Cleaning processes for silicon carbide materials

• US 7,754,609 B1
• Filed: 10/28/2003
• Issued: 07/13/2010
• Est. Priority Date: 10/28/2003
• Status: Active Grant

• Current Assignee: Quantum Global Technologies LLC (Ultra Clean Holdings Incorporated)
• Original Assignee: Applied Materials Incorporated
• Inventors: Tan, Samantha S. H.
• Primary Examiner(s): Kunemund; Robert M
• Assistant Examiner(s): Song; Matthew J
• Application Number:
  US10/696,394
• Time in Patent Office: 2,450 Days
• Field of Search: 438/689, 438/690, 438/745, 438/906, 438/905, 117/84, 117/951, 134/1, 134/1.3, 134/2, 134/3
• US Class Current: 438/689
• CPC Class Codes: B08B 11/02 Devices for holding articles during cleaning B08B9/42 takes precedence
• CPC Class Codes: B08B 3/08 the liquid having chemical or dissolving effect substances used, see the relevant classes
• CPC Class Codes: B08B 3/12 by sonic or ultrasonic vibrations washing or rinsing machines for crockery or tableware using sonic or ultrasonic waves A47L15/13; of natural teeth, of prostheses using ultrasonic techniques similar to those used for natural teeth A61C17/20; application of ultrasonic vibrations to chemical, physical or physico-chemical processes in general B01J19/10
• CPC Class Codes: B08B 9/00 Cleaning hollow articles by methods or apparatus specially adapted thereto B08B6/00 takes precedence
• CPC Class Codes: C04B 35/565 based on silicon carbide
• CPC Class Codes: C04B 41/009 characterised by the material treated
• CPC Class Codes: C04B 41/5353 Wet etching, e.g. with etchants dissolved in organic solvents
• CPC Class Codes: C04B 41/91 involving the removal of part of the materials of the treated articles, e.g. etching
• CPC Class Codes: C11D 2111/46 applying energy, e.g. irradiation
• CPC Class Codes: Y10S 438/905 Cleaning of reaction chamber
• CPC Class Codes: Y10S 438/906 Cleaning of wafer as interim step

Abstract

The cleaning of silicon carbide materials on a large-scale is described. Certain silicon carbide materials in the form of wafer-lift pins, wafer-rings and/or wafer-showerheads are cleaned by using a combination of two of more of the following steps, comprising: high temperature oxidation, scrubbing, ultrasonic assisted etching in an aqueous acid solution, ultrasonication in deionized water, immersion in an aqueous acid solution, and high temperature baking. The silicon carbide materials may either be sintered or formed by chemical vapor deposition.

Claims

1. A method for cleaning silicon carbide materials on a large scale, the method comprising the acts of:

using an integrated system that is adapted for handling a multiplicity of said silicon carbide materials during said cleaning;

purging at least one opening within each of silicon carbide materials using a continuous flow of nitrogen gas stream;

ultrasonicating said silicon carbide materials in an aqueous solution of inorganic acid after the purging has begun;

ultrasonicating said silicon carbide materials in a bath of deionized water after the purging has begun; and

wherein purging using the continuous nitrogen gas stream continues during ultrasonicating of said silicon carbide materials in the aqueous solution and in the bath of deionized water;

wherein purging the at least one opening within each of the silicon carbide materials;

blocks the migration of the aqueous solution of inorganic acid to a base material; and

occurs before placing the silicon carbide material in the solution.

2. The method of claim 1, wherein said silicon carbide materials are sintered.

3. The method of claim 1, wherein said silicon carbide materials are formed using chemical vapor deposition (CVD).

4. The method of claim 1, further comprising the act of oxidizing said silicon carbide materials.

5. The method of claim 4, wherein

the act of oxidizing comprises using a temperature from about 800 degrees Celsius to about 1500 degrees Celsius.

6. The method of claim 1, further comprising the act of scrubbing said silicon carbide materials.

7. The method of claim 6, further comprising the act of contacting said silicon carbide materials in a dilute aqueous solution of inorganic acid after ultrasonicating said silicon carbide materials in said bath of deionized water.

8. The method of claim 7, wherein said dilute aqueous solution of inorganic acid is selected from said group consisting of HF:

HNO₃;

H₂O and HF;

H₂O₂;

HNO₃.

9. The method of claim 8, wherein said dilute aqueous solution of inorganic acid comprises

0.5%-1.5% wt. HF;

1%-10% wt. H₂O₂; and

0.1%-0.5% wt. HNO3.

10. The method of claim 7, wherein a temperature of said dilute aqueous solution of inorganic acid is maintained from about 20°

C. to about 50°

C.

11. The method of claim 1, wherein said aqueous solution of inorganic acid is selected from said group consisting of HF:

HNO₃;

H₂O and HF;

H₂O₂;

HNO₃.

12. The method of claim 1, wherein said aqueous solution of inorganic acid comprises:

5%-20% wt. HF;

20%-95% wt. HNO3; and

0%-80% wt. H₂O.

13. The method of claim 1, wherein a temperature of said aqueous solution of inorganic acid is maintained from about 20 degrees Celsius to about 50 degrees Celsius.

14. The method of claim 1, wherein the act of ultrasonicating said silicon carbide materials in said aqueous solution of inorganic acid is performed for a duration of time from about 10 minutes to about 15 minutes.

15. The method of claim 1, wherein the act of ultrasonicating said silicon carbide materials in said aqueous solution of inorganic acid is performed at a power from about 30 watts per gallon to about 50 watts per gallon.

16. The method of claim 1, wherein the act of ultrasonicating said silicon carbide materials in said aqueous solution of inorganic acid is performed at an ultrasonic frequency from about 25 Kilo-hertz to about 40 Kilo-hertz.

17. The method of claim 1, wherein

the temperature of said bath of deionized water is maintained from about 20 degrees Celsius to about 50 degrees Celsius.

18. The method of claim 1, wherein the act of ultrasonicating said silicon carbide materials in said bath of deionized water is performed for a duration of time from about 30 minutes to about 61 minutes.

19. The method of claim 1, wherein the act of ultrasonicating said silicon carbide materials in said bath of deionized water is performed at a power intensity from about 80% to about 90% of 40 watts/gallon.

20. The method of claim 1, wherein the act of ultrasonicating said silicon carbide materials in said bath of deionized water is performed at an ultrasonic frequency from about 27 Kilo-hertz to about 40 Kilo-hertz.

21. The method of claim 1, wherein the act of ultrasonicating said silicon carbide materials in said bath of deionized water is performed at a power from about 30 watts per gallon to about 50 watts per gallon.

22. The method of claim 1, further comprising the act of baking said silicon carbide materials.

23. The method of claim 22, wherein the act of baking comprises using a temperature of about 200 degrees Celsius to about 300 degrees Celsius.

24. The method of claim 22, wherein the act of baking is performed for a duration of time from about 2 hours to about 3 hours for silicon carbide wafer-rings and silicon carbide wafer-lift pins.

25. The method of claim 22, wherein the act of baking is performed using a nitrogen purge oven.

26. The method of claim 22, wherein the act of baking is performed using a convection oven.

27. The method of claim 22, wherein the act of baking is performed using a vacuum oven.

28. The method of claim 1, wherein the act of purging said silicon carbide materials using said nitrogen gas stream is performed at a pressure from about 10 psi to about 20 psi.

29. The method of claim 1, further comprising the act of soaking said silicon carbide materials in said aqueous solution of inorganic acid.

30. The method of claim 29, wherein said aqueous solution of inorganic acid is selected from said group consisting of HF:

HNO₃;

H₂O and HF;

H₂O₂;

HNO₃.

31. The method of claim 29, wherein said aqueous solution of inorganic acid comprises:

5%-20% M. HF;

20%-95% M. HNO3; and

0%-80% M. H₂O.

32. The method of claim 29, wherein a temperature of said aqueous solution of inorganic acid is maintained from about 20 degrees Celsius to about 50 degrees Celsius.

33. The method of claim 1, wherein said integrated system includes chemically resistant materials that are flexible.

34. The method of claim 33, wherein said chemically resistant materials includes high-density polyethylene.

35. The method of claim 1, wherein said integrated system includes robotic mechanisms.

36. The method of claim 1, wherein said integrated system is adapted for handling silicon carbide wafer-lift pins.

37. The method of claim 36, wherein said integrated system includes one or more a pin-racks adapted for holding said silicon carbide wafer-lift pins.

38. The method of claim 1, wherein said integrated system is adapted for handling silicon carbide wafer-showerheads.

39. The method of claim 1, wherein said integrated system is adapted for handling silicon carbide wafer-rings.

40. The method of claim 39, wherein said integrated system includes one or more wafer boats adapted for holding said silicon carbide wafer-rings.

41. The method of claim 1, further comprising using a peristaltic pump and a manifold for cleaning interior surfaces of hollow silicon carbide wafer-lift pins.