partially by heating, with a colloidal solution of an aluminum compound being obtained;

(b) dispersing carbon powder in said colloidal solution, with a suspension of an aluminum compound and carbon being obtained;

(c) mixing said suspension with a carbohydrate, with a suspension being obtained of an aluminum compound and carbon in a solution which contains the carbohydrate;

(d) adding the suspension obtained from the (c) step to an alkaline solution, with spherical bodies being obtained which contain aluminum hydroxide and carbon;

(e) reducing and nitriding said spherical bodies carbothermally at a temperature of from 1350°

to 1650°

C. for a time of from 1 to 24 hours, so that powders containing aluminum nitride are obtained; and

(f) removing carbon from said powders by a calcination step carried out at a temperature of from 600°

to 700°

C., for a time of from 1 to 7 hours, under an oxygen-containing atmosphere.

2. Process according to claim 1, in which the carbohydrate to be mixed with the suspension in the (c) step is added in solution.

3. Process according to claim 1, in which the carbohydrate is a polysaccharide.

4. Process according to claim 3, in which the polysaccharide is methyl-cellulose.

5. Process according to claim 1, in which the carbon powder dispersed in the colloidal solution is comprised of particles having a particle size smaller than 40 nm.

6. Process according to claim 1, in which the heating in the (a) step is carried out in a microwave oven.