WO2015156789A1 - Polycrystalline diamond compact with enhanced thermal stability - Google Patents

Polycrystalline diamond compact with enhanced thermal stability Download PDF

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Publication number
WO2015156789A1
WO2015156789A1 PCT/US2014/033437 US2014033437W WO2015156789A1 WO 2015156789 A1 WO2015156789 A1 WO 2015156789A1 US 2014033437 W US2014033437 W US 2014033437W WO 2015156789 A1 WO2015156789 A1 WO 2015156789A1
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Prior art keywords
substrate
region
wt
diamond table
superabrasive compact
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PCT/US2014/033437
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French (fr)
Inventor
Kai Zhang
Abhijit SURYAVANSHI
Alexander Hirsch
Jessica MARSHALL
Susanne Norgren
Joel Vaughn
Hui Zhang
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Diamond Innovations, Inc.
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    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/14Anti-slip materials; Abrasives
    • C09K3/1436Composite particles, e.g. coated particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/06Processes using ultra high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
    • B01J3/062Processes using ultra high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies characterised by the composition of the materials to be processed
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24DTOOLS FOR GRINDING, BUFFING, OR SHARPENING
    • B24D3/00Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
    • B24D3/02Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent
    • B24D3/04Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially inorganic
    • B24D3/06Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially inorganic metallic or mixture of metals with ceramic materials, e.g. hard metals, "cermets", cements
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    • C22C29/02Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
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    • C22C29/067Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds comprising a particular metallic binder
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    • C22C29/06Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
    • C22C29/08Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds based on tungsten carbide
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • BPERFORMING OPERATIONS; TRANSPORTING
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    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER
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    • B22F2005/001Cutting tools, earth boring or grinding tool other than table ware
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12Both compacting and sintering
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Abstract

A superabrasive compact and a method of making the superabrasive compact are disclosed. The superabrasive compact comprises a diamond table and a substrate. The diamond table is attached to the substrate. The diamond table includes bonded diamond grains defining interstitial channels. The interstitial channels are filled with non-binder materials (42) in the first region, such as for instance SiC. The interstitial channels in the second region is filled with a binder material (46) and an additive from the substrate. The binder material is for instance Co, Fe or Ni, whereas the additive is Cr, Mn, boron or Mo. The additive lowers the melting temperature of the metallic binder to below 1350°C, thereby facilitating the infiltration of the diamond porous body.

Description

POLYCRYSTALLINE DIAMOND COMPACT WITH ENHANCED THERMAL STABILITY

TECHNICAL FIELD AND INDUSTRIAL APPLICABILITY

[0001 ] The present invention relates generally to superabrasive materials and a method of making superabrasive materials, and more particularly, to polycrystalline diamond compacts (PCD) with high temperature resistance.

SUMMARY

[0002] In one embodiment, a superabrasive compact may comprise a substrate; a diamond table attached to the substrate, wherein the diamond table has a first region and a second region, the second region is sandwiched between the first region and the substrate, wherein the diamond table includes bonded diamond grains defining interstitial channels, the interstitial channels are filled with non- binding materials in the first region, the interstitial channels in the second region are filled with a binder material and an additive from the substrate wherein the sourced material contains a binder material and an additive from the substrate, wherein the melting point of the binder material is lower than 1350 °C at an ambient pressure.

[0003] In another embodiment, a method of making a superabrasive compact may comprise steps of providing an at least partially leached polycrystalline diamond table that comprises bonded diamond grains defining interstitial channels therein; providing a composite material positioned near a surface of the at least partially leached polycrystalline diamond table; providing a substrate near the at least partially leached polycrystalline diamond table such that the at least partially leached polycrystalline diamond table is sandwiched between the composite material and the substrate; and subjecting the substrate and the at least partially leached

polycrystalline diamond table and the composite material to conditions of elevated temperature and pressure suitable for producing the polycrystalline superabrasive compact, wherein the substrate comprises a binder material and an additive in a suitable amount such that the melting point of the binder material is is less than 1350 °C.

[0004] In yet another embodiment, a superabrasive compact may comprise a substrate; a diamond table attached to the substrate, wherein the diamond table has a first region and a second region, the second region is sandwiched between the first region and the substrate, wherein the diamond table includes bonded diamond grains defining interstitial channels, the interstitial channels are filled with non-binder materials in the first region, the interstitial channels in the second region are filled with a binder material and an additive from the substrate, wherein the first region occupies from about 20% to up to about 95% volume of the diamond table, wherein the melting point of the binder material is lower than 1350 °C at an ambient pressure.

BRIEF DESCRIPTION OF THE DRAWINGS

[0005] The foregoing summary, as well as the following detailed description of the embodiments, will be better understood when read in conjunction with the appended drawings. It should be understood that the embodiments depicted are not limited to the precise arrangements and instrumentalities shown.

[0006] FIG. 1 is a schematic perspective view of a cylindrical shape thermally stable polycrystalline diamond compact produced in a high pressure high temperature (HPHT) process according to an embodiment;

[0007] FIG. 2 is an enlarged cross-sectional view of a part of diamond table on the thermally stable polycrystalline diamond compact as shown in FIG. 1 according to an embodiment; and

[0008] FIG. 3 is a flow chart illustrating a method of making reinforced thermally stable polycrystalline diamond compact. DETAILED DESCRIPTION

[0009] Before the description of the embodiment, terminology, methodology, systems, and materials are described; it is to be understood that this disclosure is not limited to the particular terminologies, methodologies, systems, and materials described, as these may vary. It is also to be understood that the terminology used in the description is for the purpose of describing the particular versions of

embodiments only, and is not intended to limit the scope of embodiments. For example, as used herein, the singular forms "a," "an," and "the" include plural references unless the context clearly dictates otherwise. In addition, the word "comprising" as used herein is intended to mean "including but not limited to." Unless defined otherwise, all technical and scientific terms used herein have the same meanings as commonly understood by one of ordinary skill in the art.

[0010] Unless otherwise indicated, all numbers expressing quantities of ingredients, properties such as size, weight, reaction conditions and so forth used in the specification and claims are to the understood as being modified in all instances by the term "about". Accordingly, unless indicated to the contrary, the numerical parameters set forth in the following specification and attached claims are approximations that may vary depending upon the desired properties sought to be obtained by the invention. At the very least, and not as an attempt to limit the application of the doctrine of equivalents to the scope of the claims, each numerical parameter should at least be construed in light of the number of reported significant digits and by applying ordinary rounding techniques.

[001 1 ] As used herein, the term "about" means plus or minus 10% of the numerical value of the number with which it is being used. Therefore, about 50% means in the range of 45%-55%. [0012] As used herein, the term "superabrasive particles" may refer to ultra-hard particles or superabrasive particles having a Knoop hardness of 3500 KHN or greater. The superabrasive particles may include diamond and cubic boron nitride, for example. The term "abrasive", as used herein, refers to any material used to wear away softer materials.

[0013] The term "particle" or "particles", as used herein, refers to a discrete body or bodies. A particle is also considered a crystal or a grain.

[0014] The term "superabrasive compact", as used herein, refers to a sintered product made using super abrasive particles, such as diamond feed or cubic boron nitride particles. The compact may include a support, such as a tungsten carbide support, or may not include a support. The "superabrasive compact" is a broad term, which may include cutting element, cutters, or polycrystalline cubic boron nitride insert.

[0015] The term "cutting element", as used herein, means and includes any element of an earth-boring tool that is used to cut or otherwise disintegrate formation material when the earth-boring tool is used to form or enlarge a bore in the formation.

[0016] The term "non-binder" material, as used herein, may refer to any material, metallic elements, non-metal, or semi-conductor materials, which do not involve or help tungsten carbide substrate chemical formation.

[0017] The term "earth-boring tool", as used herein, means and includes any tool used to remove formation material and form a bore (e.g., a wellbore) through the formation by way of removing the formation material. Earth-boring tools include, for example, rotary drill bits (e.g., fixed-compact or "drag" bits and roller cone or "rock" bits), hybrid bits including both fixed compacts and roller elements, coring bits, percussion bits, bi-center bits, reamers (including expandable reamers and fixed- wing reamers), and other so-called "hole-opening" tools. [0018] The term "feed" or "diamond feed", as used herein, refers to any type of diamond particles, or diamond powder, used as a starting material in further synthesis of PDC compacts.

[0019] The term "polycrystalline diamond", as used herein, refers to a plurality of randomly oriented or highly oriented monocrystalline diamond particles, which may represent a body or a particle consisting of a large number of smaller

monocrystalline diamond particles of any sizes. Polycrystalline diamond particles usually do not have cleavage planes.

[0020] The term "superabrasive", as used herein, refers to an abrasive possessing superior hardness and abrasion resistance. Diamond and cubic boron nitride are examples of superabrasives and have Knoop indentation hardness values of over 3500.

[0021 ] The terms "diamond particle" or "particles" or "diamond powder", which is a plurality of a large number of single crystal or polycrystalline diamond particles, are used synonymously in the instant application and have the same meaning as "particle" defined above.

[0022] Polycrystalline diamond compact (or "PCD", as used hereinafter) may represent a volume of crystalline diamond grains with embedded foreign material filling the inter-grain space. In one particular case, a compact comprises crystalline diamond grains, bound to each other by strong diamond-to-diamond bonds and form a rigid polycrystalline diamond body, and the inter-grain regions, disposed between the bounded grains and filled in one part with a catalyst material (e.g. cobalt or its alloys), which was used to promote diamond bonding during fabrication, and other part may be filled with other materials which may remain after the sintering of diamond compact. Suitable metal solvent catalysts may include the iron group transitional metal in Group VIII of the Periodic table.

[0023] "Thermally stable polycrystalline diamond" as used herein is understood to refer to intercrystalline bonded diamond that includes a volume or region that is or that has been rendered substantially free of the solvent metal catalyst or binder used to form PCD, or the solvent metal catalyst or binder used to form PCD remains in the region of the diamond body but is otherwise reacted or otherwise rendered ineffective in its ability adversely impact the bonded diamond at elevated

temperatures as discussed above.

[0024] In another particular case, a polycrystalline diamond composite compact comprises a plurality of crystalline diamond grains, which are not bound to each other, but instead are bound together by foreign bonding materials such as borides, nitrides, carbides, and others, e.g. by silicon carbide bonded diamond material.

[0025] Polycrystalline diamond compacts (or PCD compacts) may be fabricated in different ways and the examples discussed herein do not limit a variety of different types of diamond composites and PDC compacts which may be produced according to an embodiment. In one particular example, polycrystalline compacts may be formed by placing a mixture of diamond powder with a suitable solvent catalyst material (e.g. cobalt powder) on the top of WC-Co substrate, the assembly is then subjected to conditions of HPHT process, where the solvent catalyst promotes desired inter-crystalline diamond-to-diamond bonding resulted in the formation of a rigid polycrystalline diamond body and, also, provides a binding between

polycrystalline diamond body and WC-Co substrate.

[0026] In another particular example, a polycrystalline diamond compact is formed by placing diamond powder without a catalyst material on the top of substrate containing a catalyst material (e.g. WC-Co substrate). In this example, necessary cobalt catalyst material is supplied from the substrate and melted cobalt is swept through the diamond powder during the HPHT process. In still another example, a hard polycrystalline diamond composite compact is fabricated by forming a mixture of diamond powder with silicon powder and the mixture is subjected to HPHT process, thus forming a dense polycrystalline compact where diamond particles are bound together by newly formed silicon carbide material. [0027] The presence of catalyst materials inside the polycrystalline diamond body may promote the degradation of the cutting edge of the compact during the cutting process, especially if the edge temperature reaches a high enough critical value. It is theorized that the cobalt driven degradation may be caused by the large difference in coefficient of thermal expansion between diamond and catalyst (e.g. cobalt metal), and also by the catalytic effect of cobalt on diamond graphitization. Removal of catalyst from the polycrystalline diamond body of PDC compact, for example, by chemical leaching in acids, leaves an interconnected network of pores and a residual catalyst (up to about 10 vol%) trapped inside the polycrystalline diamond body. It has been demonstrated that depletion of cobalt from the polycrystalline diamond body of the PDC compact significantly improves a compact's abrasion resistance. Thus, it is theorized that a thicker cobalt depleted layer near the cutting edge, such as more than about 100 μιη may provide better abrasion resistance of the PDC compact than a thinner cobalt depleted layer, such as less than about 100 μιη.

[0028] A superabrasive compact 10 in accordance with an embodiment is shown in FIG. 1 . Superabrasive compact 10 may be inserted into a downhole of a suitable tool, such as a drill bit, for example. One example of the superabrasive compact 10 may include a diamond table 12 having a top surface 21 .

[0029] In one embodiment, the superabrasive compact 10 may be a standalone compact without a substrate. In another embodiment, the superabrasive compact 10 may include a substrate 20 attached to the diamond table 12 formed by

polycrystalline diamond particles. The substrate 20 may be metal carbide, attached to the diamond table 12 via an interface 22 separating the diamond table 12 and the substrate 20. The interface 22 may have an uneven interface. Substrate 20 may be made from cemented cobalt tungsten carbide, while the diamond table 12 may be formed from a polycrystalline ultra-hard material, such as polycrystalline diamond or diamond crystals bonded by a foreign material. [0030] Still in FIG. 1 , the diamond table 12 may include at least two layers with a first layer 26 and a second layer 24. The second layer 24 may be closer to the interface 22 and may be sandwiched between the substrate 20 and the first layer 26.

[0031 ] The compact 10 may be referred to as a polycrystalline diamond compact ("PCD") when polycrystalline diamond is used to form the diamond table 12. PCD compacts are known for their toughness and durability, which allow them to be an effective cutter in demanding applications. Although one type of superabrasive compact 10 has been described, other types of superabrasive compacts 10 may be utilized. For example, in one embodiment, superabrasive compact 10 may have a chamfer (not shown) around an outer peripheral of the top surface 21 . The chamfer may have a vertical height of about 0.5 mm or 1 mm and an angle of about 45° degrees, for example, which may provide a particularly strong and fracture resistant tool component. The superabrasive compact 10 may be a subject of procedure depleting catalyst metal (e.g. cobalt) near the cutting surface of the compact, for example, by chemical leaching of cobalt in acidic solutions. The unleached superabrasive compact may be fabricated according to processes known to persons having ordinary skill in the art. Methods for making diamond compacts and composite compacts are more fully described in United States Patent Nos.

3,141 ,746; 3,745,623; 3,609,818; 3,850,591 ; 4,394,170; 4,403,015; 4,794,326; and 4,954,139.

[0032] In certain applications, it may be desired to have a PCD body comprising a single PCD-containing volume or region, while in other applications, it may be desired that a PCD body be constructed having two or more different PCD- containing volume or regions. For example, it may be desired that the PCD body include a first PCD-containing region extending a distance D from the top surface or a working surface, as shown in FIG. 1 , and a second PCD-containing region extending from the first PCD-containing region to the substrate. The PCD-containing regions may be formed having different diamond densities and/or be formed from different diamond grain sizes, and/or be formed from leaching the PCD with acid solutions partially or fully. It is, therefore, understood that thermally stable polycrystalline diamond constructions of the invention may include one or multiple PCD regions within the PCD body as called for by a particular drilling or cutting application.

[0033] FIG. 2 illustrates the microstructure of the diamond table 12, and more specifically, a section of the thermally stable polycrystalline diamond 10. The diamond table 12 of the thermally stable region may have the first region 26 and the second region 24. The diamond table 12 may include bonded diamond grains 28 defining interstitial channels 42. A matrix of interstitial channels 42 between the bonded diamond grains may be filled with non-binder materials in the first region. In one embodiment, the non-binder materials may comprise silicon carbide. In another embodiment, the non-binder materials may comprise aluminum carbide, for example. The first thermally stable region comprising the interstitial regions free of the catalyst material is shown to extend a distance "D" from a working or cutting surface 21 of the thermally stable polycrystalline diamond 10. In one embodiment, the distance "D" is identified and measured by cross sectioning a thermally stable diamond table construction and using a sufficient level of magnification to identify the interface between the first and second regions.

[0034] The so-formed thermally stable first region 26 may not be subject to the thermal degradation encountered in the remaining areas of the PCD diamond body, resulting in improved thermal characteristics. The remaining region of the interstitial channels 42 in the second region 24 may be filled with a metal catalyst or binder material 46. The first region may comprise an additive, such as an inert chemical. The inert chemical may include glass or quartz. Glass filler may be chosen because glass has a low softening and melting point such that it may become liquid at relative low temperature, e.g., 600 °C. Quartz crystal may be chosen because quartz has the similar coefficient of thermal expansion (CTE) as diamond. The adding of quartz crystal may not cause thermal failure to the diamond table under high temperatures. The first region may occupy about 20% to up to about 95% volume of the diamond table 12. In one embodiment, the diamond table may have a uniform cylindrical shape from the top to the bottom, therefore the height D of the first region may be from about 20% to up to about 95% the total height of the diamond table 12. If the diamond table is about 2 mm thick, for example, the first region may be from about 1 mm to up to about 1 .9 mm, for example.

[0035] In one embodiment, the first region 26 of the diamond table 12 may have about 87.5% aluminum and about 12.5% silicon. The aluminum carbide and silicon carbide may be formed from a eutectic material comprising about 87.5% aluminum and about 12.5% silicon eutectic composition.

[0036] The diamond table 12 may be partially leached according to known methods. The selected region of the PCD body may be rendered thermally stable by removing substantially all of the catalyst material therefrom by exposing the desired surface or surfaces to acid leaching, as disclosed for example in U.S. Pat. No.

4,224,380, which is incorporated herein by reference. Generally, after the PCD body or compact is made by HPHT process, the identified surface or surfaces, e.g., at least a portion of the working or cutting surfaces, are placed into contact with the acid leaching agent for a sufficient period of time to produce the desired leaching catalyst material depletion depth.

[0037] Suitable leaching agents for treating the selected region to be rendered thermally stable include materials selected from the group consisting of inorganic acids, organic acids, mixtures and derivatives thereof. The particular leaching agent that is selected may depend upon such factors as the type of catalyst material used, and the type of other non-diamond metallic materials that may be present in the PCD body, e.g., when the PCD body is formed using synthetic diamond powder. While removing the catalyst material from the selected region operates to improve the thermal stability of the selected region, it is known that PCD bodies especially formed from synthetic diamond powder may include, in addition to the binder material, such as a metal selected from the group consisting of Co, Ni, Fe, and combinations thereof, or non-binder materials, such as other metallic elements that can also contribute to thermal instability. [0038] Graph itization may be reduced or eliminated in PCD materials if the binder material in PCD materials may, after sintering, be replaced with a material such as Si, aluminum, or an Si alloy. Similarly, micro-cracking may be reduced by lessening the mismatch between the expansion coefficient of the diamond phase and the binder material. Both of these goals may be accomplished by displacing the binder material with a different material or by substituting the material used as the binder material with a material having better physical properties. The PCD so formed is typically bonded to a substrate either in the same process or in a subsequent process to form a superabrasive compact. The present embodiment describes a superabrasive compact wherein the PCD is bonded to a substrate containing a binder material that melts and sweeps at low temperatures.

[0039] According to a method described below, a thermally stable polycrystalline diamond (PCD) body is placed adjacent to a substrate containing a binder material that melts at a lower temperature and subjected to a high-pressure high-temperature cycle. The PCD may degrade at high temperatures due to back-conversion to graphite or due to micro-cracking. In addition, it may be preferable to use lower pressures for bonding, so that the PCD is subjected to low internal stresses and hence less defects. Also, for a given pressing apparatus, using a lower pressure typically may mean that a large number of PCD may be pressed in a single cycle thus lowering the overall cost. In general, it may be beneficial to bond the PCD to the substrate at low temperature and low pressure while staying within the diamond stable region.

[0040] The thermally stable PCD may be made in several ways. For example, the PCD may be made from a thermally stable binder such as metal carbonate in a high pressure high temperature cycle. Alternatively, a catalyst/binder-sintered PCD may be at least partially leached in a subsequent step to remove the catalyst or binder material from the interstitial channels. The partially leached disc may be at least partially infiltrated with a non-binder material. [0041 ] In one embodiment, a substrate with a low melting point binder may be manufactured by introducing additives such as Cr or its compounds/alloys such as Cr2C3, NixCry, CrxBy or Nio.8Cro.17Bo.03 in the binder material such as Co, Ni, or Fe. The additive may be blended into the binder material and carbide powder before a green body of the substrate is pressed and sintered. Alternatively, the additive may be diffused or alloyed into the surface of a sintered substrate by a suitable technique. For example, a sintered tungsten carbide substrate may be surrounded by a boron containing material and subjected to a high temperature for a sufficient time to allow diffusion of boron onto the surface of or into the substrate.

[0042] In another embodiment, such a substrate may be manufactured by saturating the binder material with carbon while sintering the substrate, with the resulting sintered substrate having a high magnetic saturation value, typically greater than 80%, for example.

[0043] In yet another embodiment, the binder may constitute suitable low melting point alloys/solid solutions of metals, such as Co-B-V (or Ti).

[0044] Once in the press at the appropriate high pressure and high temperature, the binder material may melt and bond the substrate to the thermally stable diamond.

[0045] In one embodiment, the interstitial channels in the second region may be filled with a binder material and an additive from the substrate. The substrate may have a magnetic saturation value greater than 80%. In another embodiment, the additive may comprise more than 0.1 wt%, but less than 10 wt% of Cr. In some embodiment, the additive may comprise more than 0.1 wt%, but less than 2 wt% of Cr. In yet another embodiment, the additive may comprise more than 0.1 wt%, but less than 10 wt% Mn. In further another embodiment, the additive may comprise boron diffused onto a surface of or into the substrate. [0046] In one embodiment, as shown in FIG. 3, a method 30 of making a superabrasive compact may comprise steps of providing at least partially leached polycrystalline diamond table that comprises bonded diamond grains defining interstitial channels therein in a step 32; providing a material, such as a silicon material, positioned near a surface of the at least partially leached polycrystalline diamond table in a step 34; providing a substrate, such as cemented tungsten carbide, near the at least partially leached polycrystalline diamond table such that the at least partially leached polycrystalline diamond table is sandwiched between the material and the substrate in a step 36; and subjecting the substrate and the at least partially leached polycrystalline diamond table and the material to conditions of elevated temperature and pressure suitable for producing the polycrystalline superabrasive compact, wherein the substrate comprises a binder material and an additive in a suitable amount such that the melting point of the binder material is less than 1350 °C in a step 38.

[0047] The method 30 may further include a step of bonding the substrate to the second region of the at least partially leached polycrystalline diamond table.

Providing at least partially leached polycrystalline diamond table that comprises bonded diamond grains defining interstitial channels therein in the step 32 may further include a step of partially leaching the diamond table or fully leaching the diamond table after synthesizing the polycrystalline diamond compact. In one embodiment, the composite material includes silicon containing material. In another embodiment, the composite material may include aluminum containing material. In yet another embodiment, the composite may include a eutectic material comprising about 87.5% aluminum and about 12.5% silicon eutectic composition. During a first temperature about 1000 °C, aluminum containing material, silicon containing material, or silicon aluminum eutectic may infiltrate into the interstitial channels of the diamond table from the top of the diamond table and move toward the cemented tungsten carbide substrate. [0048] By the time when the temperature reaches about 1200 °C, the binder material, such as an iron group transitional metal, e.g., cobalt, nickel, or iron, and combinations thereof with less than 10% by weight of Cr, Mn, or boron as an additive, from the cemented carbide substrate may sweep into the interstitial channels of the diamonds. In another embodiment, the binder material may comprise a metal selected from the group consisting of Co, Ni, Fe, and combinations thereof with less than 2% by weight of Cr as the additive. In another embodiment, the additive may be blended into the binder material and carbide powder before a green body of the substrate is pressed and sintered. In further another embodiment, the additive may be diffused or alloyed into the surface of a sintered substrate by a suitable technique. For example, a sintered tungsten carbide substrate may be surrounded by a boron containing material and subjected to a high temperature for a sufficient time to allow diffusion of boron onto the surface of or into a sintered tungsten carbide. In further another embodiment, a substrate may be manufactured by saturating the binder material with carbon, such as graphite, while sintering the substrate. The resulting sintered substrate may have a high magnetic saturation value greater than 140 units, for example, and a lower melting point for the binder material.

[0049] A sintered tungsten carbide with about 12 wt% cobalt and stoichiometric carbon to tungsten ratio is expected to have a binder melting point of 1348 °C. If carbon is added before sintering to saturate the binder with carbon, then the melting point may be expected to drop to 1280 °C. If 1 .38 wt% Cr2C3 is added to the carbide powder mix before sintering, then the resulting binder melting point may be expected to be 1254 °C. If the binder is saturated with both Cr and C, the melting point may be expected to drop significantly to less than 1200 °C. Similarly, with 10 wt%

manganese to the tungsten carbide, cobalt, carbon mix being added before sintering, the melting point may be expected to drop to below 1200 °C. The actual drop may depend on the exact composition the carbide, including the amount of cobalt and carbon and other additives. [0050] The aluminum containing composite material, or silicon containing material may react with diamond to form aluminum carbide or silicon carbide at about first temperature. The aluminum or silicon may keep moving toward cemented tungsten carbide up to the interface between the first region and the second region where the binder sweeps through from cement tungsten carbide. The first region may occupy from about 20% to up to about 95% volume of the at least partially leached polycrystalline diamond table.

[0051 ] The composite material may be selected from a group consisting of as a powder, as a disk, as a ring, as a disk with perforated holes, as a triangle, as a rectangular. One or more steps may be inserted in between or substituted for each of the foregoing steps 32-38 without departing from the scope of this disclosure.

[0052] Example 1 :

[0053] PDC cutters were produced by the methods described in the prior art, composed of a starting diamond powder with an average grain size of 12 microns in diameter, or with an average grain size of 24 microns in diameter and a metal carbide, such as tungsten carbide, attached to the polycrystalline diamond via an interface between the polycrystalline diamond and tungsten carbide. The cutter was ground and finished to 16 mm in diameter, and 13 mm in height. A 45 degree bevel was placed on the edge of the diamond, with a thickness of about 0.4 mm. Some cutters were fully leached by removing the catalyst from the diamond table.

[0054] The Ta cup was loaded by pushing a WC substrate (OD 0.648") inside and the cup was laid upward. The WC substrate was pre-sintered with cobalt and an additive, such as Cr. Consequently, a fully leached porous diamond table (0.648") was loaded on top of the pre-sintered WC substrate. A piece of thin Si disc (0.002" thick) with a dimension of 0.650" was disposed on top of the diamond table evenly. Then, a Ta disc (0.005" thick and 0.650" OD) was used to cover Si disc followed by a mica disc and a graphite pill (0.1 " thick). Half of the graphite pill protruded out of the Ta cup. The assembled Ta cup with a graphite sleeve and some graphite pills were encapsulated. The Ta cup was fit inside the graphite sleeve tightly. The encapsulated cup was transferred into cell loading area, and the entire body was loaded into the cell specifically designed for belt pressing. The cell was loaded inside the die and was applied high pressure and high temperature (HPHT) cycle to the cell for 30 minutes. The soak pressure was maintained around 6.0 GPa and the soak temperature was about 1550 °C. The soak time for bonding of the thermally stable disc to the carbide was about 15 minutes. After the bonding cycle, the cup was taken out of the pressed cell for further finishing.

[0055] While reference has been made to specific embodiments, it is apparent that other embodiments and variations can be devised by others skilled in the art without departing from their spirit and scope. The appended claims are intended to be construed to include all such embodiments and equivalent variations.

Claims

1 . A superabrasive compact, comprising:
a substrate;
a diamond table attached to the substrate, wherein the diamond table has a first region and a second region, the second region is sandwiched between the first region and the substrate, wherein the diamond table includes bonded diamond grains defining interstitial channels, the interstitial channels are filled with non-binder material in the first region, the interstitial channels in the second region are filled with a material sourced from the substrate wherein the sourced material contains a binder material and an additive from the substrate, wherein the melting point of the binder material is lower than 1350 °C at an ambient pressure.
2. The superabrasive compact of the claim 1 , wherein the non-binder material in the first region comprises silicon carbide.
3. The superabrasive compact of the claim 1 , wherein the substrate has a magnetic saturation value greater than 80%.
4. The superabrasive compact of the claim 1 , wherein the additive comprises more than 0.1 wt%, but less than 10 wt% of Cr.
5. The superabrasive compact of the claim 4, wherein the additive comprises more than 0.1 wt%, but less than 10 wt% Mn.
6. The superabrasive compact of the claim 5, wherein the additive comprises boron diffused onto a surface of or into the substrate.
7. A method of making a superabrasive compact, comprising:
providing at least a partially leached polycrystalline diamond table that comprises bonded diamond grains defining interstitial channels therein; providing a material positioned near a surface of the at least partially leached polycrystalline diamond table;
providing a substrate near the at least partially leached polycrystalline diamond table such that the at least partially leached polycrystalline diamond table is sandwiched between the material and the substrate; and
subjecting the substrate and the at least partially leached polycrystalline diamond table and the material to conditions of elevated temperature and pressure suitable for producing the polycrystalline superabrasive compact, wherein the substrate comprises a binder material and an additive in a suitable amount such that the melting point of the binder material is less than 1350 °C.
8. The method of the claim 7, wherein the substrate is cemented tungsten carbide.
9. The method of the claim 7, wherein the binder material comprises a metal selected from the group consisting of Co, Ni, Fe, and combinations thereof with more than 0.1 wt%, but less than10% by weight of Cr as the additive.
10. The method of the claim 7, wherein the binder material comprises a metal selected from the group consisting of Co, Ni, Fe, and combinations thereof with more than 0.1 wt%, but less than 2% by weight of Cr as the additive.
1 1 . The method of the claim 7, wherein the substrate has a magnetic saturation value greater than 80 %.
12. The method of the claim 7, further comprising diffusing boron containing material onto surface of or into a sintered tungsten carbide.
13. The method of the claim 7, wherein the first region occupies from about 20% to up to about 95% volume of the at least partially leached polycrystalline diamond table.
14. The method of the claim 7, wherein the binder material comprises a metal selected from the group consisting of Co, Ni, Fe, and combinations thereof with more than 0.1 wt%, but less than10% by weight of Mn.
15. The method of claim 7, wherein the binder material comprises a metal selected from the group consisting of Co, Ni, Fe, and combinations thereof with more than 0.1 wt%, but less than 5% by weight of Mo.
16. The method of claim 7, wherein the binder material comprises a metal selected from the group consisting of Co, Ni, Fe, and combinations thereof with more than 0.1 wt%, but less than10% by weight of Boron.
17. A superabrasive compact, comprising:
a substrate;
a diamond table attached to the substrate, wherein the diamond table has a first region and a second region, the second region is sandwiched between the first region and the substrate, wherein the diamond table includes bonded diamond grains defining interstitial channels, the interstitial channels are filled with non-binder materials in the first region, the interstitial channels in the second region are filled with a binder material and an additive from the substrate, wherein the first region occupies from about 20% to up to about 95% volume of the diamond table, wherein the melting point of the binder material is lower than 1350 °C at an ambient pressure.
18. The superabrasive compact of the claim 17, wherein the non-binder materials comprise silicon carbide.
19. The superabrasive compact of the claim 17, wherein the additive comprises more than 0.1 wt%, but less than 10 wt% of Cr.
20. The superabrasive compact of the claim 17, wherein the additive comprises more than 0.1 wt%, but less than 2 wt% of Cr.
21 . The superabrasive compact of the claim 17, wherein the binder material comprises a metal selected from the group consisting of Co, Ni, Fe, and combinations thereof.
22. The superabrasive compact of the claim 17, wherein the additive comprises more than 0.1 wt%, but less than 10 wt% Mn.
23. The superabrasive compact of the claim 22, wherein the additive comprises boron diffused onto a surface of or into the substrate.
24. The superabrasive compact of the claim 17, wherein the additive comprises more than 0.1 wt%, but less than 5 wt% Mo.
PCT/US2014/033437 2014-04-09 2014-04-09 Polycrystalline diamond compact with enhanced thermal stability WO2015156789A1 (en)

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