IP Library Granted Patent US 10,173,899
Granted Patent B1
US 10,173,899 · App. 15/065,246 · Granted Jan 8, 2019

Aqueous leaching solutions and methods of leaching at least one interstitial constituent from a polycrystalline diamond body using the same

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Quick Facts
Patent No.
US 10,173,899
App. No.
15/065,246
Granted
Jan 8, 2019
Kind
B1
Abstract

In an embodiment, a method of fabricating a leached polycrystalline diamond (“PCD”) body is disclosed. The PCD body includes bonded diamond grains defining interstitial regions at least a portion of which include at least one interstitial constituent disposed therein. The method includes leaching the PCD body with a leaching agent to remove at least a portion of the at least one interstitial constituent therefrom. The leaching agent includes a mixture having hydrofluoric acid in a first concentration of about 10 weight % to about 50 weight %, nitric acid in a second concentration of about 5 weight % to about 25 weight %, and water in a third concentration of about 25 weight % to about 85 weight %. Further embodiments relate to different leaching methods and different leaching agent compositions.

Claims (30)

1. A method of fabricating an at least partially leached polycrystalline diamond table, the method comprising;

providing a polycrystalline diamond table including a plurality of bonded diamond grains defining a plurality of interstitial regions at least a portion of which include at least one interstitial constituent disposed therein; and

leaching the polycrystalline diamond table with a leaching agent to remove at least a portion the at least one interstitial constituent from the polycrystalline diamond table to form an at least partially leached polycrystalline diamond table, wherein the leaching agent includes a mixture having a ratio of weight % hydrofluoric acid to weight % nitric acid of about 1.0 to about 2.4, and water in a concentration of about 50 weight % to about 85 weight %.

2. The method of claim 1 , wherein leaching the polycrystalline diamond table with the leaching agent to remove at least a portion of the at least one interstitial constituent from the polycrystalline diamond table includes removing substantially all of the at least one interstitial constituent from the entire polycrystalline diamond table.

3. The method of claim 1 , further comprising, after the act of leaching, bonding a substrate to the at least partially leached polycrystalline diamond table in a high-temperature/high-pressure process effective to at least partially infiltrate the at least partially leached polycrystalline diamond table with at least one infiltrant from the substrate to form a polycrystalline diamond compact.

4. The method of claim 3 , further comprising, after the act of bonding, leaching the polycrystalline diamond compact to remove at least a portion of the at least one infiltrant from the polycrystalline diamond table of the polycrystalline diamond compact.

5. The method of claim 1 , wherein the concentration of hydrofluoric acid is about 25 weight % to about 30 weight %, the concentration of nitric acid is about 10 weight % to about 15 weight %, and the concentration of water is about 55 weight % to about 65 weight %.

6. The method of claim 1 , wherein the concentration of hydrofluoric acid is greater than about 15 weight % and the concentration of nitric acid is less than about 20 weight %.

7. The method of claim 6 , wherein the mixture exhibits a viscosity of less than about 0.5 centipoise.

8. The method of claim 1 , wherein the concentration of hydrofluoric acid is about 15 weight % to about 25 weight % and the concentration of nitric acid is about 10 weight % to about 20 weight %.

9. The method of claim 8 , wherein the mixture exhibits a viscosity of less than about 0.4 centipoise.

10. A method of fabricating a polycrystalline diamond compact, the method comprising:

providing a polycrystalline diamond table including an interfacial surface bonded to a substrate and an opposing upper surface, wherein the polycrystalline diamond table includes a plurality of bonded diamond grains defining a plurality of interstitial regions at least a portion of which include at least one interstitial constituent disposed therein; and

leaching the polycrystalline diamond table with a leaching agent to remove at least a portion of the at least one interstitial constituent from the polycrystalline diamond table, wherein the leaching agent includes a mixture having a ratio of weight % hydrofluoric acid to weight % nitric acid of about 1.0 to about 2.4, and water in a concentration of about 50 weight % to about 85 weight %.

11. The method of claim 10 , wherein the concentration of hydrofluoric acid is about 25 weight % to about 30 weight %, the concentration of nitric acid is about 10 weight % to about 15 weight %, and the concentration of water is about 55 weight % to about 65 weight %.

12. The method of claim 10 , wherein the concentration of hydrofluoric acid is greater than about 15 weight % and the concentration of nitric acid is less than about 20 weight %.

13. The method of claim 12 , wherein the mixture exhibits a viscosity of less than about 0.5 centipoise.

14. The method of claim 10 , wherein the concentration of hydrofluoric acid is about 15 weight % to about 25 weight % and the concentration of nitric acid is about 10 weight % to about 20 weight %.

15. The method of claim 14 , wherein the mixture exhibits a viscosity of less than about 0.4 centipoise.

16. The method of claim 10 , wherein the mixture includes one or more additional constituents composed to reduce a viscosity of the mixture.

17. The method of claim 10 , wherein leaching the polycrystalline diamond table with the leaching agent to remove at least a portion of the at least one interstitial constituent from the polycrystalline diamond table includes leaching the polycrystalline diamond table with the leaching agent at a temperature greater than about 75° C.

18. The method of claim 10 , further comprising, prior to the act of leaching, positioning at least a portion of the polycrystalline diamond compact in a protective leaching cup.

19. The method of claim 18 , wherein the protective leaching cup includes at least one of polyethylene, polypropylene, linear low density polyethylene, chlorosulfanted polyethylene, chlorinated polyethylene, polypropylene, fluoropolymer, perfluoroalkoxy, Kynar®, or Viton®.

20. A method of fabricating a polycrystalline diamond compact, the method comprising;

providing a polycrystalline diamond table including an interfacial surface bonded to a substrate and an opposing upper surface, wherein the polycrystalline diamond table includes a plurality of bonded diamond grains defining a plurality of interstitial regions at least a portion of which include at least one interstitial constituent disposed therein; and

leaching the polycrystalline diamond table with a leaching agent to remove at least a portion of the at least one interstitial constituent from the polycrystalline diamond table, wherein the leaching agent includes a mixture having a ratio of weight % hydrofluoric acid to weight % nitric acid of about 1.0 to about 2.4, the mixture exhibiting a viscosity of less than about 0.55 centipoise.

21. The method of claim 20 , wherein the hydrofluoric acid is present in the mixture in a concentration that is greater than about 15 weight % and the nitric acid is present in the mixture in a concentration that is less than about 20 weight %.

22. The method of claim 20 , wherein the hydrofluoric acid is present in the mixture in a concentration that is about 15 weight % to about 25 weight % and the nitric acid is present in the mixture in a concentration that is about 10 weight % to about 20 weight %.

23. The method of claim 22 , wherein the viscosity is less than about 0.4 centipoise.

24. The method of claim 10 , wherein leaching the polycrystalline diamond table with the leaching agent to remove at least a portion of the at least one interstitial constituent from the polycrystalline diamond table includes leaching the polycrystalline diamond table with the leaching agent for more than about 100 hours with the leaching agent at a temperature greater than about 25° C.

Assignments (6)
SECURITY INTEREST Recorded Jul 18, 2025
From: US SYNTHETIC CORPORATION
To: KEYBANK NATIONAL ASSOCIATION
Reel/Frame 074973/0089 →
RELEASE OF SECURITY INTEREST IN PATENTS Recorded Jul 17, 2025
From: JPMORGAN CHASE BANK, N.A.
To: CHAMPIONX LLC; APERGY ESP SYSTEMS, LLC; APERGY BMCS ACQUISITION CORP; HARBISON-FISCHER, INC.; NORRIS RODS, INC.,; NORRIS RODS, INC.,; NORRISEAL-WELLMARK, INC.; PCS FERGUSON, INC.; QUARTZDYNE, INC.; US SYNTHETIC CORPORATION
Reel/Frame 072004/0019 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 12, 2025
From: KIDD, JULIE ANN; SCHAEFER, HEATHER MARIE; XU, CHENGKUN; WIGGINS, JASON K.; BROWN, MATTHEW; FRISBY, CODY
To: US SYNTHETIC CORPORATION
Reel/Frame 070487/0302 →
RELEASE OF SECURITY INTEREST Recorded Jun 7, 2022
From: BANK OF AMERICA, N.A.
To: ACE DOWNHOLE, LLC; HARBISON-FISCHER, INC.; NORRIS RODS, INC.; PCS FERGUSON, INC.; QUARTZDYNE, INC.; SPIRIT GLOBAL ENERGY SOLUTIONS, INC.; THETA OILFIELD SERVICES, INC.; APERGY BMCS ACQUISITION CORP.; NORRISEAL-WELLMARK, INC.; US SYNTHETIC CORPORATION; WINDROCK, INC.
Reel/Frame 060305/0001 →
SECURITY INTEREST Recorded Jun 5, 2020
From: ACE DOWNHOLE, LLC; APERGY BMCS ACQUISITION CORP.; HARBISON-FISCHER, INC.; NORRIS RODS, INC.; NORRISEAL-WELLMARK, INC.; PCS FERGUSON, INC.; QUARTZDYNE, INC.; SPIRIT GLOBAL ENERGY SOLUTIONS, INC.; THETA OILFIELD SERVICES, INC.; US SYNTHETIC CORPORATION; WINDROCK, INC.
To: BANK OF AMERICA, N.A.
Reel/Frame 053790/0001 →
SECURITY AGREEMENT Recorded May 9, 2018
From: APERGY (DELAWARE) FORMATION, INC.; APERGY BMCS ACQUISITION CORP.; APERGY ENERGY AUTOMATION, LLC; HARBISON-FISCHER, INC.; NORRISEAL-WELLMARK, INC.; PCS FERGUSON, INC.; QUARTZDYNE, INC.; SPIRIT GLOBAL ENERGY SOLUTIONS, INC.; US SYNTHETIC CORPORATION; WINDROCK, INC.
To: JPMORGAN CHASE BANK, N.A.
Reel/Frame 046117/0015 →