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US4565747A
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Boron nitride containing titanium nitride, method of producing the same and composite ceramics produced therefrom
Assignee: Japan Science and Technology Agency
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Filing: 1984-11-09
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Granted: 1986-01-21
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Expires: 2004-11-09
Abstract
Abstract Boron nitride containing titanium nitride in an amount of 0.05 to 10 wt. % which is produced at a relatively low temperature, utilizing a chemical vapor deposition technique. In the deposition process, boron, titanium and nitrogen source gases are introduced into an evacuated reactor together with a carrier and/or diluent gas and contacted with a heated substrate previously mounted in the reactor, whereby boron nitride with titanium nitride is deposited onto the substrate. The deposit thus obtained has a high density, a significantly improved heat-shielding ability, a high degree of anisotropy with respect to thermal diffusivity and a high chemical stability. By using such anisotropic boron nitride with BN ceramics, very useful BN type composite ceramics can be produced.
Inventors
- 👤 Hiroyuki Nakae
- 👤 Toshitsugu Matsuda
- 👤 Naoki Uno
- 👤 Yukio Matsunami
- 👤 Toshio Hirai
- 👤 Tsuyoshi Masumoto
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-24 22:47
CPC Classifications
C; C03; C03C; C03C17/00; C03C17/22; C03C17/225; C04; C04B; C04B35/00; C04B35/515; C04B35/58; C04B35/583; C23; C23C; C23C16/00; C23C16/22; C23C16/30; C23C16/34; C03C2217/00; C03C2217/20; C03C2217/28; C03C2217/281; C03C2218/00; C03C2218/10; C03C2218/15; C03C2218/152
Claims Analysis
Total Claims: 25
Claim 1
Independent Claim
22 words
Boron nitride produced by chemical vapor deposition, said boron nitride containing titanium nitride in an amount of 0.05 to 10 wt. %.
Claim 2
Dependent Claim
22 words
Boron nitride produced by chemical vapor deposition, said boron nitride containing titanium nitride in an amount of 0.05 to 10 wt. %.
Claim 3
Dependent Claim
24 words
Boron nitride as claimed in claim 1 in which said boron nitride contains titanium nitride in an amount of 0.05 to 2.0 wt. %.
Claim 4
Dependent Claim
19 words
Boron nitride as claimed in claim 1 in which said titanium nitride is contained in a fine particle form.
Claim 5
Dependent Claim
19 words
Boron nitride as claimed in claim 3 in which said titanium nitride is contained in the state of crystal.
Claim 6
Dependent Claim
28 words
Boron nitride as claimed in claim 4 in which said titanium nitride is contained in the state of crystal with a diameter of not greater than 100 Å.
Claim 7
Dependent Claim
19 words
Boron nitride as claimed in claim 5 in which titanium nitride is contained in a single crystal particle form.
Claim 8
Dependent Claim
17 words
Boron nitride as claimed in claim 1 in which said boron nitride is in a turbostratic structure.
Claim 9
Dependent Claim
25 words
Boron nitride as claimed in claim 7 in which the interlayer spacing of said turbostratic structure is in the range of 3.35 to 3.45 Å.
Claim 10
Dependent Claim
23 words
Boron nitride as claimed in claim 1 in which said boron nitride has a density of from 1.4 to 2.3 g/cm 3 .
Claim 11
Dependent Claim
23 words
Boron nitride as claimed in claim 9 in which said boron nitride has a density of from 2.0 to 2.2 g/cm 3 .
Claim 12
Independent Claim
208 words
A method of producing boron nitride containing titanium nitride in an amount of 0.05 to 10 wt. % by a chemical vapor deposition, comprising the steps of: (a) mounting a substrate shaped into a desired form in a reactor; (b) evacuating said reactor and heating said substrate to the temperature range of 500° to 2000° C.; (c) introducing a boron depositing source gas, a nitrogen depositing source gas, a titanium depositing source gas and carrier and/or diluent gas into said evacuated reactor, and then contacting said source gases with said substrate within the substrate temperature ranging from 500° to 2000° C. and at the total internal pressure of said reactor ranging from 0.1 to 770 torr, thereby depositing said boron nitride containing titanium nitride, the ratio of said titanium depositing source gas to said boron depositing source gas being controlled to give a Ti/B atomic ratio of 0.005 to 0.45; (d) continuing to feed said source gases and said carrier and/or diluent gas while degassing to maintain said total internal pressure of said reactor within said pressure range until the desired amount of said boron nitride is deposited onto said substrate; (e) cooling and taking out said substrate; and (f) removing said deposited boron nitride from said substrate.
Claim 13
Independent Claim
208 words
A method of producing boron nitride containing titanium nitride in an amount of 0.05 to 10 wt. % by a chemical vapor deposition, comprising the steps of: (a) mounting a substrate shaped into a desired form in a reactor; (b) evacuating said reactor and heating said substrate to the temperature range of 500° to 2000° C.; (c) introducing a boron depositing source gas, a nitrogen depositing source gas, a titanium depositing source gas and carrier and/or diluent gas into said evacuated reactor, and then contacting said source gases with said substrate within the substrate temperature ranging from 500° to 2000° C. and at the total internal pressure of said reactor ranging from 0.1 to 770 torr, thereby depositing said boron nitride containing titanium nitride, the ratio of said titanium depositing source gas to said boron depositing source gas being controlled to give a Ti/B atomic ratio of 0.005 to 0.45; (d) continuing to feed said source gases and said carrier and/or diluent gas while degassing to maintain said total internal pressure of said reactor within said pressure range until the desired amount of said boron nitride is deposited onto said substrate; (e) cooling and taking out said substrate; and (f) removing said deposited boron nitride from said substrate.
Claim 14
Dependent Claim
23 words
A method as claimed in claim 11 in which said temperature of said substrate is in the range of 1000° to 1500° C.
Claim 15
Dependent Claim
23 words
A method as claimed in claim 12 in which said temperature of said substrate is in the range of 1200° to 1400° C.
Claim 16
Dependent Claim
27 words
A method as claimed in claim 11 in which said total internal pressure of said reactor is maintained at 1 to 15 torr during the deposition process.
Claim 17
Dependent Claim
36 words
A method as claimed in claim 11 in which the ratio of said titanium depositing source gas to said boron depositing source gas is controlled to give a Ti/B atomic ratio ranging from 0.01 to 0.2.
Claim 18
Dependent Claim
69 words
A method as claimed in claim 11 in which said boron depositing source gas is one or more selected from the group consisting of BCl 3 , BF 3 , B 2 H 6 , B 10 H 14 , B 3 N 3 H 6 (borazine), B 3 N 3 H 3 Cl 3 (borazol trichloride), B(C 2 H 5 ) 3 and B(CH 3 ) 3 .
Claim 19
Dependent Claim
56 words
A method as claimed in claim 11 in which said nitrogen depositing source gas is one or more selected from the group consisting of HN 3 , NH 3 , N 2 H 4 , NH 4 Cl, NH 4 Br, NH 4 F, NH 4 HF 2 , NH 4 I and N 2 .
Claim 20
Dependent Claim
36 words
A method as claimed in claim 11 in which said titanium depositing source gas is one or more selected from the group consisting of TiCl 4 , TiBr 4 , TiF 4 and TiI 4 .
Claim 21
Dependent Claim
30 words
A method as claimed in claim 11 in which one or more gases of nitrogen(N 2 ), argon(Ar), helium(He) and hydrogen(H 2 ) are employed as carrier and/or diluent gas.
Claim 22
Dependent Claim
25 words
A method as claimed in claim 11 in which said substrate is made of graphite, SiC, BN, TiB 2 , metallic molybdenum, or quartz glass.
Claim 23
Dependent Claim
21 words
A method as claimed in claim 11 in which said source gases are introduced separately through two or more inlet passages.
Claim 24
Dependent Claim
44 words
Boron nitride type composite ceramics composed of (1) one or more boron nitride ceramic base layers containing titanium nitride in an amount of 0.05 to 10 wt. % which is produced by chemical vapor deposition and (b) one or more BN ceramic surface layers.
Claim 25
Dependent Claim
44 words
Boron nitride type composite ceramics composed of (1) one or more boron nitride ceramic base layers containing titanium nitride in an amount of 0.05 to 10 wt. % which is produced by chemical vapor deposition and (b) one or more BN ceramic surface layers.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1989-01-20 | 1989-07-22 | 1990-01-21 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1993-01-20 | 1993-07-22 | 1994-01-21 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1997-01-20 | 1997-07-22 | 1998-01-21 | $7700.00 | Window Closed / Lapsed |