IP Library Granted Patent US 12,692,437
Granted Patent B2
US 12,692,437 · App. 18/848,658 · Granted Jul 28, 2026

Heat treatment of nanodiamond particles with controlled powder layer depth

Inventor: Yahua Bao (Provo, UT)
Assignee: Schlumberger Technology Corporation
C09K11/65B01J3/062C01B32/28C03C17/22B01J2203/0655B01J2203/0695C01P2006/60C03C2217/42C03C2217/70C03C2218/111C03C2218/116C03C2218/32
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Quick Facts
Patent No.
US 12,692,437
App. No.
18/848,658
Filed
Sep 19, 2024
Granted
Jul 28, 2026
Kind
B2
Art Unit
1718
USPC
427/157
Abstract

Luminescent diamond is made by creating vacancies in diamond grains and heat treating the diamond grains by controlling a thickness of the diamond grains on a substrate. The heat treatment may occur in a temperature range that does not burn the diamond grains, and the controlled thickness produces an even color change and/or promotes oxygen terminations on the diamond particle surfaces.

Claims (37)

1 . A method of making luminescent diamond consisting of:

subjecting a volume of precursor diamond grains to high-pressure/high-temperature conditions in a pressure cell and thereby forming diamond grains with luminescent centers, wherein the high-pressure/high-temperature conditions are from about 1300° C. to about 2500° C. and from about 3.0 GPa to about 10 GPa;

forming a suspension by suspending the diamond grains in a liquid;

adhering the suspension to a substrate and controlling a thickness of the suspension on the substrate;

heat treating the suspension on the substrate at a temperature not exceeding 650° C., thereby changing oxygen terminations on diamond particles of the suspension and increasing a photoluminescence intensity of the diamond grains; and

removing the diamond particles from the substrate and separating the removed diamond particles by grain size.

2 . The method of claim 1 , wherein the luminescent centers include at least one of nitrogen or silicon vacancies.

3 . The method of claim 1 , wherein the liquid includes water.

4 . The method of claim 3 , wherein the liquid includes a surface tension suppressant.

5 . The method of claim 4 , wherein the surface tension suppressant includes alcohol.

6 . The method of claim 1 , wherein the liquid is 10% to 100% alcohol by weight.

7 . The method of claim 1 , wherein the substrate is glass.

8 . The method of claim 1 , wherein the thickness is controlled to be less than 30 μm.

9 . The method of claim 8 , wherein the thickness is controlled to be less than 25 μm.

10 . The method of claim 8 , wherein the thickness is controlled to be between 1 μm and 15 μm.

11 . The method of claim 1 , wherein controlling the thickness includes removing material that exceeds a threshold thickness.

12 . The method of claim 1 , wherein adhering the suspension to the substrate includes drying the suspension.

13 . The method of claim 12 , wherein drying the suspension is performed at a temperature below a boiling point of the liquid and before heat treating the suspension.

14 . The method of claim 1 , wherein adhering the suspension to the substrate includes coating the suspension on the substrate using one or more of dip coating, spin coating, dry coating, or slip casting.

15 . The method of claim 1 , wherein heat treating the suspension includes heat treating at a temperature not exceeding 600° C.

16 . The method of claim 1 , wherein heat treating the suspension includes heat treating at a temperature not exceeding 550° C.

17 . The method of claim 1 , wherein heat treating the suspension is performed for a duration of up to two hours.

18 . The method of claim 1 , wherein heat treating the suspension is performed for a duration of between 30 minutes and 90 minutes.

19 . The method of claim 1 , wherein the pressure cell is configured to impose a differential or asymmetric pressure on the precursor diamond grains.

20 . The method of claim 1 , wherein:

the volume of precursor diamond grains is formed by consolidating and compacting a volume of pre-existing diamond grains; and

the volume of precursor diamond grains comprises intercrystalline diamond bonding.

21 . The method of claim 1 , wherein:

the volume of precursor diamond grains is formed by consolidating and compacting a volume of pre-existing diamond grains; and

the volume of precursor diamond grains does not comprise intercrystalline diamond bonding.

22 . A method of making luminescent diamond consisting of:

subjecting a volume of natural precursor diamond grains with an average grain size of from 10 μm to 50 μm to high-pressure/high-temperature conditions in a pressure cell and thereby forming diamond grains with luminescent centers, wherein the high-pressure/high-temperature conditions are from about 1300° C. to about 2500° C. and from about 3.0 GPa to about 10 GPa;

forming a suspension by separating the diamond grains into a powder and suspending the diamond grains in water;

adhering the suspension to a glass substrate and controlling a thickness of the suspension on the substrate to be from 5 μm to 15 μm, wherein the diamond grains have a concentration of from 0.1% to 10% by weight in the suspension;

heat treating the suspension on the substrate at a temperature in a range between 450° C. and 550° C. for 60 minutes, thereby changing at least one of a color of the suspension or oxygen terminations on diamond particles of the suspension and increasing a photoluminescence intensity of the diamond grains; and

removing the diamond particles from the substrate and separating the removed diamond particles by grain size,

wherein the pressure cell is configured to impose a differential or asymmetric pressure on the precursor diamond grains in order to plastically deform the precursor diamond grains and produce the luminescent centers in the diamond grains.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 31, 2024
From: BAO, YAHUA
To: SCHLUMBERGER TECHNOLOGY CORPORATION
Reel/Frame 069085/0775 →
Continuity (2)
Provisional Application 63366439 · Jun 15, 2022
Related Publication 20250215313A1 · Jul 3, 2025
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