IP Library Granted Patent US 12668872
Granted Patent B2
US 12668872 · App. 18/396,504 · Granted Jun 30, 2026

Variable-temperature vapor deposition process

Inventor: Paul Connolly Quayle (East Lansing, MI)
Assignee: Great Lakes Crystal Technologies, Inc.
C23C16/276C23C16/277C23C16/52
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Quick Facts
Patent No.
US 12668872
App. No.
18/396,504
Granted
Jun 30, 2026
Kind
B2
Abstract

A method of growing a single crystal diamond material synthesized using a homoepitaxial chemical vapor deposition process. The method includes the steps of placing a free-standing diamond starting seed substrate on a substrate holder within a reaction chamber for chemical vapor deposition; feeding a process gas into the reaction chamber, the process gas including hydrogen gas; igniting a plasma within the reaction chamber to activate the process gas by adjusting the substrate temperature to increase to a first target substrate temperature; adding a carbon-containing gas to the process gas once the substrate temperature is at or near the first target substrate temperature to initiate diamond growth; and adjusting the substrate temperature to a second target substrate temperature that is different from the first target substrate temperature during the diamond growth.

Claims (46)

1 . A method of growing a single crystal diamond material synthesized using a homoepitaxial chemical vapor deposition process, the method comprising:

placing a free-standing diamond starting seed substrate on a substrate holder within a reaction chamber for chemical vapor deposition;

feeding a process gas into the reaction chamber, the process gas including hydrogen gas;

igniting a plasma within the reaction chamber to activate the process gas by adjusting the substrate temperature to increase to a first target substrate temperature;

adding a carbon-containing gas to the process gas once the substrate temperature is at or near the first target substrate temperature to initiate diamond growth; and

adjusting the substrate temperature to a second target substrate temperature that is different from the first target substrate temperature during the diamond growth;

wherein the diamond growth at or near the first target substrate temperature defines a first stage of the diamond growth and the diamond growth at or near the second target substrate temperature defines a second stage of the diamond growth, and wherein the first stage of diamond growth includes bi-dimensional nucleation growth morphologies, and the second stage of diamond growth includes step-flow growth morphologies.

2 . The method of claim 1 , wherein the first target substrate temperature is configured to inhibit hillock and inclusion formation to promote high crystallinity.

3 . The method of claim 1 , further comprising the steps of adjusting the substrate temperature to one or more additional different substrate target temperatures.

4 . The method of claim 1 , wherein the second target substrate temperature is at least 10° C. higher or lower than the first target substrate temperature.

5 . The method of claim 1 , wherein the second target substrate temperature is at least 20° C. higher or lower than the first target substrate temperature.

6 . The method of claim 1 , further comprising adjusting the carbon or non-carbon containing gas concentrations in the process gas during the growth of the diamond.

7 . The method of claim 1 , wherein the process gas further includes a gas selected from the group consisting of nitrogen-carrier gas, boron-carrier gas, phosphorus-carrier gas, n-type dopant carrier gas, p-type dopant carrier gas, and a combination thereof.

8 . The method of claim 1 , wherein the adjusting of the substrate temperature is controlled by adjusting plasma power.

9 . The method of claim 1 , wherein the adjusting of the substrate temperature is controlled by adjusting a resistive substrate holder heater power.

10 . The method of claim 1 , wherein the adjusting of the substrate temperature is controlled by adjusting a cooling water supply.

11 . A method of growing a single crystal diamond material synthesized using a homoepitaxial chemical vapor deposition process, the method comprising:

placing a free-standing diamond starting seed substrate on a substrate holder within a reaction chamber for chemical vapor deposition;

feeding a process gas into the reaction chamber, the process gas including hydrogen gas;

igniting a plasma within the reaction chamber to activate the process gas by adjusting the substrate temperature to increase to be within a first substrate temperature range;

adding a carbon-containing gas to the process gas once the substrate temperature is within the first substrate temperature range to initiate diamond growth; and

adjusting the substrate temperature to a second substrate temperature range that is outside the first substrate temperature range during the diamond growth;

wherein the diamond growth at or near the first target substrate temperature range defines a first stage of the diamond growth and the diamond growth at or near the second target substrate temperature range defines a second stage of the diamond growth, and wherein the first stage of diamond growth includes bi-dimensional nucleation growth morphologies, and the second stage of diamond growth includes step-flow growth morphologies.

12 . The method of claim 11 , wherein the first substrate temperature range is configured to inhibit hillock and inclusion formation to promote crystallinity.

13 . The method of claim 11 , further comprising the steps of adjusting the substrate temperature to one or more different substrate temperature ranges.

14 . The method of claim 13 , wherein the first substrate temperature range, the second substrate temperature range, or the one or more different substrate temperature ranges define a range of ±12° C.

15 . The method of claim 13 , wherein the first substrate temperature range, the second substrate temperature range, or the one or more different substrate temperature ranges define a range of ±10° C.

16 . The method of claim 13 , wherein the first substrate temperature range, the second substrate temperature range, or the one or more different substrate temperature ranges define a range of ±5° C.

17 . The method of claim 13 , wherein the first substrate temperature range, the second substrate temperature range, or the one or more different substrate temperature ranges define a range of ±2° C.

18 . The method of claim 11 , further comprising adjusting carbon or non-carbon containing gas concentrations in the process gas during the growth of the diamond.

19 . The method of claim 11 , wherein the process gas further includes a gas selected from the group consisting of nitrogen-carrier gas, boron-carrier gas, phosphorus-carrier gas, n-type dopant carrier gas, p-type dopant carrier gas, and a combination thereof.

20 . The method of claim 11 , wherein the adjusting of the substrate temperature is controlled by adjusting plasma power.

21 . The method of claim 11 , wherein the adjusting of the substrate temperature is controlled by adjusting a resistive heater.

22 . The method of claim 11 , wherein the adjusting of the substrate temperature is controlled by adjusting a cooling water supply.

23 . A method of growing a single crystal diamond material synthesized using a homoepitaxial chemical vapor deposition process, the method comprising:

placing a diamond substrate on a substrate holder within a chemical vapor deposition reaction chamber;

feeding a process gas into the reaction chamber, the process gas including hydrogen gas;

igniting a plasma within the reaction chamber to activate the process gas by adjusting a substrate temperature to be within a first substrate temperature range defining a bi-dimensional nucleation growth regime;

feeding a carbon-containing gas to the process gas to grow diamond on the diamond substrate within a bi-dimensional nucleation growth regime; and

adjusting the substrate temperature to a second substrate temperature range that is outside the first substrate temperature range during the diamond growth, wherein the second substrate temperature range defines a step-flow growth regime.

24 . The method of claim 23 , wherein the first stage of diamond growth is configured to inhibit hillock and inclusion formation to promote high crystallinity.

25 . The method of claim 23 , further comprising adjusting carbon or non-carbon containing gas concentrations in the process gas during the growth of the diamond.

26 . The method of claim 23 , wherein the process gas further includes a gas selected from the group consisting of nitrogen-carrier gas, boron-carrier gas, phosphorus-carrier gas, n-type dopant carrier gas, p-type dopant carrier gas, and a combination thereof.

27 . The method of claim 23 , wherein the adjusting of the substrate temperature is controlled by adjusting plasma power.

28 . The method of claim 23 , wherein the adjusting of the substrate temperature is controlled by adjusting a resistive heater.

29 . The method of claim 23 , wherein the adjusting of the substrate temperature is controlled by adjusting a cooling water supply.