Claims
- 1. A process of preparing large size crystals of substances which are compounds or alloys of at least two constituents at least one of which is of relatively low volatility and one is of relatively high volatility comprising:
- 1. feeding continuously to the surface of a liquid phase solution which contains said components of low volatility, but does not contain said more volatile constituent, vapors of at least said component of high volatility from a source maintained at a constant temperature to vaporize and provide a vapor pressure on the surface of said liquid phase solution to continuously dissolve said vapors in said liquid so that all the constituents necessary to form said substance are then present in said solution; said process being carried out in a closed container containing said liquid phase in its one end and in its other end an interior container containing at least said component of high volatility;
- 2.
- 2. simultaneously subjecting said liquid phase solution to a first slight temperature gradient zone in which zone the temperature is sufficiently high to maintain said liquid phase and in which the temperature gradient is sufficiently slight to ensure gradual and homogeneous diffusion of said substance formed at said surface through said solution, the temperature of the upper surface end of said zone being higher than the lower end thereof, allowing said liquid phase to reach saturation with said substance in the lower end only of said first temperature gradient zone;
- 3. maintaining a second steep temperature gradient zone located beneath said first temperature gradient zone in which the temperature is lower than in said first temperature gradient zone;
- 4. crystallizing said substance at the level of the second gradient to form a solid-liquid interface;
- 5. ascertaining by the application of Fick's law when saturation of the liquid phase with said substance at said solid/liquid interface is reached;
- 6. when said saturation is reached, moving said liquid phase relative to said first and second temperature gradients while maintaining the solid-liquid interface at the same temperature and same composition within the second gradient by controlling the rate of relative movement at a speed ascertained by Fick's law and while maintaining the continuous feeding of vapor to the surface of said liquid phase; thereby
- 7. continuously forming and growing cyrstals of said substance at said
- interface. 2. A process according to claim 1 wherein said liquid phase surface is located at a constriction at the level of the lower end of a tube feeding a liquid constituent to said liquid phase.
- 3. A process according to claim 1 comprising feeding at least one other constituent as a liquid at a constriction in the median part of a container at the level of which constriction the liquid feed contacts said liquid phase.
Priority Claims (1)
Number |
Date |
Country |
Kind |
67.110074 |
Jun 1967 |
FR |
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Parent Case Info
This is a continuation of Ser. No. 232,240, filed Mar. 6, 1972, now abandoned, which is a continuation of Ser. No. 841,667, filed June 13, 1968, abandoned.
US Referenced Citations (11)
Foreign Referenced Citations (1)
Number |
Date |
Country |
265,338 |
Jun 1960 |
NL |
Non-Patent Literature Citations (4)
Entry |
Blum et al., IBM Tech. Disclosure Bulletin, vol. 9, No. 12, May 1967, pp. 1674-1676. |
Blum et al., J. Electrochem. Soc.: Solid State Science, Mar. 1968, pp. 314-325, vol. 115, No. 3. |
Lawson et al., Preparation of Single Crystals, 1958, Butterworths' Press, pp. 14-20. |
Fischer, J. of Electrochem. Soc., vol. 117, No. 2, Feb. 1970, pp. 41C-47C. |
Continuations (2)
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Number |
Date |
Country |
Parent |
232240 |
Mar 1972 |
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Parent |
841667 |
Jun 1968 |
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