US4956047A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Process of making high quality single quartz crystal using silica glass nutrient
Assignee: United States Department of the Air Force
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Filing: 1988-08-08
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Granted: 1990-09-11
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Expires: 2008-08-08
Abstract
Abstract Ultra high pure quartz is grown by a one step in-situ growth process where the nutrient is high purity silica. A negative temperature gradient is maintained between the nutrient zone and the seed zone until about the start of crystal growth. A sealable container made of silver contains the nutrient and the seed within the autoclave chamber.
Inventors
- 👤 Meckie T. Harris
- 👤 John J. Larkin
- 👤 Alton F. Armington
- 👤 John K. Kennedy
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-06 15:41
CPC Classifications
C; C30; C30B; C30B7/00; C30B29/00; C30B29/10; C30B29/16; C30B29/18; Y; Y10; Y10S; Y10S117/00; Y10S117/90; Y10T; Y10T117/00; Y10T117/10; Y10T117/1024; Y10T117/1096
Claims Analysis
Total Claims: 14
Claim 1
Independent Claim
258 words
A process of manufacturing ultra high purity quartz crystals, said process comprising the steps of: a. obtaining silica nutrient having very few impurities therein; b. providing at least one quartz seed; c. providing a sealable container having a positionable baffle therein and means for holding said at least one quartz seed, said container, said baffle and said holding means being made of a noble metal, said container being placable in a hydrothermal autoclave; d. placing the silica nutrient in a nutrient zone being a bottom section of the sealable container; e. putting a baffle over the nutrient zone and below a seed zone; f. attaching the at least one seed in the seed zone being in a top section of the container; g. filling the container with a fluid; h. sealing the container; i. placing the sealed container in a chamber of the hydrothermal autoclave; j. filling the void between the sealed container and the autoclave with a fluid; k. sealing the autoclave; l. heating said nutrient zone in a controlled manner; m. heating said seed zone in a controlled manner, said nutrient zone having a negative temperature gradient to prevent convection transport with respect to said seed zone during an initial heating before crystal growth; n. growing quartz about the seed wherein the nutrient zone is at a higher temperature than said seed zone, said nutrient zone having a positive temperature gradient to encourage convention transport with respect to said seed zone; o. cooling the autoclave; and p. removing at least one quartz crystal from the autoclave.
Claim 2
Dependent Claim
258 words
A process of manufacturing ultra high purity quartz crystals, said process comprising the steps of: a. obtaining silica nutrient having very few impurities therein; b. providing at least one quartz seed; c. providing a sealable container having a positionable baffle therein and means for holding said at least one quartz seed, said container, said baffle and said holding means being made of a noble metal, said container being placable in a hydrothermal autoclave; d. placing the silica nutrient in a nutrient zone being a bottom section of the sealable container; e. putting a baffle over the nutrient zone and below a seed zone; f. attaching the at least one seed in the seed zone being in a top section of the container; g. filling the container with a fluid; h. sealing the container; i. placing the sealed container in a chamber of the hydrothermal autoclave; j. filling the void between the sealed container and the autoclave with a fluid; k. sealing the autoclave; l. heating said nutrient zone in a controlled manner; m. heating said seed zone in a controlled manner, said nutrient zone having a negative temperature gradient to prevent convection transport with respect to said seed zone during an initial heating before crystal growth; n. growing quartz about the seed wherein the nutrient zone is at a higher temperature than said seed zone, said nutrient zone having a positive temperature gradient to encourage convention transport with respect to said seed zone; o. cooling the autoclave; and p. removing at least one quartz crystal from the autoclave.
Claim 3
Dependent Claim
21 words
A process as defined in claim 1, step a, wherein the silica nutritent is obtained through a chemical vapor deposition process.
Claim 4
Dependent Claim
27 words
A process as defined in claim 1, step b, wherein the quartz seed is cut from the X-plus growing region of a synthetic quartz, single crystal boule.
Claim 5
Dependent Claim
29 words
A process as defined in claim 1, step d, wherein the silica nutrient fills the nutrient zone only to about two thirds a vertical height in the bottom section.
Claim 6
Dependent Claim
19 words
A process as defined in claim 1, step b, wherein the seed has a thickness of about 5 millimeters.
Claim 7
Dependent Claim
26 words
A process as defined in clailm 1 further including the step of adding bulk quartz in the seed zone to reduce the dissolution of the seed.
Claim 8
Dependent Claim
26 words
A process as defined in clailm 1 further including the step of adding bulk quartz in the seed zone to reduce the dissolution of the seed.
Claim 9
Dependent Claim
24 words
A process as defined in claim 1, step g, wherein said fluid in the sealable container includes a controlled concentration of silica in solution.
Claim 10
Dependent Claim
15 words
A process as defined in claim 7 wherein the silica in solution is sodium metasilicate.
Claim 11
Dependent Claim
22 words
A process as defined in claim 1 wherein the growth temperature is about 345° C. and is reached in about one hour.
Claim 12
Dependent Claim
40 words
A process as defined in claim 1, step 1, wherein the heating of the nutrient zone provides a negative temperature gradient of about 75° to 150° C. with respect to the temperature in the seed zone during the initial heating.
Claim 13
Dependent Claim
24 words
A process as defined in claim 10 wherein the temperature of the nutrient zone is raised to a final temperature in about one hour.
Claim 14
Dependent Claim
22 words
A process as defined in claim 11 wherein the final temperature is about 350° C. and is reached in about two hours.
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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) | 1993-09-10 | 1994-03-12 | 1994-09-11 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1997-09-10 | 1998-03-12 | 1998-09-11 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2001-09-10 | 2002-03-12 | 2002-09-11 | $7700.00 | Window Closed / Lapsed |