Methods for forming large area single crystal diamond substrates with high crystallographic alignment

Patent metadata

Field	Value
Publication number	US-12098475-B2
Application number	US-201917055943-A
Country	US
Kind code	B2
Filing date	May 16, 2019
Priority date	May 18, 2018
Publication date	Sep 24, 2024
Grant date	Sep 24, 2024

Abstract

The disclosure relates to large area single crystal diamond (SCD) surfaces and substrates, and their methods of formation. Typical large area substrates can be at least about 25 mm, 50 mm, or 100 mm in diameter or square edge length, and suitable thicknesses can be about 100 μm to 1000 μm. The large area substrates have a high degree of crystallographic alignment. The large area substrates can be used in a variety of electronics and/or optics applications. Methods of forming the large area substrates generally include lateral and vertical growth of SCD on spaced apart and crystallographically aligned SCD seed substrates, with the individual SCD growth layers eventually merging to form a composite SCD layer of high quality and high crystallographic alignment. A diamond substrate holder can be used to crystallographically align the SCD seed substrates and reduce the effect of thermal stress on the formed SCD layers.

First claim

What is claimed is:

1. A method for forming a large area single crystal diamond
(SCD) surface, the method comprising:
(a) providing a first SCD substrate having a growth surface;
(b) providing a second SCD substrate having a growth surface, wherein
(i) the second SCD substrate is spaced apart from and crystallographically aligned within 1° with the first SCD substrate, and
(ii) the first SCD substrate and the second SCD substrate are spaced apart by a first distance of 0.5 mm to 5 mm;

(c) depositing a first SCD layer on the first SCD growth surface and a second SCD layer on the second SCD growth surface for a first time period, the layers extending both vertically and laterally relative to their respective growth surfaces;
(d) pausing deposition of the first SCD layer and the second SCD layer after the first time period, and then polishing (i) the first SCD layer to form a first polished SCD layer (ii) the second SCD layer to form a second polished SCD layer; and
(e) continuing deposition of the first SCD layer on the first polished SCD layer and the second SCD layer on the second polished SCD layer for a second time period at least until they join together to form a composite SCD layer, wherein upper adjacent edges of the first polished SCD layer and the second polished SCD layer are within 100 μm;
wherein providing the first SCD substrate and providing the second SCD substrate comprises:
providing a diamond substrate holder comprising (i) a first recess sized and shaped to receive the first SCD substrate and (ii) a second recess sized and shaped to receive the second SCD substrate, wherein the first recess and the second recess are spaced apart and positioned relative to each other such that the first SCD substrate and the second SCD substrate are crystallographically aligned when placed in their respective recesses; and
placing the first SCD substrate in the first recess such that the first SCD substrate growth surface is at or above a surrounding top surface of the diamond substrate holder; and
placing the second SCD substrate in the second recess such that the second SCD substrate growth surface is at or above a surrounding top surface of the diamond substrate holder.

2. The method of claim 1 , further comprising:
(f) cutting and optionally polishing the composite SCD layer to form a large area SCD substrate therefrom.

3. The method of claim 2 , wherein the large area SCD substrate has a thickness in a range of 0.1 mm to 5 mm.

4. The method of claim 2 , further comprising:
(g) cutting and optionally polishing the large area SCD substrate into a plurality of smaller SCD substrates each having a growth surface; and
(h) repeating steps (a)-(e) with at least two of the smaller SCD substrates as the first SCD substrate and the second SCD substrate.

5. The method of claim 1 , wherein:
the diamond substrate holder is formed from SCD; and
the surrounding top surface of the diamond substrate holder further comprises a metal masking layer thereon.

6. The method of claim 1 , wherein the diamond substrate holder is formed from polycrystalline diamond (PCD).

7. The method of claim 1 , wherein:
the growth surface of the first SCD substrate is a ( 100 ) crystallographic surface; and
the growth surface of the second SCD substrate is a ( 100 ) crystallographic surface.

8. The method of claim 1 , wherein the first SCD substrate and the second SCD substrate are spaced apart by a distance of 0.7 mm to 4 mm.

9. The method of claim 1 , wherein:
the distance is a normal distance between an edge or sidewall of the first SCD substrate and a corresponding edge or sidewall of the second SCD substrate; and
the edge or sidewall of the first SCD substrate is crystallographically complementary to the corresponding edge or sidewall of the second SCD substrate.

10. The method of claim 9 , wherein providing the first SCD substrate and providing a second SCD substrate comprises:
cutting a master SCD substrate along a cutting surface to form the first SCD substrate and the second SCD substrate as separate structures; and
aligning the first SCD substrate and the second SCD substrate such that the edge or sidewall of the first SCD substrate and the edge or sidewall of the second SCD substrate both correspond to the cutting surface from the master SCD substrate.

11. The method of claim 1 , wherein the first SCD substrate and the second SCD substrate each independently have:
a growth surface area in a range of 1 mm 2 to 625 mm 2 ; and
a thickness in a range of 0.1 mm to 5 mm.

12. The method of claim 1 , wherein depositing the first SCD layer and the second SCD layer comprises performing a chemical vapor deposition (CVD) process comprising operating a microwave plasma-assisted reactor in combination with a deposition source gas at a temperature and pressure sufficient to deposit the first SCD layer and the second SCD layer.

13. The method of claim 1 , wherein the first SCD layer and the second SCD layer grow freely in an open growth volume and not in contact with a support surface.

14. The method of claim 1 , wherein:
the first SCD layer and the second SCD layer have a vertical growth rate in a range of 1 μm/h to 100 μm/h;
the first SCD layer and the second SCD layer have a lateral growth rate in a range of 1 μm/h to 100 μm/h; and
the first SCD layer and the second SCD layer have a ratio of vertical growth rate:lateral growth rate in a range of 0.1 to 10.

15. The method of claim 1 , wherein:
the composite SCD layer has a thickness in a range of 0.1 mm to 5 mm; and
the composite SCD layer has a top surface area that is at least 1.1 times the combined surface area of the first SCD substrate growth surface and the second SCD substrate growth surface.

16. The method of claim 1 , wherein the composite SCD layer has a crystallographic alignment of 1° or less.

17. The method of claim 1 , wherein crystallographic alignment is expressed as an angle between (i) a first direction that is a crystallographic direction in the first SCD substrate and (ii) a second direction that is the corresponding crystallographic direction in the second SCD substrate.

18. The method of claim 17 , wherein the crystallographic direction is the direction.

19. The method of claim 1 , wherein providing the first SCD substrate and providing the second SCD substrate further comprises:
providing a substrate holder having a top surface and defining a recess therein, wherein the diamond substrate holder is positioned in the substrate holder recess such that the substrate holder top surface is above each of (i) the first SCD substrate growth surface, (ii) the second SCD substrate growth surface, and (ii the surrounding top surface of the diamond substrate holder.

20. The method of claim 19 , wherein:
the substrate holder is a metal substrate holder having one or more sidewalls defining the substrate holder recess; and
the first SCD substrate and the second SCD substrate are spaced apart from the one or more sidewalls of the metal substrate holder.

21. The method of claim 1 , wherein the upper adjacent edges of the first polished SCD layer and the second polished SCD layer are within 50 μm.

22. The method of claim 1 , wherein at least a portion of the upper adjacent edges of the first polished SCD layer and the second polished SCD layer are in contact with each other.

23. The method of claim 1 , wherein, during step (e), the first SCD substrate and the second SCD substrate are

Assignees

• Univ Michigan State
• Fraunhofer Usa

Inventors

• Grotjohn Timothy A
• Diaz Ramon
• Hardy Aaron

Classifications

• H10P14/24

  using chemical vapour deposition [CVD] · CPC title

• H10P14/3406

  Carbon, e.g. diamond-like carbon · CPC title

• H10P14/2903

  Carbon, e.g. diamond-like carbon · CPC title

• H10D62/405

  Orientations of crystalline planes · CPC title

• C30B29/68

  Crystals with laminate structure, e.g. "superlattices" · CPC title