Process for manufacturing synthetic single crystal diamond material using a pressure driven growth process and a plurality of seed pads with each seed pad comprising a plurality of single crystal diamond seeds

Patent metadata

Field	Value
Publication number	US-10370773-B2
Application number	US-201314383074-A
Country	US
Kind code	B2
Filing date	Mar 13, 2013
Priority date	Mar 15, 2012
Publication date	Aug 6, 2019
Grant date	Aug 6, 2019

Abstract

A method for manufacturing a plurality of synthetic single crystal diamonds, the method comprising: forming a plurality of seed pads, each seed pad comprising a plurality of single crystal diamond seeds anchored to, or embedded in, an inert holder; loading a carbon source, a metal catalyst, and the plurality of seed pads into a capsule; loading the capsule into a high pressure high temperature (HPHT) press; and subjecting the capsule to a HPHT growth cycle to grow single crystal diamond material on the plurality of single crystal diamond seeds, the HPHT growth cycle comprising: initiating HPHT growth of single crystal diamond material on the plurality of single crystal diamond seeds by increasing pressure and temperature; maintaining HPHT growth of single crystal diamond material on the plurality of single crystal diamond seeds via a pressure driven growth process by controlling and maintaining pressure and temperature; and terminating HPHT growth of single crystal diamond material on the plurality of single crystal diamond seeds by reducing pressure and temperature, wherein the plurality of single crystal diamond seeds remain anchored to, or embedded in, the inert holders during the HPHT growth cycle.

First claim

The invention claimed is:

1. A method for manufacturing a plurality of synthetic single crystal diamonds, the method comprising:
forming a plurality of seed pads, each seed pad comprising a plurality of single crystal diamond seeds anchored to an inert holder;
loading a carbon source, a metal catalyst, and the plurality of seed pads into a capsule, wherein the carbon source and the metal catalyst are mixed to form a reaction mixture comprising graphite in an amount in a range of from 16 to 35 wt. %, and at least a portion of the carbon source is located less than 0.1 mm from the single crystal diamond seeds;
loading the capsule into a high pressure high temperature (HPHT) press; and
subjecting the capsule to a HPHT growth cycle to grow single crystal diamond material on the plurality of single crystal diamond seeds, the HPHT growth cycle comprising:
initiating HPHT growth of single crystal diamond material on the plurality of single crystal diamond seeds by increasing pressure and temperature;
maintaining HPHT growth of single crystal diamond material on the plurality of single crystal diamond seeds via a pressure driven growth process by controlling and maintaining pressure and temperature for at least 20 hours; and
terminating HPHT growth of single crystal diamond material on the plurality of single crystal diamond seeds by reducing pressure and temperature,
wherein the plurality of single crystal diamond seeds remain anchored to the inert holders during the HPHT growth cycle, and
wherein the inert holder comprises a ceramic material.

2. A method according to claim 1 , wherein each seed pad comprises a number of single crystal diamond seeds in a range of from 8 to 3000 and/or wherein each seed pad comprises a density of single crystal diamond seeds in a range of from 0.3 to 45 seeds cm −2 .

3. A method according to claim 1 , wherein the capsule comprises a number of seed pads in a range of from 4 to 30.

4. A method according to claim 1 , wherein the seeds pads are spaced apart within the capsule such that a distance between the seeds pads is selected to be in a range of from 1 to 10-times a height of the single crystal diamond material after terminating HPHT growth and/or wherein the seeds pads are spaced apart within the capsule such that a distance between the seeds pads is selected to be in a range of from 1.0 to 12 mm.

5. A method according to claim 1 , wherein the carbon source material has a total impurity level no more than 0.1%-by weight.

6. A method according to claim 1 , wherein the carbon source material has a surface area per gram in a range of from 0.001 m 2 /g to 10 m 2 /g.

7. A method according to claim 1 , wherein the reaction mixture comprises powdered metal catalyst in an amount in the range of from 65% to 84% by weight prior to the HPHT growth cycle.

8. A method according to claim 1 , wherein the initiating step comprises raising the pressure to a target starting value P s which is below the Berman-Simon graphite/diamond thermodynamic phase stability line, raising the temperature to a value T g which exceeds a eutectic temperature for the carbon source and the metal catalyst, holding the temperature and pressure for a time t, and then raising the pressure to a target starting value P g for the maintaining step to initiate HPHT growth.

9. A method according to claim 8 , wherein the time t is in a range of from 1 to 36000 seconds.

10. A method according to claim 8 , wherein the temperature T g is in a range of from 1070 Kelvin to 2470 Kelvin.

11. A method according to claim 8 , wherein the pressure P s is within 0.01 to 2.0 GPa of pressure P g .

12. A method according to claim 8 , wherein the pressure P g is in a range of from 4.0 to 8.0 GPa.

13. A method according to claim 8 , wherein the pressure is raised from P s to P g at a rate in a range of from 0.001 to 1.0 GPa per minute.

14. A method according to claim 1 , wherein, during the maintaining step, a temperature difference between a top side and a bottom side of the capsule is maintained to be no more than 100 Kelvin.

15. A method according to claim 1 , wherein, during the maintaining step, a temperature gradient between a top side and a bottom side of the capsule is maintained to be no more than 0.66 Kelvin mm −1 .

16. A method according to claim 1 , wherein during the maintaining step the press moves anvils inwards whereby a volume of the capsule reduces by an amount in a range of from 0.5% to 50% and/or wherein during the maintaining step the press moves anvils inwards by a combined distance in the range of from 1 mm to 100 mm.

17. A method according to claim 1 , wherein during the maintaining step the temperature is decreased in a continuous or stepwise manner while maintaining growth of single crystal diamond material on the plurality of single crystal diamond seeds.

18. A method according to claim 17 , wherein the temperature is decreased at a rate in a range of from 0.1 Kelvin/hour to 2 Kelvin/hour.

19. An apparatus configured to perform the method according to claim 1 , the apparatus comprising:
a capsule comprising a plurality of seed pads and reactants including a carbon source and a metal catalyst, wherein the reactants and seed pads are provided in alternating layers, and wherein each seed pad comprises a plurality of single crystal diamond seeds anchored to, or embedded in, an inert holder; and
a HPHT press comprising a heating circuit configured to maintain a substantially uniform temperature throughout the capsule whereby diamond growth on the single crystal seeds is achieved via a pressure driven growth process.

20. A method according to claim 1 , wherein at least a portion of the carbon source is located less than 0.05 mm from the single crystal diamond seeds.

Assignees

• Element Six Tech Ltd

Inventors

• Borse Dietrich
• Gura Eugen
• Dodge Carlton Nigel
• Spits Raymond Anthony

Classifications

• C30B29/04 Primary

  Diamond · CPC title

• B01J2203/068

  Crystal growth · CPC title

• B01J2203/0655

  Diamond · CPC title

• B01J2203/0625

  Carbon · CPC title

• B01J23/755

  Nickel · CPC title