Deep-eutectic melt growth of nitride crystals

• US 8,088,220 B2
• Filed: 05/23/2008
• Issued: 01/03/2012
• Est. Priority Date: 05/24/2007
• Status: Active Grant

• Current Assignee: Crystal IS, Inc. (Asahi Kasei Corporation)
• Original Assignee: Crystal IS, Inc. (Asahi Kasei Corporation)
• Inventors: Slack, Glen A., Schujman, Sandra B.
• Primary Examiner(s): Kornakov, Michael
• Assistant Examiner(s): Bratland, Jr., Kenneth A
• Application Number:
  US12/126,334
• Publication Number:
  US 20090050050A1
• Time in Patent Office: 1,320 Days
• Field of Search: 117/11, 117/54, 117/64, 117/67, 117/73, 117/76, 117/77, 117/78, 117/81, 252/518.1
• US Class Current: 117/67
• CPC Class Codes: C30B 13/02 Zone-melting with a solvent, e.g. travelling solvent process
• CPC Class Codes: C30B 13/10 with addition of doping materials
• CPC Class Codes: C30B 29/403 AIII-nitrides

Abstract

In accordance with various embodiments, crystalline structures are formed by providing, at a growth temperature, a liquid comprising AlN and having a quality factor greater than approximately 0.14 and forming solid AlN from the liquid, the growth temperature being lower than the melting point of AlN.

Claims

1. A method of forming a crystalline structure, the method comprising:

providing, at a growth temperature, a liquid (i) consisting essentially of a mixture of AlN and a non-AlN nitride compound, and (ii) having a quality factor greater than approximately 0.14; and

forming solid AlN from the liquid, the solid AlN having an oxygen concentration less than 100 parts per million by weight,

wherein (i) the quality factor is defined as Q=Δ

T(K)/T_lm(K), Q being the quality factor, T_lm being the lower of the melting points of AlN and the non-AlN nitride compound in degrees Kelvin, and Δ

T being the difference between T_lm and the minimum liquidus temperature of the pseudo-binary system formed by AlN and the non-AlN nitride compound, and (ii) the growth temperature is lower than a melting point of AlN.

2. The method of claim 1, wherein the growth temperature is at least 500°

C. lower than the melting point of AlN.

3. The method of claim 1, wherein the non-AlN nitride compound comprises at least one of Y, B, Sc, Ti, V, Zr, La, Hf, or a rare-earth element.

4. The method of claim 1, wherein a concentration of AlN in the liquid is greater than 20 mole percent.

5. The method of claim 1, further comprising:

providing source material comprising polycrystalline AlN having a first oxygen concentration,

wherein providing the liquid comprises melting at least a portion of the source material, and the solid AlN comprises a second oxygen concentration lower than the first oxygen concentration.

6. The method of claim 1, further comprising providing an ambient pressure of nitrogen larger than both a decomposition pressure of AlN and a decomposition pressure of the non-AlN nitride compound.

7. The method of claim 1, wherein a solid solubility of AlN in the non-AlN nitride compound and a solid solubility of the non-AlN nitride compound in AlN are both less than 5%.

8. The method of claim 7, wherein the solid solubility of AlN in the non-AlN nitride compound and the solid solubility of the non-AlN nitride compound in AlN are both approximately zero.

9. The method of claim 1, wherein the growth temperature is less than 50°

C. greater than a eutectic temperature of AlN and the non-AlN nitride compound.

10. The method of claim 1, wherein a growth rate of the solid AlN is greater than 0.5 mm/hr.

11. The method of claim 10, further comprising selecting an ambient pressure of nitrogen, thereby controlling a concentration of nitrogen vacancies in the solid AlN.

12. The method of claim 11, wherein the ambient pressure of nitrogen is varied by at least one order of magnitude while forming solid AlN.

13. The method of claim 1, further comprising:

providing a rod comprising AlN and the non-AlN nitride compound at approximately their eutectic composition;

providing a seed comprising single-crystal AlN,

wherein (i) forming the liquid comprising AlN and the non-AlN nitride compound comprises melting a portion of the rod, and (ii) the liquid comprising AlN and the non-AlN nitride compound is disposed between an end of the rod and the seed; and

translating the liquid toward the rod,

whereby the solid AlN is formed on the seed as the liquid translates.

14. The method of claim 13, wherein translating the liquid consumes at least a portion of the rod.

15. The method of claim 13, further comprising providing a crucible in which the rod, the seed, and the liquid are disposed, the crucible comprising at least one of polycrystalline graphite, pyrolitic graphite, or glassy carbon.

16. The method of claim 15, further comprising providing a heating coil surrounding an outer surface of the crucible, wherein translating the heating coil translates the liquid.

17. The method of claim 15, wherein a diameter of the solid AlN formed on the seed is approximately equal to an inside diameter of the crucible.

18. The method of claim 13, wherein the liquid is translated at a rate of greater than 1 mm/hr.

19. The method of claim 13, wherein the rod comprises a dopant species, and at least a portion of the dopant species is incorporated into the solid AlN formed on the seed.

20. The method of claim 19, wherein the dopant species comprises at least one of MgO, BeO, a rare-earth element, B, Be, Li, Mg, Zn, Cd, Fe, Co, Mn, Sc, Ti, or V.

21. The method of claim 1, wherein the solid AlN is single-crystalline.

22. The method of claim 13, wherein the solid AlN is single-crystalline.

23. The method of claim 1, wherein the growth temperature is less than 50°

C. higher than the minimum liquidus temperature of the pseudo-binary system formed by AlN and the non-AlN nitride compound.