Large area nitride crystal and method for making it

• US 9,564,320 B2
• Filed: 12/31/2012
• Issued: 02/07/2017
• Est. Priority Date: 06/18/2010
• Status: Active Grant

• Current Assignee: SL Technology Incorporated (Reliv' International, Inc.)
• Original Assignee: Soraa, Inc.
• Inventors: Speck, James S., Kamber, Derrick S., Pocius, Douglas W., D'Evelyn, Mark P.
• Primary Examiner(s): Langman, Jonathan
• Application Number:
  US13/731,453
• Publication Number:
  US 20130119401A1
• Time in Patent Office: 1,499 Days
• US Class Current: 1/1
• CPC Class Codes: C30B 19/068 Substrate holders
• CPC Class Codes: C30B 19/12 characterised by the substrate
• CPC Class Codes: C30B 25/02 Epitaxial-layer growth
• CPC Class Codes: C30B 25/18 characterised by the substrate
• CPC Class Codes: C30B 29/403 AIII-nitrides
• CPC Class Codes: C30B 29/406 Gallium nitride
• CPC Class Codes: C30B 33/06 Joining of crystals
• CPC Class Codes: C30B 7/105 using ammonia as solvent, i.e. ammonothermal processes
• CPC Class Codes: H01L 21/0254 Nitrides
• CPC Class Codes: H01L 21/02609 Crystal orientation
• CPC Class Codes: H01L 29/2003 Nitride compounds

Abstract

Techniques for processing materials in supercritical fluids including processing in a capsule disposed within a high-pressure apparatus enclosure are disclosed. The disclosed techniques are useful for growing crystals of GaN, AlN, InN, and their alloys, including InGaN, AlGaN, and AlInGaN for the manufacture of bulk or patterned substrates, which in turn can be used to make optoelectronic devices, lasers, light emitting diodes, solar cells, photoelectrochemical water splitting and hydrogen generation devices, photodetectors, integrated circuits, and transistors.

Claims

1. A gallium-containing nitride merged crystal made from a process comprising:

depositing an adhesion layer on a surface of a handle substrate, said adhesion layer having a melting point at a first temperature;

while said adhesion layer is at a temperature of no less than said first temperature to melt said adhesion layer to enhance its adhesion, bonding at least a first crystal and a second crystal to said adhesion layer to form a tiled substrate, said first crystal having a first nominal crystallographic orientation (x₁ y₁ z₁), and said second crystal having a second nominal crystallographic orientation (x₂ y₂ z₂), said first nominal crystallographic orientation (x₁ y₁ z₁) and said second nominal crystallographic orientation (x₂ y₂ z₂) being identical; and

after said first and second crystals are adhered to said adhesion layer, heat treating said adhesion layer to form a heat-treated adhesion layer, said heat-treated adhesion layer having a melting point at a second temperature higher than said first temperature;

laterally and vertically growing a crystalline composition over said tiled substrate using ammonothermal growth at a third temperature to form a merged crystal, said third temperature being higher than said first temperature and below said second temperature, wherein said first and second crystals define first and second domains in said merged crystal.

2. The crystal of claim 1, wherein each of the first domain and the second domain comprises GaN.

3. The crystal of claim 1, wherein each of the first domain and the second domain is characterized by a dislocation density of less than 10⁶ cm⁻

2.

4. The crystal of claim 1, wherein each of the first domain and the second domain is characterized by a dislocation density of less than 10⁵ cm⁻

2.

5. The crystal of claim 1, wherein each of the first domain and the second domain is characterized by a dislocation density of less than 10⁴ cm⁻

2.

6. The crystal of claim 1, wherein the first domain and the second domain are separated by a line of dislocations with a linear density less than 2×

10⁵ cm<sup>−

1</sup> and the polar misorientation angle γ

between the first domain and the second domain is less than 0.3 degree and the misorientation angles α and

β

are less than 0.6 degree.

7. The crystal of claim 1, wherein the first domain and the second domain are separated by a line of dislocations with a linear density less than 1×

10⁵ cm<sup>−

1</sup> and the polar misorientation angle γ

between the first domain and the second domain is less than 0.1 degree and the misorientation angles α and

β

are less than 0.2 degrees.

8. The crystal of claim 7, wherein the first domain and the second domain are separated by a line of dislocations with a linear density less than 1×

10⁴ cm<sup>−

1</sup> and the polar misorientation angle γ

between the first domain and the second domain is less than 0.05 degrees.

9. The crystal of claim 1, wherein each of the first domain and the second domain are characterized by a nonpolar or semipolar surface crystallographic orientation and one or both of the first domain and the second domain are characterized by a stacking-fault concentration of about 10³ cm⁻

1 or less.

10. The crystal of claim 1, wherein each of the first domain and the second domain is characterized by an impurity concentration of H greater than about 10¹⁷ cm⁻

2 and an impurity concentration of at least one of Li, Na, K, Rb, Cs, F, and Cl greater than about 10¹⁵ cm<sup>−

1</sup>.

11. The crystal of claim 1, further comprising a semiconductor structure overlying at least one of the first domain and the second domain.

12. The crystal of claim 11, wherein an active layer of the semiconductor structure lies within a single domain.

13. The crystal of claim 12, wherein the semiconductor structure forms a portion of a device selected from a light emitting diode, a laser diode, a photodetector, an avalanche photodiode, a transistor, a rectifier, a thyristor, Schottky rectifier, a p-i-n diode, a metal-semiconductor-metal diode, a high-electron mobility transistor, a metal semiconductor field effect transistor, a metal oxide field effect transistor, a power metal oxide semiconductor field effect transistor, a power metal insulator semiconductor field effect transistor, a bipolar junction transistor, a metal insulator field effect transistor, a heterojunction bipolar transistor, a power insulated gate bipolar transistor, a power vertical junction field effect transistor, a cascode switch, an inner sub-band emitter, a quantum well infrared photodetector, a quantum dot infrared photodetector, and a combination of any of the foregoing.

14. The crystal of claim 1, wherein,

each of the first domain and the second domain is characterized by a crystallographic orientation within 5 degrees of a (0 0 0 1) Ga-polar plane;

and

z₁ and z₂ are unit vectors along [0 0 0 −

1], x₁ and x₂ are unit vectors along [1 0 −

1 0], and y₁ and y₂ are unit vectors along [1 −

2 1 0].

15. The crystal of claim 1 wherein,

each of the first domain and the second domain is characterized by a crystallographic orientation within 5 degrees of a {1 0 −

1 0} non-polar plane; and

z₁ and z₂ are unit vectors along [−

1 0 1 0], x₁ and x₂ are unit vectors along [1 −

2 1 0], and y₁ and y₂ are unit vectors along [0 0 0 1].

16. The crystal of claim 1, wherein each of the first domain and the second domain is characterized by a crystallographic orientation within 5 degrees of an orientation selected from a{1 1 −

2 ±

2} plane, a {6 0 −

6 ±

1} plane, a {5 0 −

5 ±

1} plane, a {40 −

4±

1} plane, a {3 0 −

3 ±

1} plane, a {5 0 −

5 ±

2} plane, a {7 0 −

7 ±

3} plane, a {2 0 −

2 ±

1} plane, a {3 0 −

3 ±

2} plane, a {4 0 −

4 ±

3}, a {5 0 −

5 ±

4} plane, a {1 0−

1 ±

1} plane, a {1 0 −

1 ±

2} plane, a {1 0 −

1 ±

3} plane, a {2 1 −

3 ±

1} plane, and a {3 0 −

3 ±

4} plane.

17. The crystal of claim 1, wherein said first domain is characterized by a first lateral dimension and a second lateral dimension, and the second domain is characterized by a third lateral dimension and a fourth lateral dimension, wherein each of the first lateral dimension, the second lateral dimension, the third lateral dimension, and the fourth lateral dimension are greater than 10 millimeters.

18. The crystal of claim 1, wherein each of the first domain and the second domain is characterized by an impurity concentration of 0, H, C, and at least one of Na and K between about 1×

10¹⁶ cm<sup>−

3</sup> and 1×

10¹⁹ cm<sup>−

3</sup>, between about 1×

10¹⁶ cm<sup>−

3</sup> and 2×

10¹⁹ cm<sup>−

3</sup>, below 1×

10¹⁷ cm<sup>−

3</sup>, and between about 3×

10¹⁵ cm<sup>−

3</sup> and 1×

10¹⁸ cm<sup>−

3</sup>, respectively, as quantified by calibrated secondary ion mass spectrometry (SIMS).

19. The crystal of claim 1, wherein each of the first domain and the second domain is characterized by an impurity concentration of O, H, C, and at least one of F and Cl between about 1×

10¹⁶ cm<sup>−

3</sup> and 1×

10¹⁹ cm<sup>−

3</sup>, between about 1×

10¹⁶ cm<sup>−

3</sup> and 2×

10¹⁹ cm<sup>−

3</sup>, below 1×

10¹⁷ cm<sup>−

3</sup>, and between about 1×

10¹⁵ cm<sup>−

3</sup> and 1×

10¹⁷ cm<sup>−

3</sup>, respectively, as quantified by calibrated secondary ion mass spectrometry (SIMS).

20. The crystal of claim 1, wherein said growing comprises epitaxial growth.

21. The crystal of claim 1, wherein

z₁ is a negative surface normal of the first nominal crystallographic orientation, and x₁ and y₁ are crystallographic vectors that are orthogonal to z₁;

z₂ is a negative surface normal of the second nominal crystallographic orientation, and x₂ and y₂ are crystallographic vectors that are orthogonal to z₂;

a polar misorientation angle γ

between z₁ and z₂ is greater than about 0.005 degrees and less than about 0.5 degrees;

a misorientation angle α

between x₁ and x₂ is greater than about 0.01 degrees and less than about 1 degree; and

a misorientation angle β

between y₁ and y₂ is greater than about 0.01 degrees and less than about 1 degree.

22. The crystal of claim 1, wherein said first temperature is no greater than about 500°

C., said second temperature is no less than about 700°

C., and said third temperature is no less than 600°

C.