Processes for the continuous preparation of single crystals

• US 4,565,600 A
• Filed: 05/11/1983
• Issued: 01/21/1986
• Est. Priority Date: 04/27/1981
• Status: Expired due to Fees

• Current Assignee: Criceram
• Original Assignee: Criceram
• Inventors: Ricard, Jean
• Primary Examiner(s): Bernstein, Hiram H.
• Application Number:
  US06/492,368
• Time in Patent Office: 986 Days
• Field of Search: 156/608, 156/617 SP, 156/617 V, 156/DIG. 96, 156/DIG. 88, 169/60
• US Class Current: 117/25
• CPC Class Codes: C30B 15/08 Downward pulling
• CPC Class Codes: C30B 29/20 Aluminium oxides
• CPC Class Codes: Y10S 117/91 Downward pulling

Abstract

Processes for the continuous preparation of single crystals having a predetermined shape and requiring little or no subsequent machining which processes comprise placing a single crystal-forming material in a crucible fitted in its lower portion with a capillary conduit having a length equal to or greater than the retention length of the molten material in the capillary at the selected temperature and pressure, heating the crystal-forming material to a temperature above its melting point, bringing a performed appropriately oriented crystal seed into contact with the pendant drop formed at the lower point of the capillary, and pulling the seed crystal away from the feed material in the crucible so that the amount of crystal-forming material fed per unit of time is at every instant substantially equal to the quantity of material pulled into single crystal form, together with novel apparatus comprising a capillary-containing crucible, heating means, feed means, enclosure, seed-supporting carrier, means for moving and rotating the carrier, and means for controlling the movement of the carrier.

Claims

1. A continuous process for the preparation of single crystals having a predetermined shape, which process comprises:

(a) charging the crystal-forming material to a crucible tapped in its lower region by a capillary conduit with a height greater than or equal to the retention height of the melted crystal-forming material in the capillary at the temperature and pressure used,

(b) bringing th crystal-forming material to a temperature above its melting point so as to form a drop at the lower end of the capillary,

(c) contacting a preformed seed crystal having a selected crystal orientation with the drop, and

(d) pulling the seed crystal in contact with the drop downwardly away from the crucible to form a single crystal, at a growth front between the crystal and the melted crystal-forming material, the quantity of crystal-forming material fed per unit of time being substantially equal to the amount of material pulled into the single crystal and the force at the growth front being substantially nil.

2. A process according to claim 1 wherein the crystal formed is periodically removed at selected time intervals.

3. A process according to claim 1 wherein the crystal-forming material is sodium chloride, potassium chloride, pure or doped silicon, undoped alumina, doped alumina, yttrium garnet, or alumina or alumina-magnesia spinels.

4. A process according to claim 1 wherein the crystal-forming material is in the form of beads.

5. A process according to claim 1 wherein the crystal-forming material is in the form of grains.

6. A process according to claim 1 wherein the crystal-forming material is a powder.

7. A process according to claim 1 carried out under an inert atmosphere.

8. A process according to claim 1 carried out under vacuum.

9. A process according to claim 1 where the quantity fed is controlled to obtain a single crystal with substantially plane surfaces.

10. A process according to claim 1 wherein at least two different crystal-forming materials are charged to the crucible.

11. A process according to claim 1 wherein at least two different crystal-forming materials are charged to the crucible serially.

12. A process according to claim 1 wherein at least two different crystal-forming materials are charged to the crucible in amounts which are varied over a period of time.

13. A process according to claim 1 wherein the material is brought to a temperature above its melting point by radio frequency induction heating.

14. A process according to claim 1 wherein the speed of downward movement is from about 10 to about 500 mm/hr.

15. A process according to claim 1 wherein at least one of the lower edges of the capillary is in a different horizontal plane than the other edges.

16. A process according to claim 15 wherein H is from about one to about three millimeters.

17. A process according to claim 1 wherein the crucible contains a few cubic centimeters of crystal-forming material.