Patent US3853487A successfully refreshed from Google Patents.
US3853487A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Method of forming crystals by the control of volatile constituent diffusion path distances through a melt
Assignee: US Philips Corp
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Filing: 1973-03-09
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Granted: 1974-12-10
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Expires: 1993-03-09
Abstract
Abstract Method of producing a rod shaped crystal of a compound from a liquid solution as the compound in a solution containing as a solvent a constituent of the compound and to which there is constantly supplied with a constituent of the compound more volatile than the solvent.
Inventors
- 👤 J Meuleman
- 👤 G Jacob
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-01 12:39
CPC Classifications
C; C30; C30B; C30B29/00; C30B29/10; C30B29/40; C30B11/00; C30B11/04; C30B11/06; Y; Y10; Y10T; Y10T117/00; Y10T117/10; Y10T117/1024; Y10T117/1092
Claims Analysis
Total Claims: 13
Claim 1
Independent Claim
156 words
A METHOD OF MANUFACTURING IN A SPACE CRYSTALLINE RODS OF A COMPOUND FROM A LIQUID SOLUTION OF THE SAID COMPOUNDS IN AT LEAST ONE OF THE CONSTITUENTS THEREOF, WHICH SOLUTION IS CONSTANTLY SUPPLIED WITH AT LEAST ONE CONSTITUENT WHICH IS MORE VOLATILE THAN THE SOLVENT, SAID MORE VOLATILE CONSTITUENT DIFFUSING, THROUGH THE SOLUTION WHICH SHOWS A CONCENTRATION GRADIENT OF THE MORE VOLATILE CONSTITUENT, TO A CRYSTALLIZATION INTERFACE PRESENT IN A STEEP TEMPERATURE GRADIENT, SAID TEMPERATURE GRADIENT BEING GRADUALLY TRAVERSED BY SAID SPACE, CHARACTERIZED IN THAT THE DISTANCE IN THE LIQUID BETWEEN SAID CRYSTALLIZATION INTERFACE ON THE ONE HAND AND ANOTHER FACE PRESENT BETWEEN THE SAID LIQUID WITH THE CONCENTRATION GRADIENT AND A PORTION OF THE LIQUID FACE WHERE SAID CONCENTRATION GRADIENT TERMINATES OF CONSTANT CONCENTRATION WHICH IS CONSTANTLY SUPPLIED WITH THE MORE VOLATILE CONSTITUENT ON THE OTHER HAND, IS MAINTAINED CONSTANT DURING THE WHOLE CRYSTAL GROWTH BY THE ADDITION OF THE CONSTITUENT SERVING AS A SOLVENT.
Claim 2
Independent Claim
156 words
A METHOD OF MANUFACTURING IN A SPACE CRYSTALLINE RODS OF A COMPOUND FROM A LIQUID SOLUTION OF THE SAID COMPOUNDS IN AT LEAST ONE OF THE CONSTITUENTS THEREOF, WHICH SOLUTION IS CONSTANTLY SUPPLIED WITH AT LEAST ONE CONSTITUENT WHICH IS MORE VOLATILE THAN THE SOLVENT, SAID MORE VOLATILE CONSTITUENT DIFFUSING, THROUGH THE SOLUTION WHICH SHOWS A CONCENTRATION GRADIENT OF THE MORE VOLATILE CONSTITUENT, TO A CRYSTALLIZATION INTERFACE PRESENT IN A STEEP TEMPERATURE GRADIENT, SAID TEMPERATURE GRADIENT BEING GRADUALLY TRAVERSED BY SAID SPACE, CHARACTERIZED IN THAT THE DISTANCE IN THE LIQUID BETWEEN SAID CRYSTALLIZATION INTERFACE ON THE ONE HAND AND ANOTHER FACE PRESENT BETWEEN THE SAID LIQUID WITH THE CONCENTRATION GRADIENT AND A PORTION OF THE LIQUID FACE WHERE SAID CONCENTRATION GRADIENT TERMINATES OF CONSTANT CONCENTRATION WHICH IS CONSTANTLY SUPPLIED WITH THE MORE VOLATILE CONSTITUENT ON THE OTHER HAND, IS MAINTAINED CONSTANT DURING THE WHOLE CRYSTAL GROWTH BY THE ADDITION OF THE CONSTITUENT SERVING AS A SOLVENT.
Claim 3
Dependent Claim
69 words
A method as claimed in claim 1, characterized in that the more volatile constituent is supplied to the surface of the solution in the vapour phase from a container which communicates with said surface, the position of said container and its volatile constituent contents being fixed relative to the said other face of the portion of the liquid which shows a constant concentration gradient relative to the crystallization interface.
Claim 4
Dependent Claim
67 words
A method as claimed in claim 2, characterized in that a constant supply of liquid solvent takes place by means of a tube which is dipped in the solution, an equilibrium on either side of the wall of said tube being maintained between the manometric pressure of the supplied liquid and the vapor pressure which prevails above the surface to which the more volatile constituent is supplied.
Claim 5
Dependent Claim
44 words
A method as claimed in claim 3, characterized in that the pressure of an inert gas above the surface of the added liquid is gradually increased during the crystallization so as to compensate for the decrease of the manometric height of the supplied liquid.
Claim 6
Dependent Claim
38 words
A method as claimed in claim 4, characterized in that the said increase in gaS pressure above the surface of the added liquid is obtained by lowering the crystallization space which produces a volume decrease of said gas.
Claim 7
Dependent Claim
61 words
A method of claim 2, characterized in that the more volatile constituent is constantly supplied to a supply of a liquid solvent which is separated from the solution in which the diffusion is adjusted by a wall which is permeable to the solution, said wall being fixed relative to the crystallization interface and said supply of liquid solvent is constantly homogenized.
Claim 8
Dependent Claim
23 words
A method as claimed in claim 6, characterized in that the said first volume is homogenized by stirring by means of a stirrer.
Claim 9
Dependent Claim
45 words
A method as claimed in claim 7, characterized in that the said first volume is homogenized by means of a rotating stirrer which gives the liquid along the said wall a speed which is higher than the rate of crystallization by several orders of magnitude.
Claim 10
Dependent Claim
46 words
A method as claimed in claim 6, characterized in that the supply of volatile constituent to the supply of liquid solvent is carried out outside the crystallization space, a circulation of the supplied liquid being ensured between the point of the supply and the said wall.
Claim 11
Dependent Claim
21 words
A method as claimed in claim 9 characterized in that the solvent is gallium and the solution is supplied with phosphorus.
Claim 12
Dependent Claim
116 words
A device for carrying out the method as claimed in claim 1 which comprises a vertical tight space the lower end of which is formed so as to receive a seed, heating means which are provided outside the said space and in which the latter is vertically movable, and means to slowly lower the said space through the said heating means, characterized in that a container which is arranged inside the said space has a permeable lower wall and means for stirring the liquid above said permeable wall, and means which pass through the wall of said space so as to maintain the said permeable wall in a fixed position relative to the said heating means.
Claim 13
Dependent Claim
14 words
A single crystal manufactured by means of the method as claimed in claim 1.
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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) | 1977-12-09 | 1978-06-10 | 1978-12-10 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1981-12-09 | 1982-06-10 | 1982-12-10 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1985-12-09 | 1986-06-10 | 1986-12-10 | $7700.00 | Window Closed / Lapsed |