Methods of at least partially removing at least one interstitial constituent from a polycrystalline diamond body using a removing agent including a supercritical fluid component

Patent metadata

Field	Value
Publication number	US-9597775-B2
Application number	US-201414520188-A
Country	US
Kind code	B2
Filing date	Oct 21, 2014
Priority date	Oct 30, 2013
Publication date	Mar 21, 2017
Grant date	Mar 21, 2017

Abstract

Embodiments relate to methods of fabricating polycrystalline diamond compacts (“PDCs”) in which a removing agent includes at least one supercritical fluid component that is used to remove at least one interstitial constituent from at least a portion of a polycrystalline diamond (“PCD”) body and applications for such PDCs. Removing the at least one interstitial constituent using the removing agent including the at least one supercritical fluid component may provide more rapid and effective removal of the at least one interstitial constituent from a PCD body than conventional acid leaching. In an embodiment, a method of fabricating at least partially porous PCD body includes providing a PCD body in which at least one interstitial constituent is disposed throughout, and removing at least a portion of the at least one interstitial constituent from the PCD body with a removing agent including at least one supercritical fluid component.

First claim

What is claimed is:

1. A method of fabricating an at least partially porous polycrystalline diamond body, the method comprising:
providing a polycrystalline diamond body including a plurality of bonded diamond grains defining a plurality of interstitial regions having at least one interstitial constituent disposed therein; and
at least partially removing the at least one interstitial constituent from the polycrystalline diamond body with a removing agent to form an at least partially porous polycrystalline diamond body, wherein the removing agent includes at least one supercritical fluid component.

2. The method of claim 1 , further comprising bonding the at least partially porous polycrystalline diamond body to a substrate to form a polycrystalline diamond compact.

3. The method of claim 1 wherein the at least one supercritical fluid includes at least one member selected from the group consisting of carbon dioxide, water, methane, ethane, propane, ethylene, propylene, methanol, ethanol, acetone, pentane, butane, hexamine, heptane, sulfur hexafluoride, xenon dichlorodifluoromethane, trifluoromethane, isopropanol, nitrous oxide, ammonia, methylamine, and diethyl ether.

4. The method of claim 1 wherein the removing agent is substantially free of an aqueous component.

5. The method of claim 1 wherein the removing agent includes a leaching agent that includes an aqueous component.

6. The method of claim 5 wherein the aqueous component includes hydrofluoric acid, nitric acid, hydrochloric acid, aqua regia, or combinations thereof.

7. The method of claim 5 wherein the leaching agent includes at least one chelating agent.

8. The method of claim 7 wherein the at least one chelating agent includes at least one member selected from the group consisting of an amphiphilic surfactant, an organic solvent, a dithiocarbamate, 2-ethyl hexyl 2-ethyl hexyl phosphonic acid, a 2-ethyl sodium bis-(2-ethyl hexyl)sulfosuccinate, crown ethers, β-diketones, fluorinated deketones; a fluorinated sodium bis-(2-ethyl hexyl)sulfosuccinate a 2,2′-bipyridine and its derivatives (e.g., 4,4′-dimehtyl-2,2′-bipyridyl), a perfluoropolyether phosphate, perfluro-1-octane-sulfonic acid tetraethylammonium salt, and a fluorinated surfactant including a fluorocarbon tail.

9. The method of claim 7 wherein the at least one chelating agent acts as a surfactant that aids in the formation of a microemulsion supercritical fluid.

10. The method of claim 7 , further comprising stirring the leaching agent so that the at least one supercritical component and the at least one chelating agent form an emulsion.

11. The method of claim 10 wherein stirring the leaching agent so that the at least one supercritical component and the at least one chelating agent form an emulsion includes stirring the leaching agent for a period of less than about 1.5 hours.

12. The method of claim 10 wherein the emulsion is substantially homogeneously dispersed.

13. The method of claim 1 wherein at least partially removing the at least one interstitial constituent from the polycrystalline diamond body with the removing agent includes:
placing the polycrystalline diamond body in an extraction apparatus; and
heating and pressurizing the extraction apparatus containing the polycrystalline diamond body and the removing agent sufficiently to at least partially remove the interstitial constituent from the polycrystalline diamond body.

14. The method of claim 13 wherein the extraction apparatus is heated to a temperature of less than about 400° C.

15. The method of claim 13 wherein the extraction apparatus is pressurized to a pressure of less than about 3500 psi.

16. The method of claim 13 wherein the extraction apparatus is a closed system or an open system.

17. The method of claim 1 wherein the interstitial constituent is includes at least one of a catalyst or a metallic infiltrant.

18. A method of forming a polycrystalline diamond compact, the method comprising:
forming a polycrystalline diamond body having a catalyst dispersed therethrough;
positioning the polycrystalline diamond body in an extraction apparatus;
flowing a leaching agent into the extraction apparatus, wherein the leaching agent includes a supercritical fluid component, an aqueous component, and at least one chelating agent;
stirring the leaching agent in the extraction apparatus to form an emulsion;
at least partially leaching the polycrystalline diamond body with the emulsion to at least partially remove the metal-solvent catalyst from the polycrystalline diamond body;
infiltrating the at least partially leached polycrystalline diamond body with a metallic infiltrant under conditions effective to bond the infiltrated polycrystalline diamond body to the substrate to form the polycrystalline diamond compact; and
removing at least a portion of the metallic infiltrant from the infiltrated polycrystalline diamond body of the polycrystalline diamond compact by flowing additional leaching agent across a working surface of the infiltrated polycrystalline diamond body, wherein the additional leaching agent includes a supercritical fluid component and an aqueous component.

19. The method of claim 18 wherein the supercritical fluid component of the leaching agent and the additional leaching agent includes at least one member selected from the group consisting of carbon dioxide, supercritical carbon dioxide, water, methane, ethane, propane, ethylene, propylene, methanol, ethanol, acetone, pentane, butane, hexamine, heptane, sulfur hexafluoride, xenon dichlorodifluoromethane, trifluoromethane, isopropanol, nitrous oxide, ammonia, methylamine, and diethyl ether.

20. The method of claim 18 wherein the aqueous component of the leaching agent and the additional leaching agent includes hydrofluoric acid, nitric acid, hydrochloric acid, aqua regia, or combinations thereof and the at least one chelating agent includes at least one member selected from the group consisting of an amphiphilic surfactant, an organic solvent, a dithiocarbamate, 2-ethyl hexyl 2-ethyl hexyl phosphonic acid, a 2-ethyl sodium bis-(2-ethyl hexyl)sulfosuccinate, crown ethers, β-diketones, fluorinated deketones; a fluorinated sodium bis-(2-ethyl hexyl)sulfosuccinate a 2,2′-bipyridine and its derivatives (e.g., 4,4′-dimehtyl-2,2′-bipyridyl), a perfluoropolyether phosphate, perfluro-1-octane-sulfonic acid tetraethylammonium salt, and a fluorinated surfactant including a fluorocarbon tail.

21. The method of claim 18 wherein stirring the leaching agent of the leaching agent and the additional leaching agent in the extraction apparatus to form an emulsion includes stirring the leaching agent for a time of less than about 1.5 hours.

22. The method of claim 17 wherein removing at least a portion of the metallic infiltrant from the infiltrated polycrystalline diamond body of the polycrystalline diamond compact by flowing additional leaching agent across a working surface of the infiltrated polycrystalline diamond body includes leaching a portion of the metallic infiltrant present in the infiltrated polycrystalline diamond body to a selected leach depth of about 50 μm to about 800 μm.

23. A method of fabricating a polycrystalline diamond compact, the method comprising:
providing a polycrystalline diamond body including a plurality of bonded diamond grains defining a plurality of interstitial regions having at least one interstitial constituent disposed therein;
at least partially removing the at least one int

Assignees

• Us Synthetic Corp

Inventors

• Vail Michael A

Classifications

• B22F2998/10

  Processes characterised by the sequence of their steps · CPC title

• B24D3/10 Primary

  for porous or cellular structure, e.g. for use with diamonds as abrasives · CPC title

• E21B10/567

  with preformed cutting elements mounted on a distinct support, e.g. polycrystalline inserts · CPC title