Source: https://patents.google.com/patent/US10132121B2/en
Timestamp: 2019-05-23 21:40:46
Document Index: 629921924

Matched Legal Cases: ['Application No. 0802233', 'Application No. 1210470', 'application No. 08', 'Application No. 2619547', 'Application No. 0708915', 'Application No. 0820881', 'Application No. 0820881', 'Application No. 0820881', 'Application No. 1101214', 'Application No. 1206076', 'Application No. 08101339', 'Application No. 200980127904', 'Application No. 200980127904', 'Application No. 200980127904', 'Application No. 200980127904', 'Application No. 201080036092', 'Application No. 0708915', 'Application No. 0805168', 'Application No. 0820881', 'Application No. 2619526']

US10132121B2 - Polycrystalline diamond constructions having improved thermal stability - Google Patents
Polycrystalline diamond constructions having improved thermal stability Download PDF
US10132121B2
US10132121B2 US13/085,089 US201113085089A US10132121B2 US 10132121 B2 US10132121 B2 US 10132121B2 US 201113085089 A US201113085089 A US 201113085089A US 10132121 B2 US10132121 B2 US 10132121B2
US13/085,089
US20110247278A1 (en
Peter Thomas Cariveau
2007-03-21 Priority to US11/689,434 priority Critical patent/US7942219B2/en
2011-04-12 Application filed by Smith International Inc filed Critical Smith International Inc
2011-04-12 Priority to US13/085,089 priority patent/US10132121B2/en
2011-06-27 Assigned to SMITH INTERNATIONAL, INC. reassignment SMITH INTERNATIONAL, INC. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: GRIFFO, ANTHONY, CARIVEAU, PETER THOMAS, KESHAAVAN, MADAPUSI K., EYRE, RONALD K.
2011-08-22 Assigned to SMITH INTERNATIONAL, INC. reassignment SMITH INTERNATIONAL, INC. CORRECTIVE ASSIGNMENT TOCORRECT THE TYPOGRAPHICAL ERROR IN THE FIRST APPLICANT'S NAME PREVIOUSLY RECORDED AT REEL 026507, FRAME 0303. Assignors: GRIFFO, ANTHONY, CARIVEAU, PETER THOMAS, KESHAVAN, MADAPUSI K., EYRE, RONALD K.
2011-10-13 Publication of US20110247278A1 publication Critical patent/US20110247278A1/en
2018-11-20 Publication of US10132121B2 publication Critical patent/US10132121B2/en
A method for making a polycrystalline diamond construction is disclosed, which includes the steps of treating a polycrystalline diamond body having a plurality of bonded together diamond crystals and a solvent catalyst material to remove the solvent catalyst material therefrom, wherein the solvent catalyst material is disposed within interstitial regions between the bonded together diamond crystals, replacing the removed solvent catalyst material with a replacement material, and treating the body having the replacement material to remove substantially all of the replacement material from a first region of the body extending a depth from a body surface, and allowing the remaining amount of the replacement material to reside in a second region of the body that is remote from the surface.
This patent application is a divisional patent application of U.S. patent application Ser. No. 11/689,434, filed on Mar. 21, 2007.
This invention relates to polycrystalline diamond constructions, and methods for forming the same, that are specially engineered having differently composed regions for the purpose of providing improved thermal characteristics when used, e.g., as a cutting element or the like, during cutting and/or wear applications when compared to conventional polycrystalline diamond constructions comprising a solvent catalyst material.
Polycrystalline diamond construction (PCD) of this invention comprise a plurality of bonded together diamond crystals forming a polycrystalline diamond body. The body includes a surface and has material microstructure comprising a first region positioned remote from the surface and that includes a replacement material. In an example embodiment, the replacement material is a noncatalyzing material that is disposed within interstitial regions between the diamond crystals in the first region. The noncatalyzing material can have a melting temperature of less than about 1,200° C., and can be selected from metallic materials and/or alloys including elements, which can include those from Group IB of the Periodic table, such as copper.
Polycrystalline diamond (PCD) constructions of this invention have a material microstructure comprising a polycrystalline matrix first phase that is formed from bonded together diamond grains or crystals. The diamond body further includes interstitial regions disposed between the diamond crystals, wherein in one region of the body the interstitial regions are filled with a replacement or noncatalyzing material, and wherein in another region of the body the interstitial regions are substantially free of the replacement or noncatalyzing material. The PCD construction can additionally comprise a substrate that is attached to the PCD body, thereby forming a compact. Such PCD constructions and compacts configured in this matter are specially engineered to provide improved thermal characteristics such as thermal stability when exposed to cutting and wear applications when compared to conventional PCD constructions, i.e., those that are formed from and that include solvent metal catalyst materials. PCD compacts of this invention, comprising a substrate attached thereto, facilitate attachment of the construction to a desired tooling, cutting, machining, and/or wear device, e.g., a drill bit used for drilling subterranean formations.
As used herein, the term “PCD” is used to refer to polycrystalline diamond that has been formed at high pressure/high temperature (HPHT) conditions and that has a material microstructure comprising a matrix phase of bonded together diamond crystals. PCD is also understood to include a plurality of interstitial regions that are disposed between the diamond crystals. PCD useful for making PCD constructions of this invention can be formed by conventional method of subjecting precursor diamond grains or powder to HPHT sintering conditions in the presence of a solvent catalyst material that functions to facilitate the bonding together of the diamond grains at temperatures of between about 1,350 to 1,500° C. and pressures of 5,000 Mpa or higher. Suitable solvent catalyst materials useful for making PCD include those metals identified in Group VIII of the Periodic table.
As used herein, the term “thermal characteristics” is understood to refer to the thermal stability of the resulting PCD construction, which can depend on such factors as the relative thermal compatibilities, such as thermal expansion properties, of the materials occupying the different construction material phases.
A feature of PCD constructions of this invention is that they comprise a diamond body that retains the matrix phase of bonded together diamond crystals, but the body has been modified so that it no longer includes the solvent metal catalyst material that was used to facilitate the diamond bonding forming the matrix phase. Rather, the body has been specially treated so that the interstitial regions that previously included the solvent catalyst material are configured into one phase that includes a replacement or noncatalyzing material and another phase that does not include the replacement or noncatalyzing material. As used herein, the term “noncatalyzing material” is understood to refer to materials that are not identified in Group VIII of the Periodic table, and that do not promote the change or interaction of the diamond crystals within the diamond body at temperatures below about 2,000° C.
FIGS. 2A, 2B, and 2C each schematically illustrate an example embodiment PCD construction 30 of this invention at different stages of formation. FIG. 2A illustrates a first stage of formation, starting with a conventional PCD body 32 in its initial form after sintering by conventional HPHT sintering process. At this early stage, the PCD body 32 comprises a polycrystalline diamond matrix first phase and a solvent catalyst metal material, such as cobalt, disposed within the interstitial regions between the bonded together diamond crystals forming the matrix. The solvent catalyst metal material can be added to the precursor diamond grains or powder as a raw material powder prior to sintering, it can be contained within the diamond grains or powder, or it can be infiltrated into the diamond grains or powder during the sintering process from a substrate containing the solvent metal catalyst material and that is placed adjacent the diamond powder and exposed to the HPHT sintering conditions. In an example embodiment, the solvent metal catalyst material is provided as an infiltrant from a substrate 34, e.g., a WC—Co substrate, during the HPHT sintering process.
The diamond powder or green-state part is loaded into a desired container for placement within a suitable HPHT consolidation and sintering device. In an example embodiment, where the source of the solvent metal catalyst material is provided by infiltration from a substrate, a suitable substrate material is disposed within the consolidation and sintering device adjacent the diamond powder mixture. In a preferred embodiment, the substrate is provided in a preformed state. Substrates useful for forming the PCD body can be selected from the same general types of materials conventionally used to form substrates for conventional PCD materials, including carbides, nitrides, carbonitrides, ceramic materials, metallic materials, cermet materials, and mixtures thereof. A feature of the substrate used for forming the PCD body is that it include a solvent metal catalyst capable of melting and infiltrating into the adjacent volume of diamond powder to facilitate conventional diamond-to-diamond intercrystalline bonding forming the PCD body. A preferred substrate material is cemented tungsten carbide (WC—Co).
Where the solvent metal catalyst is provided by infiltration from a substrate, the container including the diamond power and the substrate is loaded into the HPHT device and the device is then activated to subject the container to a desired HPHT condition to effect consolidation and sintering of the diamond powder. In an example embodiment, the device is controlled so that the container is subjected to a HPHT process having a pressure of 5,000 Mpa or more and a temperature of from about 1,350° C. to 1,500° C. for a predetermined period of time. At this pressure and temperature, the solvent metal catalyst melts and infiltrates into the diamond powder, thereby sintering the diamond grains to form conventional PCD.
As used herein, the term “removed” is used to refer to the reduced presence of the solvent metal catalyst material in the PCD body, and is understood to mean that a substantial portion of the solvent metal catalyst material no longer resides within the PCD body. However, it is to be understood that some small trace amounts of the solvent metal catalyst material may still remain in the microstructure of the PCD body within the interstitial regions and/or adhered to the surface of the diamond crystals. Additionally, the term “substantially free”, as used herein to refer to the remaining PCD body after the solvent metal catalyst material has been removed, is understood to mean that there may still be some trace small amounts of the solvent metal catalyst remaining within the PCD body as noted above.
FIG. 2C schematically illustrates an example embodiment PCD construction 30 prepared according to principles of this invention after a third stage of formation. Specifically, at a stage where the solvent metal catalyst material removed from the PCD body has now been replaced with a replacement material. In the example embodiment noted above, the replacement material is preferably one that: (1) is relatively inert (in that it does not act as a catalyst relative to the polycrystalline matrix first phase at temperatures below about 2,000° C.); and/or (2) enhances one or more mechanical property of the existing PCD body; and/or (3) optionally facilitates attachment of the PCD body to a substrate, thereby forming a compact.
The term “filled”, as used herein to refer to the presence of the replacement material in the voids or pores of the PCD body presented by the removal of the solvent metal catalyst material, is understood to mean that a substantial volume of such voids or pores contain the replacement material. However, it is to be understood that there may also be a volume of voids or pores within the same region of the PCD body that do not contain the replacement material, and that the extent to which the replacement material effectively displaces the empty voids or pores will depend on such factors as the particular microstructure of the PCD body, the effectiveness of the process used for introducing the replacement material, and the desired mechanical and/or thermal properties of the resulting PCD construction.
In addition to the properties noted above, it is also desired that the replacement material have a melting temperature that is lower than that of the remaining polycrystalline matrix first phase. In an example embodiment, it is desired that the replacement material have a melting/infiltration temperature that is less than about 1,200° C. A desired feature of the replacement material is that it enhances the strength of the matrix first phase. Another desired feature of the replacement material is that it display little shrinkage after being disposed within the matrix to prevent the formation of unfavorable resultant matrix stresses, while still maintaining the desired mechanical and materials properties of the matrix. It is to be understood that the replacement material selected may have one or more of the above-noted features.
In an example embodiment, wherein the PCD body is treated to remove the solvent metal catalyst material, Co, therefrom, the resulting PCD body was again subjected to HPHT processing for a period of approximately 100 seconds at a temperature below that of the melting temperature of the replacement material, which was copper. The source of the copper replacement material was a WC—Cu substrate that was positioned adjacent a desired surface portion of the PCD body prior to HPHT processing. The HPHT process was controlled to bring the contents to the melting temperature of copper (less than about 1,200° C., at a pressure of about 3,400 to 7,000 Mpa) to infiltrate into and fill the pores or voids in the PCD body. During the HPHT process, the substrate containing the copper material was attached to the PCD body to thereby form a PCD compact.
In an example embodiment, the substrate used to form the PCD compact is formed from a cermet material that is substantially free of any Group VIII solvent metal catalyst materials. In a preferred embodiment, when the substrate is used as the source of the replacement material, the substrate is formed from a cermet, such as a WC, further comprising a binder material that is the replacement material used to fill the PCD body. Suitable binder materials include Group IB metals of the Periodic table or alloys thereof. Preferred Group IB metals and/or alloys thereof include Cu, Ag, Au, Cu—W, Cu—Ti, Cu—Nb, or the like.
It is preferred that the substrate binder material have a melting temperature that is less than about 1,200° C. This melting temperature criteria is designed to ensure that the binder material in the substrate can be melted and infiltrated into the PCD body during the HPHT process under conditions that will not cause any catalyzing material that may be present in the substrate to melt and possibly enter the PCD body. Thereby, ensuring that the PCD body remain completely free any solvent catalyzing material.
In a preferred embodiment, substrates useful for forming PCD compacts of this invention and providing a source of replacement material comprise WC—Cu or WC—Cu alloy. In such embodiment, the carbide particles used to form the substrate are coated with metals such as Ti, W and others that facilitate wetting of the coated particle by the noncatalyzing material. The carbide particles can be coated using conventional techniques to provide a desired coating thickness that is desired to both provide the necessary wetting characteristic to form the substrate, and to also contribute the desired mechanical properties to the substrate for its intended use as a cutting and/or wear element. In an example embodiment, the grain size of the WC particles in the substrate are in the range of from about 0.5 to 3 micrometers. In such example embodiment, the substrate comprises in the range of from about 10 to 20 percent by volume of the noncatalyzing material, based on the total volume of the substrate.
If desired, the substrate can comprise two or more different regions that are each formed from a different material. For example, the substrate can comprise a first region that is positioned adjacent a surface of the substrate positioned to interface and attached with the PCD body, and a second region that extends below the first region. An interface 48 within the substrate 44 between any two such regions is illustrated in phantom in FIG. 2H. A substrate having this construction can be used, for example, to provide a source of the replacement material to the PCD body, attach the substrate to the PCD body during HPHT processing, and to introduce any mechanical properties to the substrate that may facilitate its attachment to the end-use cutting or wear device. For example, such a substrate construction may comprise a first region formed from WC—Cu or a WC—Cu alloy that is positioned along an interfacing surface with the PCD body, and a second region formed from WC—Co positioned remote from the interfacing surface. Here, the Co in the substrate second region would not melt and not infiltrate into the PCD body so long as the process used to infiltrate the Cu replacement material into the PCD body was conducted at a temperature below about 1,200° C., i.e., below the melting temperature of the Co in the substrate second region.
Substrates useful for attaching to the PCD body already filled with the replacement material include those typically used for forming conventional PCD compacts, such as those described above like ceramic materials, metallic materials, cermet materials, or the like. In an example embodiment, the substrate can be formed from a cermet material such as WC—Co. In the event that the substrate includes a binder material that is a Group VIII element, then it may be desired to use an intermediate material between the substrate and the PCD body.
The intermediate material can be formed from those materials that are capable of forming a suitable attachment bond between both the PCD body and the substrate. In the event that the substrate material includes a binder material that is a Group VIII element, it is additionally desired that the intermediate material operate as a barrier to prevent or minimize the migration of the substrate binder material into the PCD body during the attachment process. Suitable intermediate materials include those described above as being useful as the replacement material, e.g., can be a noncatalyzing material, and/or can have a melting temperature that is below the melting temperature of any binder material in the substrate. Suitable intermediate materials can be cermet materials comprising a noncatalyzing material such as WC—Cu, WC—Cu alloy, or the like.
1. A method for making a polycrystalline diamond construction comprising the steps of:
treating a polycrystalline diamond body comprising a plurality of bonded together diamond crystals and a solvent catalyst material to remove substantially all of the solvent catalyst material therefrom, wherein the solvent catalyst material is disposed within interstitial regions between the bonded together diamond crystals;
replacing substantially all of the removed solvent catalyst material with a replacement material not initially used to form the diamond body, wherein the replacement material fills the interstitial regions; and
treating the body comprising the replacement material to remove substantially all of the replacement material from a first region of the body extending a depth from a body surface, wherein the depth is greater than about 0.05 mm from the surface, and allowing the remaining amount of the replacement material to reside in a second region of the body that is remote from the surface.
2. The method as recited in claim 1 wherein during the step of replacing, the replacement material that is used has a melting temperature of less than about 1,200° C.
3. The method as recited in claim 1 wherein during the step of replacing, the replacement material that is used is selected from Group IB of the Periodic table.
4. The method as recited in claim 1 further comprising the step of attaching a substrate to the body.
5. The method as recited in claim 4 wherein the step of attaching takes place during the step of replacing, and wherein the substrate includes a binder material that is formed from the replacement material, and wherein the substrate is a cermet material.
6. The method as recited in claim 4 wherein the step of attaching takes place after the step of replacing.
7. The method as recited in claim 6 wherein the step of attaching takes place before the step of treating.
8. A method for making a polycrystalline diamond construction comprising the steps of:
treating a polycrystalline diamond body comprising a plurality of bonded together diamond crystals and a solvent catalyst disposed within interstitial regions to remove substantially all of the solvent catalyst material therefrom;
attaching the polycrystalline diamond body to a substrate, wherein during the step of attaching, a constituent of the substrate infiltrates into the polycrystalline diamond body to fill the interstitial regions, wherein the constituent of the substrate is a non-catalyst material not initially used to form the diamond body; and
leaching the polycrystalline diamond body to remove a portion of the infiltrated constituent from a region depth extending from a working surface of the body, wherein the infiltrated constituent remains in another region of the body.
9. The method as recited in claim 8 wherein during the step of treating, the polycrystalline diamond body is rendered substantially free of the solvent catalyst material.
10. The method as recited in claim 8 wherein during the step of leaching, the partial depth of the polycrystalline diamond body is rendered substantially free of the constituent.
11. The method as recited in claim 8 wherein the step of attaching is conducted at high pressure/high temperature conditions.
12. The method as recited in claim 8 wherein during the leaching step rendering interstitial regions within the partial depth of the diamond body substantially empty.
13. A method for making a polycrystalline diamond construction comprising the steps of:
treating a polycrystalline diamond body comprising a plurality of bonded together diamond crystals and a solvent catalyst material to remove substantially all of the solvent catalyst material therefrom to form a thermally stable diamond body, wherein the solvent catalyst material is disposed within interstitial regions between the bonded together diamond crystals;
infiltrating a replacement material through the entire polycrystalline diamond body to fill the interstitial regions, wherein the replacement material is inert up to about 2000° C. and is a material not initially used to form the diamond body; and
attaching the thermally stable diamond body to a substrate,
wherein after attachment to the substrate, the thermally stable diamond body comprises a first region adjacent the substrate having the interstitial regions filled with the replacement material, and a second region remote from the substrate being substantially free of the replacement material.
14. The method of claim 13, wherein the replacement material infiltrates the entire polycrystalline diamond body, and wherein the method further comprises:
removing the replacement material from a portion of the interstitial regions to form the second region remote from the substrate.
US13/085,089 2007-03-21 2011-04-12 Polycrystalline diamond constructions having improved thermal stability Active US10132121B2 (en)
US11/689,434 US7942219B2 (en) 2007-03-21 2007-03-21 Polycrystalline diamond constructions having improved thermal stability
US13/085,089 US10132121B2 (en) 2007-03-21 2011-04-12 Polycrystalline diamond constructions having improved thermal stability
US11/689,434 Division US7942219B2 (en) 2007-03-21 2007-03-21 Polycrystalline diamond constructions having improved thermal stability
US20110247278A1 US20110247278A1 (en) 2011-10-13
US10132121B2 true US10132121B2 (en) 2018-11-20
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US11/689,434 Active 2027-10-04 US7942219B2 (en) 2007-03-21 2007-03-21 Polycrystalline diamond constructions having improved thermal stability
US13/085,089 Active US10132121B2 (en) 2007-03-21 2011-04-12 Polycrystalline diamond constructions having improved thermal stability
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Free format text: CORRECTIVE ASSIGNMENT TOCORRECT THE TYPOGRAPHICAL ERROR IN THE FIRST APPLICANT S NAME PREVIOUSLY RECORDED AT REEL 026507, FRAME 0303;ASSIGNORS:KESHAVAN, MADAPUSI K.;EYRE, RONALD K.;GRIFFO, ANTHONY;AND OTHERS;SIGNING DATES FROM 20110414 TO 20110610;REEL/FRAME:026811/0860