Method for quantification of extended defects in gallium-containing nitride crystals

1. A method for quantifying extended defects in a gallium-containing nitride crystal, wafer, or device, comprising:

providing a gallium-containing nitride crystal, wafer, or device, wherein the crystal, wafer, or device comprises gallium and nitrogen, has a wurtzite crystal structure, and comprises a first surface having a crystallographic orientation that is miscut from a {10-10} m-plane by between about 0.01 degrees and about 60 degrees toward a [000-1] −c-direction and by up to about 10 degrees toward an orthogonal <1-210> a-direction;

preparing an etchant composition;

processing the gallium-containing nitride crystal, wafer, or device in the etchant composition at a temperature between about 100 degrees Celsius and about 500 degrees Celsius for a time between about 5 minutes and about 5 hours, wherein the processing temperature and time are selected so as to cause formation of etch pits with diameters between about 1 micrometer and about 25 micrometers;

removing the gallium-containing nitride crystal, wafer, or device from the etchant composition; and

quantifying a concentration of at least one of etch pits and etch grooves,

wherein quantifying the concentration of etch pits is performed by counting a number of the etch pits within a field of view; and quantifying the concentration of etch grooves is performed by calculating a total length of the etch grooves within a field of view.

2. The method of claim 1 , wherein the etchant composition comprises one or more of NaOH and KOH.

3. The method of claim 1 , wherein the etchant composition comprises a solution of one or more of H 3 PO 4 , H 3 PO 4 that has been conditioned by prolonged heat treatment to form polyphosphoric acid, and H 2 SO 4 .

4. The method of claim 3 , wherein the etchant composition is prepared by conditioning of reagent-grade phosphoric acid to form polyphosphoric acid.

5. The method of claim 1 , wherein the first surface has been prepared by chemical-mechanical polishing prior to performing the etch treatment.

6. The method of claim 1 , further comprising protecting one or more surfaces of the gallium-containing nitride crystal using one or more of an etch-resistant tape, clamping an end or face of a crystal against an etch-resistant material, and coating with a paint comprising an etch-resistant material.

7. The method of claim 1 , further comprising preparing a second surface that is substantially parallel to the first surface, wherein both the first surface and the second surface are chemical-mechanically polished, and processing both the first surface and the second surface in the etchant composition simultaneously.

8. The method of claim 1 , wherein the gallium-containing nitride crystal, wafer, or device has been grown in an m-direction, the first surface is miscut from a {10-10} m-plane by between about 1 degree and about 5 degrees toward a [000-1] −c-direction and by up to about 5 degrees toward an orthogonal <1-210> a-direction, and the concentration of at least one of threading dislocations and stacking faults is determined as a function of distance from the m-plane growth surface.

9. The method of claim 1 , wherein the first surface has a crystallographic orientation that is miscut from a {10-10} m-plane by between about 0.05 degree and about 60 degrees toward a [000-1] −c-direction and by up to about 10 degrees toward an orthogonal <1-210> a-direction.

10. A method for quantifying extended defects in a gallium-containing nitride crystal, wafer, or device, comprising:

providing a gallium-containing nitride crystal, wafer, or device, wherein the crystal, wafer, or device comprises gallium and nitrogen, has a wurtzite crystal structure, and comprises a surface having a crystallographic orientation within 5 degrees of a (0001) +c-plane;

preparing a first etchant composition;

processing the gallium-containing nitride crystal, wafer, or device in the first etchant composition at a temperature between about 100 degrees Celsius and about 500 degrees Celsius for a time between about 30 seconds and about 5 hours, wherein the processing temperature and time are selected so as to cause formation of etch pits with diameters between about 1 micrometer and about 25 micrometers;

removing the gallium-containing nitride crystal, wafer, or device from the first etchant composition;

quantifying a concentration of at least one of etch pits and etch grooves on a (0001) +c-plane surface;

preparing a vicinal m-plane surface on the gallium-containing nitride crystal, wafer, or device, the vicinal m-plane surface having a crystallographic orientation that is miscut from a {10-10} m-plane by between about 0.01 degree and about 5 degrees toward a [000-1] −c-direction and by up to about 10 degrees toward an orthogonal <1-210> a-direction;

preparing a second etchant composition;

processing the gallium-containing nitride crystal gallium-containing nitride crystal, wafer, or device in the second etchant composition at a temperature between about 100 degrees Celsius and about 500 degrees Celsius for a time between about 5 minutes and about 5 hours, wherein the processing temperature and time are selected so as to cause formation of etch pits with diameters between about 1 micrometer and about 25 micrometers on the vicinal m-plane surface;

removing the gallium-containing nitride crystal gallium-containing nitride crystal, wafer, or device from the second etchant composition; and

quantifying a concentration of at least one of etch pits and etch grooves on the vicinal m-plane surface,

wherein quantifying the concentration of etch pits is performed by counting a number of the etch pits within a field of view; and quantifying the concentration of etch grooves is performed by calculating a total length of the etch grooves within the field of view.

11. The method of claim 10 , wherein the first etchant composition comprises one or more of NaOH and KOH and the gallium-containing nitride crystal, wafer, or device is processed in the first etchant composition at a temperature between about 170 degrees Celsius and about 500 degrees Celsius for a time between about five minutes and about five hours.

12. The method of claim 10 , wherein the second etchant composition is a solution comprising one or more of H 3 PO 4 , H 3 PO 4 that has been conditioned by prolonged heat treatment to form polyphosphoric acid, and H 2 SO 4 .

13. The method of claim 12 , wherein the second etchant composition is prepared by conditioning of reagent-grade phosphoric acid to form polyphosphoric acid, increasing its boiling point.

14. The method of claim 10 , wherein the vicinal m-plane surface has been prepared by chemical-mechanical polishing prior to performing the etch treatment.

15. The method of claim 10 , further comprising protecting one or more surfaces of the gallium-containing nitride crystal using one or more of an etch-resistant tape, clamping an end or face of a crystal against an etch-resistant material, and coating with a paint comprising an etch-resistant material.

16. A method for quantifying extended defects in a gallium-containing nitride crystal, wafer, or device, comprising:

providing a gallium-containing nitride crystal, wafer, or device, wherein the crystal, wafer, or device comprises gallium and nitrogen, has a wurtzite crystal structure, and comprises a surface having a crystallographic orientation that is miscut from a {10-10} m-plane by between about −1 degree and about +60 degrees toward a [000-1] −c-direction and by up to about 10 degrees toward an orthogonal <1-210> a-direction;

preparing an etchant composition; the etchant composition comprising a solution prepared by conditioning of reagent-grade phosphoric acid to form polyphosphoric acid, increasing its boiling point;

processing the gallium-containing nitride crystal, wafer, or device in the etchant composition at a temperature between about 100 degrees Celsius and about 500 degrees Celsius for a time between about 5 minutes and about 5 hours, wherein the processing temperature and time are selected so as to cause formation of etch pits with diameters between about 1 micrometer and about 25 micrometers;

removing the gallium-containing nitride crystal, wafer, or device from the etchant composition; and

quantifying a concentration of at least one of etch pits and etch grooves,

wherein quantifying the concentration of etch pits is performed by counting a number of the etch pits within a field of view; and quantifying the concentration of etch grooves is performed by calculating a total length of the etch grooves within the field of view.

17. The method of claim 16 , further comprising protecting one or more surfaces of the gallium-containing nitride crystal using one or more of an etch-resistant tape, clamping an end or face of a crystal against an etch-resistant material, and coating with a paint comprising an etch-resistant material.

18. The method of claim 16 , wherein the surface having a crystallographic orientation that is miscut from a {10-10} m-plane by between about −1 degree and about +60 degrees toward a [000-1] −c-direction and by up to about 10 degrees toward an orthogonal <1-210> a-direction has been prepared by chemical-mechanical polishing prior to performing etch treatment.

19. A method for quantifying extended defects in a gallium-containing nitride crystal, wafer, or device, comprising:

providing a gallium-containing nitride crystal, wafer, or device, wherein the crystal, wafer, or device comprises gallium and nitrogen, has a wurtzite crystal structure, and comprises a surface having a crystallographic orientation within 5 degrees of a (0001) +c-plane;

preparing a first etchant composition;

processing the gallium-containing nitride crystal, wafer, or device in the first etchant composition at a temperature between about 100 degrees Celsius and about 500 degrees Celsius for a time between about 5 minutes and about 5 hours, wherein the processing temperature and time are selected so as to cause formation of etch pits with diameters between about 1 micrometer and about 25 micrometers;

removing the gallium-containing nitride crystal, wafer, or device from the first etchant composition;

quantifying a concentration of at least one of etch pits and etch grooves on a (0001) +c-plane surface;

preparing a vicinal m-plane surface on the gallium-containing nitride crystal, wafer, or device, the vicinal m-plane surface having a crystallographic orientation that is miscut from a {10-10} m-plane by between about 0.05 degree and about 5 degrees toward a [000-1] −c-direction and by up to about 5 degrees toward an orthogonal <1-210> a-direction;

preparing a second etchant composition;

processing the gallium-containing nitride crystal gallium-containing nitride crystal, wafer, or device in the second etchant composition at a temperature between about 100 degrees Celsius and about 500 degrees Celsius for a time between about 5 minutes and about 5 hours, wherein the processing temperature and time are selected so as to cause formation of etch pits with diameters between about 1 micrometer and about 25 micrometers on the vicinal m-plane surface;

removing the gallium-containing nitride crystal gallium-containing nitride crystal, wafer, or device from the second etchant composition; and

quantifying the concentrations of at least one of etch pits and etch grooves on the vicinal m-plane surface,

wherein quantifying the concentration of etch pits is performed by counting a number of the etch pits within a field of view; and quantifying the concentration of etch grooves is performed by calculating a total length of the etch grooves within the field of view.

20. The method of claim 19 , wherein the vicinal m-plane surface has been prepared by chemical-mechanical polishing prior to performing the etch treatment.