US5053365A
Expired / Lapsed
US
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Method for the low temperature preparation of amorphous boron nitride using alkali metal and haloborazines
Assignee: Ohio State University Research Foundation
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Filing: 1990-02-28
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Granted: 1991-10-01
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Expires: 2010-02-28
Abstract
Abstract The invention relates to an energy efficient method for the production of boron nitride materials at temperatures of from about 100 degrees to about 230 degrees Centigrade. The boron nitride materials produced by the present invention are carbon-free and are prepared by combining at reduced pressure an alkali metal, such as potassium, rubidium, cesium, or mixtures thereof, or a potassium/sodium mixture, with a boron-, nitrogen-, and halogen-containing material, such as a haloborazine, haloborazane, or haloaminoborane. The preferred boron-, nitrogen-, and halogen-containing materials are trihalogenated, the preferred halogen is chlorine, and the preferred alkali metal is cesium.
Inventors
- 👤 Sheldon G. Shore
- 👤 Shawn E. Dolan
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-06 13:21
CPC Classifications
C; C01; C01B; C01B21/00; C01B21/06; C01B21/064
Claims Analysis
Total Claims: 32
Claim 1
Independent Claim
98 words
A method for preparing carbon-free boron nitride comprising the steps: combining substantially in the absence of oxygen and at reduced vapor pressure, an alkali metal selected from the group consisting of potassium, rubidium, cesium, and mixtures thereof with a boron-, nitrogen, and halogen-containing compound to form a mixture, wherein the alkali metal and the boron-, nitrogen-, and halogen-containing compound are present in the mixture in a mole ratio of from about 1 to 100 to about 5 to 1, respectively, and heating the mixture to a temperature above about 100 degrees Centigrade and below about 230 degrees Centigrade.
Claim 2
Independent Claim
98 words
A method for preparing carbon-free boron nitride comprising the steps: combining substantially in the absence of oxygen and at reduced vapor pressure, an alkali metal selected from the group consisting of potassium, rubidium, cesium, and mixtures thereof with a boron-, nitrogen, and halogen-containing compound to form a mixture, wherein the alkali metal and the boron-, nitrogen-, and halogen-containing compound are present in the mixture in a mole ratio of from about 1 to 100 to about 5 to 1, respectively, and heating the mixture to a temperature above about 100 degrees Centigrade and below about 230 degrees Centigrade.
Claim 3
Dependent Claim
29 words
The method of claim 1 wherein the boron-, nitrogen-, and halogen-containing compound is selected from the group consisting of trihaloborazines, dihaloborazines, monohaloborazines, trihaloborazanes, dihaloborazines, monohaloborazines, trihaloaminoborane, dihaloaminoborane, and monohaloaminoborane.
Claim 4
Dependent Claim
38 words
The method of claim 1 wherein the alkali metal and the boron-, and nitrogen-, and halogen-containing compound are combined in a vessel at a pressure in the range of from about 0.1×10 -5 Torr to about one atmosphere.
Claim 5
Dependent Claim
23 words
The method of claim 1 further comprising the step of removing alkali metal halide by-products by water washing of the boron nitride produced.
Claim 6
Dependent Claim
27 words
The method of claim 1 further comprising the step of removing from the boron nitride any alkali metal halide by-products by sublimation of said alkali metal halide.
Claim 7
Dependent Claim
23 words
The method of claim 1 wherein the alkali metal is preheated and vaporized before being combined with the boron-, nitrogen-, and halogen-containing compound.
Claim 8
Dependent Claim
23 words
The method of claim 1 wherein the boron-, nitrogen-, and halogen-containing compound is preheated and vaporized before being combined with the alkali metal.
Claim 9
Dependent Claim
24 words
The method of claim 1 wherein the boron-, nitrogen-, and halogen-containing compound and the alkali metal are both preheated and vaporized before being combined.
Claim 10
Dependent Claim
56 words
The method of claim 1 wherein the boron-, nitrogen-, and halogen-containing compound is B-trichloroborazine, the alkali metal is cesium, the B-trichloroborazine and the cesium are combined in a vessel at a reduced pressure of less than about 0.1×10 -1 Torr, and wherein the mixture is then heated to a temperature of above about 100 degrees Centigrade.
Claim 11
Dependent Claim
56 words
The method of claim 1 wherein the boron-, nitrogen-, and halogen-containing compound is B-trichloroborazine, the alkali metal is rubidium, the B-trichloroborazine and the rubidium are combined in a vessel at a reduced pressure of less than about 0.1×10 -1 Torr, and wherein the mixture is then heated to a temperature of above about 180 degrees Centigrade.
Claim 12
Dependent Claim
56 words
The method of claim 1 wherein the boron-, nitrogen-, and halogen-containing compound is B-trichloroborazine, the alkali metal is potassium, the B-trichloroborazine and the potassium are combined in a vessel at a reduced pressure of less than about 0.1×10 -1 Torr, and wherein the mixture is then heated to a temperature of above about 220 degrees Centigrade.
Claim 13
Dependent Claim
57 words
The method of claim 1 wherein the boron-, nitrogen-, and halogen-containing compound is B-tribromoborazine, the alkali metal is cesium, the B-tribromobcrazine and the cesium are combined in a vessel at a reduced pressure of less than about 0.1×10 -1 Torr, and wherein the mixture is then heated to a temperature between about 100 and 120 degrees Centigrade.
Claim 14
Dependent Claim
57 words
The method of claim 1 wherein the boron-, nitrogen-, and halogen-containing compound is B-tribromoborazine, the alkali metal is rubidium, the B-tribromoborazine and the rubidium are combined in a vessel at a reduced pressure of less than about 0.1×10 -1 Torr, and wherein the mixture is then heated to a temperature between about 130 and 150 degrees Centigrade.
Claim 15
Dependent Claim
57 words
The method of claim 1 wherein the boron-, nitrogen-, and halogen-containing compound is B-tribromoborazine, the alkali metal is potassium, the B-tribromoborazine and the potassium are combined in a vessel at a reduced pressure of less than about 0.1×10 -1 Torr, and wherein the mixture is then heated to a temperature between about 210 and 230 degrees Centigrade.
Claim 16
Dependent Claim
55 words
The method of claim 1 wherein the boron-, nitrogen-, and halogen-containing compound is B-trifluoroborazine, the alkali metal is cesium, the B-trifluoroborazine and the cesium are combined in a vessel at a reduced pressure of about 0.1×10 -1 Torr, and wherein the mixture is then heated to a temperature between about 100 and 140 degrees Centigrade.
Claim 17
Dependent Claim
57 words
The method of claim 1 wherein the boron-, nitrogen-, and halogen-containing compound is B-trifluoroborazine, the alkali metal is rubidium, the B-trifluoroborazine and the rubidium are combined in a vessel at a reduced pressure of less than about 0.1×10 -1 Torr, and wherein the mixture is then heated to a temperature between about 100 and 150 degrees Centigrade.
Claim 18
Dependent Claim
57 words
The method of claim 1 wherein the boron-, nitrogen-, and halogen-containing compound is B-trifluoroborazine, the alkali metal is potassium, the B-trifluoroborazine and the potassium are combined in a vessel at a reduced pressure of less than about 0.1×10 -1 Torr, and wherein the mixture is then heated to a temperature between about 100 and 200 degrees Centigrade.
Claim 19
Dependent Claim
54 words
The method of claim 1 wherein the boron-, nitrogen-, and halogen-containing compound is B-trichloroborazane, the alkali metal is cesium, the B-trichloroborazane and the cesium are combined in a vessel at a reduced pressure of less than about 0.1×10 -1 Torr, and wherein the mixture is then heated to a temperature above 125 degrees Centigrade.
Claim 20
Dependent Claim
55 words
The method of claim 1 wherein the boron-, nitrogen-, and halogen-containing compound is B-trichloroborazane, the alkali metal is rubidium, the B-trichloroborazane and the rubidium are combined in a vessel at a reduced pressure of less than about 0.1×10 -1 Torr, and wherein the mixture is then heated to a temperature above about 160 degrees Centigrade.
Claim 21
Dependent Claim
55 words
The method of claim 1 wherein the boron-, nitrogen-, and halogen-containing compound is B-trichloroborazane, the alkali metal is potassium, the B-trichloroborazane and the potassium are combined in a vessel at a reduced pressure of less than about 0.1×10 -1 Torr, and wherein the mixture is then heated to a temperature above about 180 degrees Centigrade.
Claim 22
Dependent Claim
57 words
The method of claim 1 wherein the boron-, nitrogen-, and halogen-containing compound is B-tribromoborazane, the alkali metal is cesium, the B-tribromoborazane and the cesium are combined in a vessel at a reduced pressure of less than about 0.1×10 -1 Torr, and wherein the mixture is then heated to a temperature between about 100 and 230 degrees Centigrade.
Claim 23
Dependent Claim
57 words
The method of claim 1 wherein the boron-, nitrogen-, and halogen-containing compound is B-tribromoborazane, the alkali metal is rubidium, the B-tribromoborazane and the rubidium are combined in a vessel at a reduced pressure of less than about 0.1×10 -1 Torr, and wherein the mixture is then heated to a temperature between about 100 and 230 degrees Centigrade.
Claim 24
Dependent Claim
57 words
The method of claim 1 wherein the boron-, nitrogen-, and halogen-containing compound is B-tribromoborazane, the alkali metal is potassium, the B-tribromoborazane and the potassium are combined in a vessel at a reduced pressure of less than about 0.1×10 -1 Torr, and wherein the mixture is then heated to a temperature between about 100 and 230 degrees Centigrade.
Claim 25
Dependent Claim
57 words
The method of claim 1 wherein the boron-, nitrogen-, and halogen-containing compound is B-trifluoroborazane, the alkali metal is cesium, the B-trifluoroborazane and the cesium are combined in a vessel at a reduced pressure of less than about 0.1×10 -1 Torr, and wherein the mixture is then heated to a temperature between about 100 and 230 degrees Centigrade.
Claim 26
Dependent Claim
57 words
The method of claim 1 wherein the boron-, nitrogen-, and halogen-containing compound is B-trifluoroborazane, the alkali metal is rubidium, the B-trifluoroborazane and the rubidium are combined in a vessel at a reduced pressure of less than about 0.1×10 -1 Torr, and wherein the mixture is then heated to a temperature between about 100 and 230 degrees Centigrade.
Claim 27
Dependent Claim
57 words
The method of claim 1 wherein the boron-, nitrogen-, and halogen-containing compound is B-trifluoroborazane, the alkali metal is potassium, the B-trifluoroborazane and the potassium are combined in a vessel at a reduced pressure of less than about 0.1×10 -1 Torr, and wherein the mixture is then heated to a temperature between about 100 and 230 degrees Centigrade.
Claim 28
Dependent Claim
82 words
The method of claim 1 wherein the boron-, nitrogen-, and halogen-containing compound is an aminohaloborane selected from the group consisting of NH 3 BCl 3 , NH 3 BHCl 2 , NH 3 BH 2 Cl, NH 3 BF 3 , NH 3 BHF 2 , NH 3 BH 2 F, NH 3 BBr 3 , NH 3 BHBr 2 , NH 3 BH 2 Br, NH 3 BI 3 , NH 3 BHI 2 , and NH 3 BH 2 I.
Claim 29
Independent Claim
104 words
A method for preparing carbon-free boron nitride comprising the steps: combining substantially in the absence of oxygen and at reduced pressure, a composition of sodium and potassium, wherein the atom ratio of sodium to potassium is from about 1 to 4 to about 1 to about 99, with a boron-, nitrogen-, and halogen-containing compound to form a mixture, wherein the potassium-sodium composition and the boron-, nitrogen-, and halogen-containing compound are present in the mixture in a mole ratio of from about 1 to 100 to about 5 to 1, respectively, and heating the mixture to a temperature between 275 and about 300 degrees Centigrade.
Claim 30
Independent Claim
104 words
A method for preparing carbon-free boron nitride comprising the steps: combining substantially in the absence of oxygen and at reduced pressure, a composition of sodium and potassium, wherein the atom ratio of sodium to potassium is from about 1 to 4 to about 1 to about 99, with a boron-, nitrogen-, and halogen-containing compound to form a mixture, wherein the potassium-sodium composition and the boron-, nitrogen-, and halogen-containing compound are present in the mixture in a mole ratio of from about 1 to 100 to about 5 to 1, respectively, and heating the mixture to a temperature between 275 and about 300 degrees Centigrade.
Claim 31
Dependent Claim
29 words
The method of claim 28 wherein the boron-, nitrogen-, and halogen-containing compound is selected from the group consisting of trihaloborazines, dihaloborazines, monohaloborazines, trihaloborazanes, dihaloborazines, monohaloborazines, trihaloaminoborane, dihaloaminoborane, and monohaloaminoborane.
Claim 32
Dependent Claim
19 words
The method of claim 28 wherein the mixture of sodium and potassium has the general composition K 2 Na.
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