CVD single crystal diamond material

• US 9,017,633 B2
• Filed: 01/14/2011
• Issued: 04/28/2015
• Est. Priority Date: 01/18/2010
• Status: Active Grant

• Current Assignee: Element Six Technologies US Corporation (Anglo American PLC)
• Original Assignee: Element Six Technologies US Corporation (Anglo American PLC)
• Inventors: Friel, Ian, Geoghegan, Sarah Louise, Twitchen, Daniel James, Dodson, Joseph Michael
• Primary Examiner(s): GREGORIO, GUINEVER S
• Application Number:
  US13/006,682
• Publication Number:
  US 20110176563A1
• Time in Patent Office: 1,565 Days
• Field of Search: None
• US Class Current: 423/446
• CPC Class Codes: C30B 25/02 Epitaxial-layer growth
• CPC Class Codes: C30B 29/04 Diamond
• CPC Class Codes: H01S 3/094 by coherent light
• CPC Class Codes: H01S 3/163 characterised by a crystal matrix
• CPC Class Codes: H01S 3/30 using scattering effects, e.g. stimulated Brillouin or Raman effects
• CPC Class Codes: Y10T 428/24942 including components having same physical characteristic in differing degree
• CPC Class Codes: Y10T 428/26 Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
• CPC Class Codes: Y10T 428/2982 Particulate matter [e.g., sphere, flake, etc.]
• CPC Class Codes: Y10T 428/30 Self-sustaining carbon mass or layer with impregnant or other layer

Abstract

Single crystal diamond material produced using chemical vapour deposition (CVD), and particularly diamond material having properties suitable for use in optical applications such as lasers, is disclosed. In particular, a CVD single crystal diamond material having preferred characteristics of longest linear internal dimension, birefringence and absorption coefficient, when measured at room temperature, is disclosed. Uses of the diamond material, including in a Raman laser, and methods of producing the diamond are also disclosed.

Claims

1. A CVD single crystal diamond material wherein the diamond material has the following characteristics, when measured at room temperature:

a longest linear internal dimension greater than 7 mm, a birefringence of below 1×

10<sup>−

5</sup> determined using a light beam with a cross-sectional area greater than 0.01 mm² and along an internal path greater than 7 mm and an absorption coefficient below 0.010 cm<sup>−

1</sup> determined at a wavelength of 1064 nm.

2. The CVD single crystal diamond material of claim 1, wherein the CVD single crystal diamond material has a longest linear optically accessible dimension of greater than 7 mm.

3. The CVD single crystal diamond material of claim 1, wherein the CVD single crystal diamond material has a property T₂, and T₂, measured at room temperature, is determined to be greater than 4 ps.

4. The CVD single crystal diamond material of claim 1, wherein the CVD single crystal diamond material contains single-substitutional nitrogen in the neutral charge state, wherein the single-substitutional nitrogen in the neutral charge state content within the CVD single crystal diamond material measured by EPR is less than or equal to 5×

10¹⁵ atoms cm<sup>−

3</sup>.

5. The CVD single crystal diamond material of claim 1, wherein the CVD single crystal diamond material contains dislocations, wherein the dislocation density is below 10⁴ dislocations cm⁻

2.

6. The CVD single crystal diamond material of claim 1, wherein the CVD single crystal diamond material exhibits a thermal conductivity, the thermal conductivity, measured at room temperature, being greater than 2000 Wm⁻

1K<sup>−

1</sup>.

7. The CVD single crystal diamond material of claim 1, wherein the CVD single crystal diamond material is grown as a second or subsequent stage in a multi-stage growth process.

8. The CVD single crystal diamond material of claim 7 wherein the multi-stage growth process consists of two stages.

9. The CVD single crystal diamond material of claim 7, wherein the diamond grown during at least one of the previous stages prior to the stage in which the CVD single crystal diamond material of claim 1 is grown possesses an absorption at a wavelength of 1064 nm greater than 0.010 cm⁻

1.

10. The CVD single crystal diamond material of claim 7, wherein the diamond grown during at least one of the previous stages prior to the stage in which the CVD single crystal diamond material of claim 1 is grown possesses a longest linear internal dimension less than 7 mm.

11. The CVD single crystal diamond material of any of claim 7, wherein the diamond grown during at least one of the previous stages prior to the stage in which the CVD single crystal diamond material of claim 1 is grown contains single substitutional nitrogen in the neutral charge state, the single substitutional nitrogen in the neutral charge state content within one of the previous stages measured by EPR being greater than 1×

10¹⁶ atoms cm<sup>−

3</sup>.

18. A method of producing the CVD single crystal diamond of claim 1 wherein the CVD technique includes multiple growth stages.

19. The method of claim 18 wherein the CVD single crystal diamond material of claim 1 is produced in a stage of growth after the first stage of growth.

20. The method of claim 18, wherein the CVD technique utilises a gas phase, the gas phase containing nitrogen which is incorporated into the growing diamond material, the stages of the growth process being distinguished by a change in the incorporation rate of nitrogen within the deposited diamond.

21. The method of claim 20 wherein the incorporation rate of nitrogen is decreased relative to at least one of the earlier growth stages for the growth stage that produces the CVD single crystal diamond of claim 1.

22. The method of claim 20 wherein the incorporation rate of nitrogen is altered by changing the concentration of nitrogen in the process gas.

23. The method of claim 22 wherein the incorporation of nitrogen is decreased by decreasing the concentration of nitrogen in the process gas.

24. The method of claim 22, wherein the nitrogen concentration within the gas phase is between 300 parts per billion and 5 parts per million, calculated as molecular nitrogen, during at least one stage of growth prior to a final stage of growth.

25. The method of claim 24, wherein the nitrogen concentration is between 0.001 parts per billion and 250 parts per billion, calculated as molecular nitrogen, during a subsequent growth stage.

12. A Raman laser containing a Raman scattering medium comprising a CVD single crystal diamond material, wherein the diamond material has the following characteristics, when measured at room temperature:

a longest linear internal dimension greater than 7 mm, a birefringence of below 1×

10<sup>−

5</sup> determined using a light beam with a cross-sectional area greater than 0.01 mm² and along an internal path greater than 7 mm and an absorption coefficient below 0.010 cm<sup>−

1</sup> determined at a wavelength of 1064 nm.

13. The Raman laser of claim 12 further comprising a pumping light source, wherein the pumping light source produces a pumping light beam having a wavelength that is different to an output light beam of the laser by one or more Stokes shifts of the Raman scattering medium.

14. The Raman laser of claim 13, wherein the output light beam has a beam quality defined by a M² factor, the M² factor of the output light beam being less than 10.0.

15. The Raman laser of claim 12, wherein the CVD single crystal diamond material exhibits a thermal figure of merit, the thermal figure of merit being at 1.064 μ

m being greater than 600.

16. A method of producing a CVD single crystal diamond within a CVD reactor using a gas phase with multiple growth stages, at least two of the multiple growth stages being distinguished by changing the nitrogen concentration in the gas phase within the CVD reactor, at least one of the at least two growth stages having a nitrogen concentration within the gas phase of greater than or equal to 300 parts per billion and less than 5 parts per million, calculated as molecular nitrogen, and at least one other of the at least two growth stages having a nitrogen concentration within the gas phase of greater than 0.001 parts per billion and less than 250 parts per billion, calculated as molecular nitrogen, wherein the diamond material has the following characteristics, when measured at room temperature:

a longest linear internal dimension greater than 7 mm, a birefringence of below 1×

10<sup>−

5</sup> determined using a light beam with a cross-sectional area greater than 0.01 mm² and along an internal path greater than 7 mm and an absorption coefficient below 0.010 cm<sup>−

1</sup> determined at a wavelength of 1064 nm.

17. The method of claim 16, wherein the multiple growth stages consist of two stages.