# US 5,350,719 A · Preparation of titanium nitride-containing refractory material composites > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 5,350,719 A - Document ID: US5350719A - Status: Granted - Kind: A - Application number: 07/972,333 - Filed: 1992-11-06 - Granted: 1994-09-27 - Earliest claimed: 1992-11-06 - Assignees: Ford Motor Company - Inventors: Chaitanya K. Narula; Gary M. Crosbie - Web page: https://patentgrep.com/patent/US5350719A ## CPC - C04B 35/58014: {based on titanium nitrides, e.g. TiAlON} - C04B 35/584: based on silicon nitride - 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 ## 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. ## Claims ### Claim 1 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.degree. 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.degree. C. to densify the pyrolyzed mixture to a solid composite. ### Claim 2 (depends on 1) The process for preparing a titanium nitride-containing refractory material composite according to claim 1, wherein the titanium tetrahalide comprises titanium tetrachloride. ### Claim 3 (depends on 1) The process for preparing a titanium nitride-containing refractory material composite according to claim 1, wherein the disilazane comprises hexamethyldisilazane. ### Claim 4 (depends on 1) 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 5 (depends on 4) 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 6 (depends on 1) 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 7 (depends on 1) 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.degree. C. to about 100.degree. C. ### Claim 8 (depends on 1) The process for preparing a titanium nitride-containing refractory material composite according to claim 1, wherein the refractory material powder comprises Si.sub.3 N.sub.4. ### Claim 9 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.degree. C. to about 100.degree. 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.degree. 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.degree. C. to densify the pyrolyzed mixture to a solid composite. ### Claim 10 (depends on 9) The process for preparing a titanium nitride-containing refractory material composite according to claim 9, wherein the titanium tetrahalide comprises titanium tetrachloride. ### Claim 11 (depends on 9) The process for preparing a titanium nitride-containing refractory material composite according to claim 9, wherein the disilazane comprises hexamethyldisilazane. ### Claim 12 (depends on 9) 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 13 (depends on 9) The process for preparing a titanium nitride-containing refractory material composite according to claim 9, wherein the refractory material powder comprises Si.sub.3 N.sub.4. ### Claim 14 A process for preparing a Si.sub.3 N.sub.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.degree. C. to about 100.degree. C. and for a period of time sufficient to prepare a titanium-containing organometallic precursor; B) mixing the titanium-containing organometallic precursor with Si.sub.3 N.sub.4. the weight ratio of titanium-containing organometallic precursor to Si.sub.3 N.sub.4 being from about 1:50 to about 1:1; C) heating the mixture of titanium-containing organometallic precursor and Si.sub.3 N.sub.4 in an inert atmosphere to a temperature of at least 600.degree. 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.degree. C. to densify the pyrolyzed mixture to a solid composite.