US4689129A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Process for the preparation of submicron-sized titanium diboride
Assignee: Dow Chemical Co
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Filing: 1985-07-16
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Granted: 1987-08-25
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Expires: 2005-07-16
Abstract
Abstract Ultrafine titanium diboride powder is produced by subjecting a gaseous mixture of BCl 3 , H 2 , and TiCl 4 to an amount of laser radiation effective to convert at least a portion of the volatile boron and titanium sources to titanium diboride. The TiB 2 powders consist primarily of monodispersed equiaxial particles having a diameter of about 0.025 micron to about 0.3 micron.
Inventors
- 👤 Arne K. Knudsen
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-27 18:05
CPC Classifications
B; B01; B01J; B01J19/00; B01J19/08; B01J19/12; B01J19/121; C; C01; C01B; C01B35/00; C01B35/02; C01B35/04
Claims Analysis
Total Claims: 18
Claim 1
Independent Claim
118 words
A process for the preparation of substantially pure, ultrafine titanium diboride powder, which comprises subjecting a continuous stream of reactant gases consisting essentially of a volatile boron source and a volatile titanium source, the amount of said sources corresponding to a ration of from about 0.4:1 to about 15:1 and from about 100 to about 500 mole percent of the stoichiometric amount of hydrogen calculated on said boron source at an absolute pressure of at least about 0.7 atm., to at least an amount of laser radiation effective to convert at least a portion of the volatile boron and titanium sources to titanium diboride, said laser radiation having a wavelength suitable to be absorbed by said reactant gases.
Claim 2
Dependent Claim
118 words
A process for the preparation of substantially pure, ultrafine titanium diboride powder, which comprises subjecting a continuous stream of reactant gases consisting essentially of a volatile boron source and a volatile titanium source, the amount of said sources corresponding to a ration of from about 0.4:1 to about 15:1 and from about 100 to about 500 mole percent of the stoichiometric amount of hydrogen calculated on said boron source at an absolute pressure of at least about 0.7 atm., to at least an amount of laser radiation effective to convert at least a portion of the volatile boron and titanium sources to titanium diboride, said laser radiation having a wavelength suitable to be absorbed by said reactant gases.
Claim 3
Dependent Claim
22 words
The process according to claim 1, wherein said absolute pressure is in the range of about 0.7 atm. to about 2 atm.
Claim 4
Dependent Claim
31 words
The process according to claim 1, wherein said boron source comprises a member of the group comprising of an alkyl boron, an alkyl borate, a boron hydride and a boron halide.
Claim 5
Dependent Claim
36 words
The process according to claim 1, wherein the hydrogen is present in an amount of from about 100 to about 400 mole percent of the stoichiometric amount of a boron source in the starting gas mixture.
Claim 6
Dependent Claim
36 words
The process according to claim 4, wherein the hydrogen is present in an amount of from about 100 to about 200 mole percent of the stoichiometric amount of a boron source in the starting gas mixture.
Claim 7
Dependent Claim
18 words
The process according to claim 1, wherein the laser provides a power of at least about 100 watts.
Claim 8
Dependent Claim
14 words
The process according to claim 1, wherein said volatile titanium source is titanium tetrachloride.
Claim 9
Dependent Claim
50 words
The process of claim 1, which comprises bubbling said continuous stream of reactant gases through a heated solution of titanium tetrachloride and subjecting the resultant gases directly to an amount of laser radiation effective to convert at least a portion of the boron trichloride and titanium tetrachloride to titanium diboride.
Claim 10
Dependent Claim
100 words
A process for the preparation of substantially pure, ultrafine titanium diboride powder, which comprises bubbling a continous stream of hydrogen gas through a heated solution consisting essentially of titanium tetrachloride, mixing the resultant vapor with boron trichloride in an amount corresponding to a boron trichloride/titanium tetrachloride (BCl 3 /TiCl 4 ) ratio within the range of about 0.4:1 to about 15:1, subjecting the mixed vapors to a pressure of at least about 0.7 atm., and subjecting the result to an amount of CO 2 laser radiation effective to convert at least a portion of the boron trichloride to titanium diboride.
Claim 11
Dependent Claim
100 words
A process for the preparation of substantially pure, ultrafine titanium diboride powder, which comprises bubbling a continous stream of hydrogen gas through a heated solution consisting essentially of titanium tetrachloride, mixing the resultant vapor with boron trichloride in an amount corresponding to a boron trichloride/titanium tetrachloride (BCl 3 /TiCl 4 ) ratio within the range of about 0.4:1 to about 15:1, subjecting the mixed vapors to a pressure of at least about 0.7 atm., and subjecting the result to an amount of CO 2 laser radiation effective to convert at least a portion of the boron trichloride to titanium diboride.
Claim 12
Dependent Claim
25 words
The process of claim 9, wherein the mixed vapors are subjected to a pressure within the range of about 0.7 atm. to about 2 atm.
Claim 13
Dependent Claim
39 words
The process of claim 9, wherein the resultant vapor is mixed with the boron trichloride in an amount corresponding to a boron trichloride/titanium tetrachloride (BCl 3 /TiCl 4 ) ratio within the range of about 0.4:1 to about 5.0:1.
Claim 14
Dependent Claim
18 words
The process of claim 9, wherein said ultrafine titanium diboride powder is a high purity titanium diboride powder.
Claim 15
Dependent Claim
18 words
The process of claim 9, wherein said ultrafine titanium diboride powder is an ultrahigh purity titanium diboride powder.
Claim 16
Dependent Claim
24 words
The process of claim 9, wherein said ultrafine titanium diboride powder has a diameter within the range of about 0.025 to about 0.3 micron.
Claim 17
Dependent Claim
24 words
The process of claim 14, wherein said ultrafine titanium diboride powder has a diameter within the range of about 0.08 to about 0.17 micron.
Claim 18
Dependent Claim
19 words
The process of claim 9, wherein said ultrafine titanium diboride powder consists of particles which are monodispersed and equiaxed.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1990-08-24 | 1991-02-23 | 1991-08-25 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1994-08-24 | 1995-02-23 | 1995-08-25 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1998-08-24 | 1999-02-23 | 1999-08-25 | $7700.00 | Window Closed / Lapsed |