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US5350719A Expired / Lapsed US ⏱️ 0.0 years remaining

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
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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 01:07
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

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1997-09-26 1998-03-28 1998-09-27 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 2001-09-26 2002-03-28 2002-09-27 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 2005-09-26 2006-03-28 2006-09-27 $7700.00 Window Closed / Lapsed

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