# US 10,309,158 B2 · Method of partially infiltrating an at least partially leached polycrystalline diamond table and resultant polycrystalline diamond compacts > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 10,309,158 B2 - Document ID: US10309158B2 - Status: Granted - Kind: B2 - Application number: 12/961,787 - Filed: 2010-12-07 - Published: 2012-06-07 - Granted: 2019-06-04 - Earliest claimed: 2010-12-07 - Assignees: US Synthetic Corporation - Applicants: Debkumar Mukhopadhyay; Kenneth E. Bertagnolli; Jair J. Gonzalez - Inventors: Debkumar Mukhopadhyay; Kenneth E. Bertagnolli; Jair J. Gonzalez - Web page: https://patentgrep.com/patent/US10309158B2 ## CPC - C23F 1/28: for etching iron group metals - E21B 10/5735: {Interface between the substrate and the cutting element} - B22F 7/06: of composite workpieces or articles from parts, e.g. to form tipped tools {(B22F7/002 takes precedence)} - B24D 3/10: for porous or cellular structure, e.g. for use with diamonds as abrasives - C22C 26/00: Alloys containing diamond {or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes} - C23F 1/02: Local etching - E21B 10/55: with preformed cutting elements - E21B 10/567: with preformed cutting elements mounted on a distinct support, e.g. polycrystalline inserts - B22F 2005/001: {Cutting tools, earth boring or grinding tool other than table ware} - Y10T 428/24777: Edge feature - C23F: NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE (working metal by laser beams B23K26/00; desurfacing by applying flames B23K7/00; working of metal by electro-erosion B23H; producing decorative effects by removing surface material, e.g. by engraving, by etching, B44C1/22; electrolytic etching or polishing C25F); INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25 - E21B: EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS - B22F: WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER (making alloys by powder metallurgy C22C); APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER - B24D: TOOLS FOR GRINDING, BUFFING OR SHARPENING (abrading-bodies specially designed for tumbling apparatus, e.g. abrading-balls B24B31/14; honing tools B24B33/08; lapping tools B24B37/11) - C22C: ALLOYS (treatment of alloys C21D, C22F) - Y10T: TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION ## Abstract In an embodiment, a method of fabricating a polycrystalline diamond compact (“PDC”) includes forming a polycrystalline diamond (“PCD”) table in the presence of a metal-solvent catalyst in a first high-pressure/high-temperature (“HPHT”) process. The PCD table includes bonded diamond grains defining interstitial regions, with the metal-solvent catalyst disposed therein. The method includes at least partially leaching the PCD table to remove at least a portion of the metal-solvent catalyst therefrom. The method includes subjecting the at least partially leached PCD table and a substrate to a second HPHT process under diamond-stable temperature-pressure conditions to partially infiltrate the at least partially leached PCD table with an infiltrant. A maximum temperature (T), a total process time (t), and a maximum pressure (P) of the second HPHT process are chosen so that β is about 2° Celsius·hours/gigapascals (“° C.·h/GPa”) to about 325° C.·h/GPa, with β represented as β=T·t/P. ## Claims ### Claim 1 A method of fabricating a polycrystalline diamond compact, comprising: forming a polycrystalline diamond table in the presence of a metal-solvent catalyst including one of cobalt, iron, nickel, or alloys thereof in a first high-pressure/high-temperature process, the polycrystalline diamond table including a plurality of bonded diamond grains defining a plurality of interstitial regions, at least a portion of the plurality of interstitial regions including the metal-solvent catalyst disposed therein, the plurality of bonded diamond grains exhibiting an average grain size of about 40 μm or less; at least partially leaching the polycrystalline diamond table to remove at least a portion of the metal-solvent catalyst therefrom; subjecting the at least partially leached polycrystalline diamond table and a substrate to a second high-pressure/high-temperature process under diamond-stable temperature-pressure conditions to partially infiltrate the at least partially leached polycrystalline table with an infiltrant including one of iron, nickel, cobalt, or alloys of the foregoing metals and attach the partially infiltrated polycrystalline diamond table to the substrate; wherein a maximum temperature (T), a total process time (t), and a maximum internal cell pressure (P) of the second high-pressure/high-temperature process are chosen so that β is greater than 75° Celsius·hours/gigapascals (“° C.·h/GPa”) to about 325° C.·h/GPa, with β represented as β=T·t/P; wherein P in the second high-pressure/high-temperature process is greater than a maximum internal cell pressure of the first high-pressure/high-temperature process; and wherein the infiltrated polycrystalline diamond table includes a first region adjacent to the substrate including the infiltrant disposed in at least a portion of the interstitial regions thereof and a second region extending inwardly from an exterior working surface to a selected depth of at least about 700 μm, the second region being substantially free of the infiltrant without having been leached of the infiltrant. ### Claim 2 (depends on 1) The method of claim 1 wherein P is about 6 GPa to about 10 GPa, T is about 1250° C. to about 3250° C., and t is about 60 seconds to about 1 hour. ### Claim 3 (depends on 1) The method of claim 1 wherein P is about 6 GPa to about 8 GPa, T is about 1250° C. to about 1500° C., and t is about 200 seconds to about 450 seconds. ### Claim 4 (depends on 1) The method of claim 1 wherein β is about 75° C.·h/GPa to about 100° C.·h/GPa. ### Claim 5 (depends on 1) The method of claim 1 wherein β is about 75° C.·h/GPa to about 150° C.·h/GPa. ### Claim 6 (depends on 1) The method of claim 1 wherein p is about 100° C.·h/GPa to about 200° C.·h/GPa. ### Claim 7 (depends on 1) The method of claim 1 wherein the selected depth is about 750 μm to about 2100 μm. ### Claim 8 (depends on 1) The method of claim 1 wherein the selected depth is about 1000 μm to about 2000 μm. ### Claim 9 (depends on 1) The method of claim 1 wherein the infiltrated polycrystalline diamond table comprises a nonplanar interface between the first region and the second region. ### Claim 10 (depends on 1) The method of claim 1 wherein at least one of T or t of the first high-pressure/high-temperature conditions are different from a maximum temperature or total process time of the second high-pressure/high-temperature conditions. ### Claim 11 (depends on 1) The method of claim 1 wherein the infiltrant is provided from the substrate. ### Claim 12 (depends on 1) The method as recited in claim 1 wherein the second region of the infiltrated polycrystalline diamond table is essentially free of silicon, nickel, or combinations thereof. ### Claim 13 (depends on 1) The method of claim 1, further comprising: positioning the plurality of diamond particles adjacent to a first substrate; wherein the first high-pressure/high-temperature process comprises subjecting the plurality of diamond particles and the first substrate to the first high-pressure/high-temperature process to sinter the plurality of diamond particles and form a polycrystalline diamond table on the first substrate; and further comprising separating the polycrystalline diamond table from the first substrate. ### Claim 14 (depends on 1) The method of claim 1 wherein a thickness of the infiltrated polycrystalline diamond table is about 0.065 inch to about 0.080 inch. ### Claim 15 (depends on 1) The method of claim 1 wherein the average grain size of the polycrystalline diamond table is about 30 μm or less. ### Claim 16 (depends on 1) The method of claim 1 wherein a thickness of the infiltrated polycrystalline diamond table is about 0.065 inch to about 0.080 inch, and the average grain size of the polycrystalline diamond table is about 30 μm or less. ### Claim 17 (depends on 1) The method of claim 1, further comprising attaching the substrate having the infiltrated polycrystalline diamond table attached thereto to a bit body of a rotary drill bit. ### Claim 18 A method of fabricating a rotary drill bit, comprising: attaching at least one polycrystalline diamond compact to a bit body of the rotary drill bit by a method including: forming a polycrystalline diamond table in the presence of a metal-solvent catalyst including one of cobalt, iron, nickel, or alloys thereof in a first high-pressure/high-temperature process, the polycrystalline diamond table including a plurality of bonded diamond grains defining a plurality of interstitial regions, at least a portion of the plurality of interstitial regions including the metal-solvent catalyst disposed therein, the plurality of bonded diamond grains exhibiting an average grain size of about 40 μm or less; at least partially leaching the polycrystalline diamond table to remove at least a portion of the metal-solvent catalyst therefrom; subjecting the at least partially leached polycrystalline diamond table and a substrate to a second high-pressure/high-temperature process under diamond-stable temperature-pressure conditions to partially infiltrate the at least partially leached polycrystalline table with an infiltrant including at least one additional metal-solvent catalyst including one of cobalt, iron, nickel, or alloys thereof and attach the partially infiltrated polycrystalline diamond table to the substrate; wherein a maximum temperature (T), a total process time (t), and a maximum internal cell pressure (P) of the second high-pressure/high-temperature process are chosen so that β is greater than 75° Celsius·hours/gigapascals (“° C.·h/GPa”) to about 325° C.·h/GPa, with β represented as β=T·t/P; wherein P in the second high-pressure/high-temperature process is greater than a maximum internal cell pressure of the first high-pressure/high-temperature process; and wherein the infiltrated polycrystalline diamond table includes a first region adjacent to the substrate including the infiltrant disposed in at least a portion of the interstitial regions thereof and a second region extending inwardly from an exterior working surface to a selected depth of at least about 700 μm, the second region being substantially free of the infiltrant without having been leached of the infiltrant. ### Claim 19 (depends on 1) The polycrystalline diamond compact of claim 1, further comprising at least partially leaching the partially infiltrated polycrystalline diamond table attached to the substrate to remove a portion of the infiltrant material from the first region. ### Claim 20 (depends on 18) The polycrystalline diamond compact of claim 18, further comprising at least partially leaching the partially infiltrated polycrystalline diamond table attached to the substrate to remove a portion of the infiltrant material from the first region. ### Claim 21 (depends on 1) The method of claim 1, wherein the maximum internal cell pressure of the first high-pressure/high-temperature process is about 5 GPa to about 7 GPa and the P of the second high-pressure/high-temperature process is about 6.2 GPa to about 10 GPa. ### Claim 22 (depends on 1) The method of claim 1, wherein the infiltrant includes a cobalt cementing constituent from the substrate. ### Claim 23 (depends on 1) The method of claim 1, wherein the total process time t includes a time to ramp-up to a maximum temperature, a soak time at the maximum temperature, and a cool down time from the maximum temperature. ### Claim 24 (depends on 23) The method of claim 23, wherein the selected depth is at least about one third of a thickness of the infiltrated polycrystalline diamond table.