Method of preparing silicon carbide surfaces for crystal growth

• US 4,946,547 A
• Filed: 10/13/1989
• Issued: 08/07/1990
• Est. Priority Date: 10/13/1989
• Status: Expired due to Term

• Current Assignee: CREE Incorporated (Wolfspeed, Inc.)
• Original Assignee: Cree Research, Inc.
• Inventors: Kong, Hua-Shuang, Edmond, John A., Palmour, John W.
• Primary Examiner(s): Powell, William A.
• Application Number:
  US07/421,375
• Time in Patent Office: 298 Days
• Field of Search: 156/610, 156/612, 156/613, 156/614, 156/636, 156/643, 156/645, 156/646, 156/662, 156/DIG. 111, 427/38, 427/39, 427/309, 204/192.23, 204/192.3, 204/192.32, 204/192.37, 437/100, 437/234, 252/79.1
• US Class Current: 117/97
• CPC Class Codes: H01L 21/02378 Silicon carbide
• CPC Class Codes: H01L 21/02433 Crystal orientation
• CPC Class Codes: H01L 21/02529 Silicon carbide
• CPC Class Codes: H01L 21/02609 Crystal orientation
• CPC Class Codes: H01L 21/02631 Physical deposition at reduced pressure, e.g. MBE, sputtering, evaporation
• CPC Class Codes: H01L 21/02658 Pretreatments cleaning in general H01L21/02041
• CPC Class Codes: H01L 21/465 Chemical or electrical treatment, e.g. electrolytic etching to form insulating layers H01L21/469

Abstract

The invention is a method of forming a substantially planar surface on a monocrystalline silicon carbide crystal by exposing the substantially planar surface to an etching plasma until any surface or subsurface damage caused by any mechanical preparation of the surface is substantially removed. The etch is limited, however, to a time period less than that over which the plasma etch will develop new defects in the surface or aggravate existing ones, and while using a plasma gas and electrode system that do not themselves aggravate or cause substantial defects in the surface.

Claims

1. A method of epitaxially growing a monocrystalline silicon carbide thin film on a silicon carbide surface that reduces defect density in the resulting thin film and in the interface between the thin film and the silicon carbide surface, the method comprising:

forming a substantially planar surface on a monocrystalline silicon carbide crystal;

exposing the substantially planar surface to an etching plasma until any surface or subsurface damage caused by the mechanical preparation is substantially removed, but for a time period less than that over which the plasma etch will develop new defects in the surface or aggravate existing ones, and while using a plasma gas and electrode system that do not themselves cause substantial defects in the surface; and

depositing a thin film of monocrystalline silicon carbide upon the etched surface by chemical vapor deposition.

2. A method according to claim 1 wherein the step of forming a substantially planar surface on a silicon carbide crystal comprises mechanically preparing the silicon carbide crystal to form a substantially planar surface.

3. A method according to claim 2 wherein the step of mechanically preparing a silicon carbide crystal comprises:

slicing a silicon carbide crystal to expose a generally planar surface;

lapping the generally planar surface with an abrasive paste; and

polishing the generally planar surface with an abrasive paste to produce a substantially planar surface.

4. A method according to claim 1 wherein the step of exposing the substantially planar surface to an etching plasma for a time period less than that over which the plasma etch will develop new defects in the surface or aggravate existing ones comprises limiting the depth of etch to between about 0.02 and 10 microns.

5. A method according to claim 1 wherein the step of exposing the substantially planar surface to an etching plasma for a time period less than that over which the plasma etch will develop new defects in the surface or aggravate existing ones comprises limiting the depth of etch to between about 0.5 and 1 micron.

6. A method according to claim 1 wherein the step of depositing a thin film of monocrystalline silicon carbide upon the etched surface by chemical vapor deposition comprises depositing a thin film layer of 6H silicon carbide on a flat interface 6H silicon carbide surface that is inclined more than one degree off axis with respect to a basal plane thereof substantially towards one of the <

1120>

directions.

7. A method according to claim 1 wherein the step of depositing a thin film of monocrystalline silicon carbide upon the etched surface by chemical vapor deposition comprises epitaxially depositing a beta silicon carbide thin film in the [111] growth direction on the (0001) Si face of a 6H silicon carbide surface such that the (111) crystallography of the beta silicon carbide thin film matches the (0001) crystallography of the 6H silicon carbide surface and such that the beta silicon carbide (101) face is parallel to the 6H silicon carbide (1120) face and the beta silicon carbide (111) face is parallel to the 6H silicon carbide (0001) face.

8. A method according to claim 1 wherein the step of exposing the substantially planar surface to an etching plasma while using a plasma gas and electrode system that do not themselves cause substantial defects in the surface comprises:

applying a plasma generating potential across two electrodes;

generating a plasma between the two electrodes by introducing a gas between the electrodes, and wherein the gas is easily dissociated substantially into its elemental species in the plasma and wherein substantially all of the dissociated species from the gas are volatile in the plasma and wherein at least one of the dissociated species is reactive with silicon carbide;

positioning the substantially planar silicon carbide surface as a target on one of the electrodes, and wherein the electrode is formed from a material with a low sputter yield and wherein the electrode material is reactive with the dissociated species; and

reacting the plasma with the silicon carbide to thereby etch the silicon carbide while the reaction of the dissociated species with the electrode and the electrode'"'"'s low sputter yield prevents contamination of the target with either sputtered materials from the supporting electrode or nonvolatile dissociated species from the plasma.

9. A method according to claim 8 wherein the step of generating a plasma between the two electrodes by introducing a gas between the electrodes comprises introducing a mixture of a fluorine containing gas and an oxygen containing gas that is easily dissociated substantially into its elemental species in the plasma and wherein substantially all of the dissociated species from the gas mixture are volatile in the plasma and wherein at least one of the dissociated species is reactive with silicon carbide and with the proviso that none of the resulting species otherwise interferes with the etching process or the silicon carbide surface being prepared.

10. A method according to claim 8 wherein the step of generating a plasma comprises forming a reactive ion plasma from nitrogen trifluoride.

11. A method according to claim 10 wherein the step of generating a reactive ion plasma comprises applying a direct current bias to the plasma.

12. A method according to claim 8 further comprising the step of applying a magnetic field to the target to enhance the etch rate of the silicon carbide target in the plasma.

13. A method according to claim 12 wherein the step of applying a magnetic field comprises placing a magnet adjacent the silicon carbide target.

14. A method according to claim 8 wherein the step of positioning the silicon carbide target on one of the electrodes comprises positioning the silicon carbide target on a carbon cathode.

15. A method according to claim 8 wherein the step of positioning the silicon carbide target on one of the electrodes comprises positioning the silicon carbide target on a quartz cathode.

16. A method according to claim 8 wherein the step of applying a plasma generating potential comprises applying between about 10 and about 400 watts of power to the electrodes.

17. A method according to claim 8 wherein the step of applying a plasma generating potential comprises applying a power density of between about 0.04 and about 2 watts per square centimeter to the powered electrode.

18. A method according to claim 8 wherein the step of applying a plasma generating potential comprises applying a power density of between about 0.4 and 0.9 watts per square centimeter to the powered electrode.

19. A method according to claim 8 wherein the step of introducing a gas between the electrodes comprises introducing the gas at a pressure of between about 5 and 5000 milliTorr.

20. A method according to claim 8 wherein the step of introducing a gas comprises introducing a gas at a flow rate of between about 1 and about 500 standard cubic centimeters per minute.

21. A method according to claim 8 wherein the step of introducing a gas comprises introducing a gas at a flow rate of about 50 standard cubic centimeters per minute.

22. A method according to claim 8 wherein the step of introducing a gas comprises introducing a mixture of about ten percent nitrous oxide in nitrogen trifluoride at a pressure of about 100 milliTorr.

23. A method according to claim 8 wherein the step of generating a plasma comprises generating a reactive ion beam plasma.

24. A method according to claim 8 wherein the step of generating a plasma comprises generating a electron cyclotron resonance plasma.

25. A method of etching of a silicon carbide target comprising:

applying a plasma generating potential across an anode and a quartz cathode;

generating a plasma between the anode and the quartz cathode by introducing a mixture of about ten percent nitrous oxide in nitrogen trifluoride therebetween;

positioning a silicon carbide target to be etched on the quartz cathode whereby the quartz cathode exhibits a low sputter yield and is reactive with dissociated fluorine from the nitrogen trifluoride; and

reacting the plasma with the silicon carbide until any surface or subsurface damage caused by the mechanical preparation is substantially removed, but for a time period less than that over which the plasma etch will develop new defects in the surface or aggravate existing ones, to thereby etch the silicon carbide while the reaction of dissociating fluorine with the quartz cathode, and the cathode'"'"'s low sputter yield prevents contamination of the target with either sputtered materials from the cathode or polymerized fluorine species from the plasma.