Patent US4174380A successfully refreshed from Google Patents.
US4174380A
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Annealing synthetic diamond type Ib
Assignee: General Electric Co
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Filing: 1977-12-14
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Granted: 1979-11-13
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Expires: 1997-12-14
Abstract
Abstract Type Ib synthetic diamond crystal is annealed at an annealing temperature ranging from about 1500 DEG C. to about 2200 DEG C. under a pressure which prevents significant graphitization of the diamond during the annealing to convert at least about 20% of the total amount of type Ib nitrogen present in the crystal to type Ia nitrogen.
Inventors
- 👤 Herbert M. Strong
- 👤 Richard M. Chrenko
- 👤 Roy E. Tuft
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-02 20:42
CPC Classifications
C; C09; C09K; C09K3/00; C09K3/14; C09K3/1409; C09K3/1418; B; B01; B01J; B01J3/00; B01J3/06; B01J3/062; C30; C30B; C30B29/00; C30B29/02; C30B29/04; C30B33/00; B01J2203/00; B01J2203/06; B01J2203/0605; B01J2203/062; B01J2203/065; B01J2203/0655; B01J2203/0675; B01J2203/069; B01J2203/0695
Claims Analysis
Total Claims: 13
Claim 1
Independent Claim
206 words
An annealing process for converting type Ib nitrogen in synthetic diamond crystal to type Ia nitrogen, said crystal having a minimum size of one micron as measured along the longest edge dimension of the crystal which consists essentially of subjecting said synthetic diamond crystal to an annealing temperature ranging from about 1500° C. to about 2200° C. under at least a pressure which prevents significant graphitization of said crystal at said annealing temperature for a period of time ranging from about one minute to about 50 hours and sufficient to convert at least about 20% of the total amount of type Ib nitrogen present in said crystal to type Ia nitrogen, the minimum pressure ranging from 48 kilobars at said annealing temperature of 1500° C. to a minimum pressure of 70 kilobars at said annealing temperature of 2200° C., and recovering the resulting annealed free synthetic diamond crystal wherein the dissolved nitrogen detectable by ultraviolet, visible and infrared absorption spectra and electron paramagnetic resonance consists of types Ib and Ia nitrogen, said type Ib nitrogen always being present in said annealed crystal in at least a detectable amount, said annealing process making no significant change in the morphology and physical dimensions of said synthetic diamond crystal.
Claim 2
Dependent Claim
206 words
An annealing process for converting type Ib nitrogen in synthetic diamond crystal to type Ia nitrogen, said crystal having a minimum size of one micron as measured along the longest edge dimension of the crystal which consists essentially of subjecting said synthetic diamond crystal to an annealing temperature ranging from about 1500° C. to about 2200° C. under at least a pressure which prevents significant graphitization of said crystal at said annealing temperature for a period of time ranging from about one minute to about 50 hours and sufficient to convert at least about 20% of the total amount of type Ib nitrogen present in said crystal to type Ia nitrogen, the minimum pressure ranging from 48 kilobars at said annealing temperature of 1500° C. to a minimum pressure of 70 kilobars at said annealing temperature of 2200° C., and recovering the resulting annealed free synthetic diamond crystal wherein the dissolved nitrogen detectable by ultraviolet, visible and infrared absorption spectra and electron paramagnetic resonance consists of types Ib and Ia nitrogen, said type Ib nitrogen always being present in said annealed crystal in at least a detectable amount, said annealing process making no significant change in the morphology and physical dimensions of said synthetic diamond crystal.
Claim 3
Dependent Claim
41 words
An annealing process according to claim 1 wherein said annealing temperature ranges from about 1600° C. to about 2000° C., and said minimum pressure ranges from 51 kilobars at 1600° C. to a minimum pressure of 63 kilobars at 2000° C.
Claim 4
Dependent Claim
15 words
An annealing process according to claim 2 wherein said annealing temperature is about 1900° C.
Claim 5
Dependent Claim
30 words
An annealing process according to claim 1 wherein at least about 50% of the total amount of type Ib nitrogen present in the crystal is converted to type Ia nitrogen.
Claim 6
Dependent Claim
41 words
An annealing process according to claim 1 wherein the resulting annealed crystal is mixed type Ib-Ia which is further annealed in accordance with the process of claim 1 to convert an additional amount of type Ib nitrogen to type Ia nitrogen.
Claim 7
Dependent Claim
129 words
A free annealed synthetically grown diamond crystal wherein the morphology of said crystal is substantially as-synthetically grown, said as-synthetically grown morphology consisting essentially of sharp edges and flat faces, said crystal having nitrogen dissolved therein detectable by ultraviolet, visible and infrared absorption spectra and electron paramagnetic resonance which consists of types Ia and Ib with said type Ib nitrogen always being present in said crystal in at least a detectable amount, and wherein at least about 20% of the total amount of said detectable nitrogen present in the crystal is type Ia, said crystal having a minimum size as measured along the longest edge dimension of the crystal of one micron, said free annealed synthetically grown diamond crystal being produced by the process of claim 1 or claim 5.
Claim 8
Dependent Claim
30 words
An annealed synthetically grown diamond crystal according to claim 6 wherein at least about 50% of the total amount of said detectable nitrogen present in the crystal is type Ia.
Claim 9
Dependent Claim
29 words
An annealed synthetically grown diamond crystal according to claim 6 wherein more than 99% of the total amount of said detectable nitrogen present in the crystal is type Ia.
Claim 10
Dependent Claim
17 words
An annealed synthetically grown diamond crystal according to claim 6 wherein said crystal has an octahedral morphology.
Claim 11
Dependent Claim
17 words
An annealed synthetically grown diamond crystal according to claim 6 wherein said crystal has a cubo-octahedral morphology.
Claim 12
Dependent Claim
161 words
A free annealed synthetically grown diamond crystal wherein the nitrogen dissolved therein detectable by ultraviolet, visible and infrared absorption spectra and electron paramagnetic resonance consists of type Ia nitrogen and type Ib nitrogen with said type Ib nitrogen always being present in said crystal in at least a detectable amount, said type Ia nitrogen being present in an amount of at least 20% of the total amount of said detectable nitrogen present in the crystal, said crystal having a minimum size as measured along the longest edge dimension of the crystal of 0.25 millimeter, said crystal under a microscope showing scattered light reflected from scattering centers therein when a beam of light is shined at an angle thereon, said reflected scattered light and scattering centers not being shown by natural type Ia diamond, said reflected scattered light characterizing said crystal as synthetically grown, said free annealed synthetically grown diamond crystal being produced by the process of claim 1 or claim 5.
Claim 13
Dependent Claim
120 words
A free annealed synthetically grown diamond crystal having nitrogen dissolved therein detectable by ultraviolet, visible and infrared absorption spectra and electron paramagnetic resonance, said dissolved nitrogen consisting of types Ia and Ib with said type Ib nitrogen always being present in said crystal in at least a detectable amount, and wherein at least about 20% of the total amount of said detectable nitrogen present in the crystal is type Ia, said synthetically grown crystal containing an inclusion of a diamond growing metal catalyst, said crystal having a minimum size as measured along the longest edge dimension of the crystal of 1 micron, said free annealed synthetically grown diamond crystal being produced by the process of claim 1 or claim 5.
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) | 1982-11-12 | 1983-05-14 | 1983-11-13 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1986-11-12 | 1987-05-14 | 1987-11-13 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1990-11-12 | 1991-05-14 | 1991-11-13 | $7700.00 | Window Closed / Lapsed |