US5814149A
Expired / Lapsed
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Methods for manufacturing monocrystalline diamond films
Assignee: Kobe Steel Ltd
•
Filing: 1995-11-17
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Granted: 1998-09-29
•
Expires: 2015-11-17
Abstract
Abstract A method is related to grow monocrystalline diamond films by chemical vapor deposition on large area at low cost. The substrate materials are either bulk single crystals of Pt or its alloys, or thin films of those materials deposited on suitable supporting materials. The surfaces of those substrates must be either (111) or (001), or must have domain structures consisting of (111) or (001) crystal surfaces. Those surfaces can be inclined within ±10 degree angles from (111) or (001). In order to increase the nucleation density of diamond, the substrate surface can be scratched by buff and/or ultrasonic polishing, or carbon implanted. Monocrystalline diamond films can be grown even though the substrate surfaces have been roughened. Plasma cleaning of substrate surfaces and annealing of Pt or its alloy films are effective in growing high quality monocrystalline diamond films.
Inventors
- 👤 Yoshihiro Shintani
- 👤 Takeshi Tachibana
- 👤 Kozo Nishimura
- 👤 Koichi Miyata
- 👤 Yoshihiro Yokota
- 👤 Koji Kobashi
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-26 12:31
CPC Classifications
C; C23; C23C; C23C16/00; C23C16/22; C23C16/26; C23C16/27; C23C16/271; C23C16/02; C23C16/0254; C23C16/0263; C23C16/0272; C23C16/0281; C23C16/272; C23C16/274; C23C16/275; C30; C30B; C30B25/00; C30B25/02; C30B29/00; C30B29/02; C30B29/04
Claims Analysis
Total Claims: 32
Claim 1
Independent Claim
54 words
A method for forming monocrystalline diamond films by chemical vapor deposition (CVD) on substrates which are made of platinum or its alloys and have either (111) or (001) crystal surfaces and/or inclined crystal surfaces with angular deviations within ±10 degrees from (111) or (001), respectively, on the substrate surfaces entirely or at least partly.
Claim 2
Independent Claim
54 words
A method for forming monocrystalline diamond films by chemical vapor deposition (CVD) on substrates which are made of platinum or its alloys and have either (111) or (001) crystal surfaces and/or inclined crystal surfaces with angular deviations within ±10 degrees from (111) or (001), respectively, on the substrate surfaces entirely or at least partly.
Claim 3
Independent Claim
61 words
A method for forming monocrystalline diamond films by CVD on substrates each of which comprises of a film of platinum or its alloys deposited on the entire or at least part of the supporting material surface, where the film has either (111) or (001) crystal surfaces and/or inclined crystal surfaces with angular deviations within ±10 degrees from (111) or (001), respectively.
Claim 4
Independent Claim
61 words
A method for forming monocrystalline diamond films by CVD on substrates each of which comprises of a film of platinum or its alloys deposited on the entire or at least part of the supporting material surface, where the film has either (111) or (001) crystal surfaces and/or inclined crystal surfaces with angular deviations within ±10 degrees from (111) or (001), respectively.
Claim 5
Dependent Claim
35 words
A method for forming monocrystalline diamond films according to claim 2, wherein the thicknesses of the said films of Pt or Pt alloys are more than about 1000 Å and less than about 0.5 mm.
Claim 6
Dependent Claim
56 words
A method for forming monocrystalline diamond films according to claim 2, wherein the minority components of the said Pt alloys comprise of single or plural elements selected from the group of the VIA elements, the VIIIA elements, and the IB elements, and the total concentration of the minority components is not greater than 50 atomic %.
Claim 7
Dependent Claim
42 words
A method for forming monocrystalline diamond films according to claim 1, wherein the surface of said substrate consists of domains of said crystal surface, whereby monocrystalline diamond films with (111) or (001) crystal surfaces grow on the corresponding domains of the substrate.
Claim 8
Dependent Claim
55 words
A method for forming monocrystalline diamond films according to claim 2, wherein said supporting material is made of a single crystal of at least one member selected from the group consisting of lithium fluoride, calcium fluoride, magnesium oxide, nickel oxide, zirconium oxide, aluminum oxide, strontium titanate, barium titanate, lead titanate, potassium tantalate and lithium niobate.
Claim 9
Dependent Claim
24 words
A method for forming monocrystalline diamond films according to claim 2, wherein said supporting material is made of single crystal silicon, quartz or glass.
Claim 10
Dependent Claim
29 words
A method for forming monocrystalline diamond films according to claim 2, wherein said film is annealed at a temperature not lower than 300° C. during and/or after the deposition.
Claim 11
Dependent Claim
20 words
A method for forming monocrystalline diamond films according to claim 8, wherein said film is annealed in an oxidation atmosphere.
Claim 12
Dependent Claim
32 words
A method for forming monocrystalline diamond films according to claim 1, wherein the surfaces of said substrates have been buff and/or ultrasonically polished with diamond powder or paste prior to diamond CVD.
Claim 13
Dependent Claim
49 words
A method for forming monocrystalline diamond films according to claim 1, wherein the surfaces of said substrates have been ion-implanted with carbon using the conditions that the acceleration voltage is between 40 and 120 keV and the carbon implantation density is between 10 16 -10 20 cm -2 .
Claim 14
Dependent Claim
80 words
A method for forming monocrystalline diamond films according to claim 1, wherein prior to diamond CVD, said substrate is treated in a vacuum better than 10 -6 Torr above 300° C. for more than 15 minutes, and then cleaned in a plasma which comprises at least one gas selected from the group consisting of hydrogen, oxygen, chlorine and fluorine, or at least one inert gas selected from the group consisting of helium neon and argon, or a mixture of both.
Claim 15
Dependent Claim
69 words
A method for forming monocrystalline diamond films according to claim 12, wherein after cleaning said substrate the surface of said substrate is treated by a plasma which comprises a carbon-containing gas and, optionally, at least one gas selected from the group consisting of hydrogen, oxygen, chlorine and fluorine, and at least one inert gas selected from the group consisting of helium neon and argon, or a mixture of both.
Claim 16
Dependent Claim
26 words
A method for forming monocrystalline diamond films according to claim 1, wherein said substrate is applied with a bias voltage in a plasma of carbon-containing gas.
Claim 17
Dependent Claim
20 words
A method for forming monocrystalline diamond films according to claim 14, wherein the reaction gas is free of hydrogen atoms.
Claim 18
Dependent Claim
74 words
A method for forming monocrystalline diamond films according to claim 14, wherein the nuclei are formed from a carbon-containing gas diluted by hydrogen to a concentration of 0.1 to 10 vol % under the conditions that the gas pressure is 1 to 100 Torr, the substrate temperature is 400° to 1100° C., the DC voltage is -70 to -30 V or +70 to +350 V and the biasing time is 1 to 90 minutes.
Claim 19
Dependent Claim
26 words
A method for forming monocrystalline diamond films according to claim 1, wherein diamond CVD is undertaken using a source gas which is free of hydrogen atoms.
Claim 20
Dependent Claim
69 words
A method for forming monocrystalline diamond films according to claim 1, wherein diamond CVD is done using a mixture of methane, oxygen and hydrogen, where the methane concentration is between 0.1 and 5%, and the oxygen concentration is between 0.1 and 3%, at a substrate temperature higher than 750° C., whereby a monocrystalline diamond film with (111) crystal surface is deposited on the (111) crystal surface of said substrate.
Claim 21
Dependent Claim
69 words
A method for forming monocrystalline diamond films according to claim 1, wherein diamond CVD is done using a mixture of methane, oxygen and hydrogen, where the methane concentration is between 5 and 15%, and the oxygen concentration is between 1 and 7%, at a substrate temperature lower than 850° C., whereby a monocrystalline diamond film with (001) crystal surface is deposited on the (001) crystal surface of said substrate.
Claim 22
Dependent Claim
42 words
A method for forming monocrystalline diamond films according to claim 2, wherein the surface of said substrate consists of domains of said crystal surface, whereby monocrystalline diamond films with (111) or (001) crystal surfaces grow on the corresponding domains of the substrate.
Claim 23
Dependent Claim
32 words
A method for forming monocrystalline diamond films according to claim 2, wherein the surface of said substrates have been buff and/or ultrasonically polished with diamond powder or paste prior to diamond CVD.
Claim 24
Dependent Claim
49 words
A method for forming monocrystalline diamond films according to claim 2, wherein the surfaces of said substrates have been ion-implanted with carbon using the conditions that the acceleration voltage is between 40 and 120 keV and the carbon implantation density is between 10 16 -10 20 cm -2 .
Claim 25
Dependent Claim
80 words
A method for forming monocrystalline diamond films according to claim 2, wherein prior to diamond CVD, said substrate is treated in a vacuum better than 10 -6 Torr above 300° C. for more than 15 minutes, and then cleaned in a plasma which comprises at least one gas selected from the group consisting of hydrogen, oxygen, chlorine and fluorine, or at least one inert gas selected from the group consisting of helium, neon and argon, or a mixture of both.
Claim 26
Dependent Claim
69 words
A method for forming monocrystalline diamond films according to claim 23, wherein after cleaning said substrate the surface of said substrate is treated by a plasma which comprises a carbon-containing gas and, optionally, at least one gas selected from the group consisting of hydrogen, oxygen, chlorine and fluorine, and at least one inert gas selected from the group consisting of helium, neon and argon, or a mixture of both.
Claim 27
Dependent Claim
26 words
A method for forming monocrystalline diamond films according to claim 2, wherein said substrate is applied with a bias voltage in a plasma of carbon-containing gas.
Claim 28
Dependent Claim
20 words
A method for forming monocrystalline diamond films according to claim 25, wherein the reaction gas is free of hydrogen atoms.
Claim 29
Dependent Claim
74 words
A method for forming monocrystalline diamond films according to claim 25, wherein the nuclei are formed from a carbon-containing gas diluted by hydrogen to a concentration of 0.1 to 10 vol % under the conditions that the gas pressure is 1 to 100 Torr, the substrate temperature is 400° to 1100° C., the DC voltage is -70 to -30 V or +70 to +350 V and the biasing time is 1 to 90 minutes.
Claim 30
Dependent Claim
26 words
A method for forming monocrystalline diamond films according to claim 2, wherein diamond CVD is undertaken using a source gas which is free of hydrogen atoms.
Claim 31
Dependent Claim
69 words
A method for forming monocrystalline diamond films according to claim 2, wherein diamond CVD is done using a mixture of methane, oxygen and hydrogen, where the methane concentration is between 0.1 and 5%, and the oxygen concentration is between 0.1 and 3%, at a substrate temperature higher than 750° C., whereby a monocrystalline diamond film with (111) crystal surface is deposited on the (111) crystal surface of said substrate.
Claim 32
Dependent Claim
69 words
A method for forming monocrystalline diamond films according to claim 2, wherein diamond CVD is done using a mixture of methane, oxygen and hydrogen, where the methane concentration is between 5 and 15%, and the oxygen concentration is between 1 and 7%, at a substrate temperature lower than 850° C., whereby a monocrystalline diamond film with (001) crystal surface is deposited on the (001) crystal surface of said substrate.
References Cited (Backward Citations)
JPS61286299A
Cited
EP0386726A1
Cited
JPH03274001A
Cited
EP0492159A1
Cited
EP0534729A2
Cited
US5298286A
Cited
EP0598361A1
Cited
EP0636706A2
Cited
US5404835A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 2001-09-28 | 2002-03-30 | 2002-09-29 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 2005-09-28 | 2006-03-30 | 2006-09-29 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2009-09-28 | 2010-03-30 | 2010-09-29 | $7700.00 | Window Closed / Lapsed |