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US5350719A
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Preparation of titanium nitride-containing refractory material composites
Assignee: NATIONAL INSTITUTE FOR STRATEGIC TECHNOLOGY
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Filing: 1992-11-06
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Granted: 1994-09-27
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Expires: 2012-11-06
Abstract
Abstract A titanium tetrahalide is reacted with a disilazane to prepare a titanium containing organometallic precursor, which is thereafter mixed with a refractory material powder and pyrolyzed to form a titanium nitride-containing refractory material composite containing crystalline titanium nitride.
Inventors
- 👤 Chaitanya K. Narula
- 👤 Gary M. Crosbie
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-09 01:14
CPC Classifications
C; C04; C04B; C04B35/00; C04B35/515; C04B35/58; C04B35/58007; C04B35/58014; C04B35/584
Claims Analysis
Total Claims: 17
Claim 1
Independent Claim
129 words
A process for preparing a titanium nitride-containing refractory material solid composite, comprising the steps of: A) contacting a titanium tetrahalide with a disilazane at a temperature and for a period of time sufficient to prepare a titanium-containing organometallic precursor; B) mixing the titanium-containing organometallic precursor with a refractory material powder, the weight ratio of titanium-containing organometallic precursor to refractory material powder being from about 1:50 to about 1:1; C) heating the mixture of titanium-containing organometallic precursor and refractory material powder in an inert atmosphere to a temperature of at least about 600° C. and for a period of time sufficient to pyrolyze the precursors; and D) further heating the pyrolyzed mixture at a temperature of at least about 1,600° C. to densify the pyrolyzed mixture to a solid composite.
Claim 2
Dependent Claim
129 words
A process for preparing a titanium nitride-containing refractory material solid composite, comprising the steps of: A) contacting a titanium tetrahalide with a disilazane at a temperature and for a period of time sufficient to prepare a titanium-containing organometallic precursor; B) mixing the titanium-containing organometallic precursor with a refractory material powder, the weight ratio of titanium-containing organometallic precursor to refractory material powder being from about 1:50 to about 1:1; C) heating the mixture of titanium-containing organometallic precursor and refractory material powder in an inert atmosphere to a temperature of at least about 600° C. and for a period of time sufficient to pyrolyze the precursors; and D) further heating the pyrolyzed mixture at a temperature of at least about 1,600° C. to densify the pyrolyzed mixture to a solid composite.
Claim 3
Dependent Claim
21 words
The process for preparing a titanium nitride-containing refractory material composite according to claim 1, wherein the titanium tetrahalide comprises titanium tetrachloride.
Claim 4
Dependent Claim
19 words
The process for preparing a titanium nitride-containing refractory material composite according to claim 1, wherein the disilazane comprises hexamethyldisilazane.
Claim 5
Dependent Claim
30 words
The process for preparing a titanium nitride-containing refractory material composite according to claim 1, wherein the mole ratio of titanium tetrahalide to disilazane is from about 1:0.5 to about 1.3.
Claim 6
Dependent Claim
25 words
The process for preparing a titanium nitride-containing refractory material composite according to claim 4, wherein the mole ratio is from about 1:1 to about 1:2.
Claim 7
Dependent Claim
25 words
The process for preparing a titanium nitride-containing refractory material composite according to claim 1, wherein step A is conducted in the presence of a solvent.
Claim 8
Dependent Claim
29 words
The process for preparing a titanium nitride-containing refractory material composite according to claim 1, wherein step A is conducted at temperature from about -100° C. to about 100° C.
Claim 9
Dependent Claim
25 words
The process for preparing a titanium nitride-containing refractory material composite according to claim 1, wherein the refractory material powder comprises Si 3 N 4 .
Claim 10
Dependent Claim
157 words
A process for preparing a titanium nitride-containing refractory material composite, comprising the steps of: A) contacting a titanium tetrahalide with a disilazane, the mole ratio of titanium tetrahalide to disilazane being from about 1:0.5 to about 1:3, optionally in the presence of a solvent, at a temperature from about -100° C. to about 100° C. and for a period of time sufficient to prepare a titanium-containing organometallic precursor; B) mixing the titanium-containing organometallic precursor with a refractory material powder, the weight ratio of titanium-containing organometallic precursor to refractory material powder being from about 1:50 to about 1:1; C) heating the mixture of titanium-containing organometallic precursor and refractory material powder in an inert atmosphere to a temperature of at least about 600° C. for a period of time sufficient to pyrolyze the precursor; and D) further heating the pyrolyzed mixture at a temperature of at least about 1,600° C. to densify the pyrolyzed mixture to a solid composite.
Claim 11
Dependent Claim
157 words
A process for preparing a titanium nitride-containing refractory material composite, comprising the steps of: A) contacting a titanium tetrahalide with a disilazane, the mole ratio of titanium tetrahalide to disilazane being from about 1:0.5 to about 1:3, optionally in the presence of a solvent, at a temperature from about -100° C. to about 100° C. and for a period of time sufficient to prepare a titanium-containing organometallic precursor; B) mixing the titanium-containing organometallic precursor with a refractory material powder, the weight ratio of titanium-containing organometallic precursor to refractory material powder being from about 1:50 to about 1:1; C) heating the mixture of titanium-containing organometallic precursor and refractory material powder in an inert atmosphere to a temperature of at least about 600° C. for a period of time sufficient to pyrolyze the precursor; and D) further heating the pyrolyzed mixture at a temperature of at least about 1,600° C. to densify the pyrolyzed mixture to a solid composite.
Claim 12
Dependent Claim
21 words
The process for preparing a titanium nitride-containing refractory material composite according to claim 9, wherein the titanium tetrahalide comprises titanium tetrachloride.
Claim 13
Dependent Claim
19 words
The process for preparing a titanium nitride-containing refractory material composite according to claim 9, wherein the disilazane comprises hexamethyldisilazane.
Claim 14
Dependent Claim
30 words
The process for preparing a titanium nitride-containing refractory material composite according to claim 9, wherein the mole ratio of titanium tetrahalide to disilazane is from about 1:1 to about 1:2.
Claim 15
Dependent Claim
25 words
The process for preparing a titanium nitride-containing refractory material composite according to claim 9, wherein the refractory material powder comprises Si 3 N 4 .
Claim 16
Dependent Claim
158 words
A process for preparing a Si 3 N 4 --TiN composite, comprising the steps of: A) contacting titanium tetrachloride with hexamethyldisilazane, the mole ration of titanium tetrahalide to hexamethyldisilazane being from about 1:1 to about 1:2, optionally in the presence of a solvent, at a temperature from about -100° C. to about 100° C. and for a period of time sufficient to prepare a titanium-containing organometallic precursor; B) mixing the titanium-containing organometallic precursor with Si 3 N 4 . the weight ratio of titanium-containing organometallic precursor to Si 3 N 4 being from about 1:50 to about 1:1; C) heating the mixture of titanium-containing organometallic precursor and Si 3 N 4 in an inert atmosphere to a temperature of at least 600° C. for a period of time sufficient to pyrolyze the precursor; and D) further heating the pyrolyzed mixture at a temperature of at least about 1,600° C. to densify the pyrolyzed mixture to a solid composite.
Claim 17
Dependent Claim
158 words
A process for preparing a Si 3 N 4 --TiN composite, comprising the steps of: A) contacting titanium tetrachloride with hexamethyldisilazane, the mole ration of titanium tetrahalide to hexamethyldisilazane being from about 1:1 to about 1:2, optionally in the presence of a solvent, at a temperature from about -100° C. to about 100° C. and for a period of time sufficient to prepare a titanium-containing organometallic precursor; B) mixing the titanium-containing organometallic precursor with Si 3 N 4 . the weight ratio of titanium-containing organometallic precursor to Si 3 N 4 being from about 1:50 to about 1:1; C) heating the mixture of titanium-containing organometallic precursor and Si 3 N 4 in an inert atmosphere to a temperature of at least 600° C. for a period of time sufficient to pyrolyze the precursor; and D) further heating the pyrolyzed mixture at a temperature of at least about 1,600° C. to densify the pyrolyzed mixture to a solid composite.
References Cited (Backward Citations)
US3853567A
Cited
US4208215A
Cited
US4421528A
Cited
US4613455A
Cited
US4859639A
Cited
US4900700A
Cited
US5087593A
Cited
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