Polycrystalline diamond compact with increased leaching surface area and method of leaching a polycrystalline diamond compact
11680449 · 2023-06-20
Assignee
Inventors
- William Brian Atkins (Houston, TX)
- Gagan Saini (The Woodlands, TX, US)
- Grant O. Cook, III (Spring, TX, US)
Cpc classification
C22C26/00
CHEMISTRY; METALLURGY
B22F2999/00
PERFORMING OPERATIONS; TRANSPORTING
E21B10/5673
FIXED CONSTRUCTIONS
B22F2998/10
PERFORMING OPERATIONS; TRANSPORTING
B22F7/06
PERFORMING OPERATIONS; TRANSPORTING
B22F2998/10
PERFORMING OPERATIONS; TRANSPORTING
C22C26/00
CHEMISTRY; METALLURGY
B22F7/06
PERFORMING OPERATIONS; TRANSPORTING
B22F2999/00
PERFORMING OPERATIONS; TRANSPORTING
E21B10/46
FIXED CONSTRUCTIONS
E21B10/5735
FIXED CONSTRUCTIONS
B22F3/24
PERFORMING OPERATIONS; TRANSPORTING
E21B10/573
FIXED CONSTRUCTIONS
International classification
B22F3/24
PERFORMING OPERATIONS; TRANSPORTING
B22F7/06
PERFORMING OPERATIONS; TRANSPORTING
C22C26/00
CHEMISTRY; METALLURGY
E21B10/46
FIXED CONSTRUCTIONS
E21B10/567
FIXED CONSTRUCTIONS
Abstract
The present disclosure provides a sintering assembly and a polycrystalline diamond compact (PDC) including a acid-labile leach-enhancing material, a PDC including cavities formed by removal of an acid-labile leach-enhancing material, and a method of forming a leached PDC using an acid-labile leach-enhancing material. The present disclosure further includes drill bits using PDCs formed suing an acid-labile leach-enhancing material.
Claims
1. An unleached polycrystalline diamond compact (PDC) comprising: a substrate; and an unleached polycrystalline diamond table including an acid-labile leach-enhancing material and a sintering aid, wherein the acid-labile leach-enhancing material is more labile in an acid than the sintering aid and comprises a mixture of both of microstructures having an average largest linear dimension of less than 100 μm and nanostructures having an average largest linear dimension of less than 1000 nm.
2. The PDC of claim 1, wherein the sintering aid comprises cobalt and the acid-labile leach-enhancing material comprises tungsten (W).
3. The PDC of claim 1, wherein the acid-labile leach-enhancing material is configured for removal in the acid to define a plurality of cavities of less than 100 μm within the polycrystalline diamond table that increase the leaching surface area of the polycrystalline diamond table as a result of the removal of the acid-labile leach-enhancing material.
4. An unleached polycrystalline diamond compact (PDC) comprising: a substrate; and an unleached polycrystalline diamond table including an acid-labile leach-enhancing material and a sintering aid, wherein the acid-labile leach-enhancing material is more labile in an acid than the sintering aid and comprises one or both of microstructures having an average largest linear dimension of less than 100 μm and nanostructures having an average largest linear dimension of less than 1000 nm, wherein one or both of the microstructures and the nanostructures of the acid-labile leach-enhancing material are oriented in a pattern in the polycrystalline diamond table.
5. The PDC of claim 4, wherein the sintering aid comprises cobalt and the acid-labile leach-enhancing material comprises tungsten (W).
6. The PDC of claim 4, wherein the acid-labile leach-enhancing material is in the form of a mixture of both the microstructures and the nanostructures.
7. The PDC of claim 4, wherein the acid-labile leach-enhancing material is configured for removal in the acid to define a plurality of cavities of less than 100 μm within the polycrystalline diamond table that increase the leaching surface area of the polycrystalline diamond table as a result of the removal of the acid-labile leach-enhancing material.
8. A polycrystalline diamond (PDC) sintering assembly comprising: a substrate; polycrystalline diamond grains; a sintering aid; one or both of microstructures having an average largest linear dimension of less than 100 μm or nanostructures having an average largest linear dimension of less than 1000 nm of an acid-labile leach-enhancing material disposed in the polycrystalline diamond grains, wherein the acid-labile leach-enhancing material is oriented in a pattern in the polycrystalline diamond grains; and a can in which the substrate, polycrystalline diamond grains, sintering aid, and acid-labile leach-enhancing material are disposed.
9. The PDC sintering assembly of claim 8, wherein the substrate comprises the sintering aid.
10. The PDC sintering assembly of claim 8, wherein the acid-labile leach-enhancing material is more labile in an acid than the sintering aid.
11. The PDC sintering assembly of claim 8, wherein the acid-labile leach-enhancing material comprises tungsten (W).
12. A polycrystalline diamond (PDC) sintering assembly comprising: a substrate; polycrystalline diamond grains; a sintering aid; one or both of microstructures having an average largest linear dimension of less than 100 μm or nanostructures having an average largest linear dimension of less than 1000 nm of an acid-labile leach-enhancing material disposed in the polycrystalline diamond grains, wherein the acid-labile leach-enhancing material has a dog-bone structure; and a can in which the substrate, polycrystalline diamond grains, sintering aid, and acid-labile leach-enhancing material are disposed.
13. The PDC sintering assembly of claim 12, wherein the substrate comprises the sintering aid.
14. The PDC sintering assembly of claim 12, wherein the acid-labile leach-enhancing material is more labile in an acid than the sintering aid.
15. The PDC sintering assembly of claim 12, wherein the acid-labile leach-enhancing material comprises tungsten (W).
16. A polycrystalline diamond (PDC) sintering assembly comprising: a substrate; polycrystalline diamond grains; a sintering aid; one or both of microstructures having an average largest linear dimension of less than 100 μm or nanostructures having an average largest linear dimension of less than 1000 nm of an acid-labile leach-enhancing material disposed in the polycrystalline diamond grains, wherein the acid-labile leach-enhancing material is in the form of a template or mesh or adhered to the can; and a can in which the substrate, polycrystalline diamond grains, sintering aid, and acid-labile leach-enhancing material are disposed.
17. The PDC sintering assembly of claim 16, wherein the substrate comprises the sintering aid.
18. The PDC sintering assembly of claim 16, wherein the acid-labile leach-enhancing material is more labile in an acid than the sintering aid.
19. The PDC sintering assembly of claim 16, wherein the acid-labile leach-enhancing material comprises tungsten (W).
Description
BRIEF DESCRIPTION OF THE DRAWINGS
(1) A more complete understanding of the present embodiments and advantages thereof may be acquired by referring to the following description taken in conjunction with the accompanying drawings, which show particular embodiments of the current disclosure, in which like numbers refer to similar components, and in which:
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DETAILED DESCRIPTION
(25) The present disclosure relates to unleached PDCs with an acid-labile leach-enhancing material included in the polycrystalline diamond table. This acid-labile leach-enhancing material may be removed prior to or during leaching to increase the surface area of the polycrystalline diamond table available for further leaching. The present disclosure also includes leached PDCs containing cavities where acid-labile leach-enhancing material was located, or backfill material in such cavities. The present disclosure further provides methods of leaching the polycrystalline diamond table of a PDC using increased leaching surface area made available by removing acid-labile leach-enhancing material to leave cavities in the polycrystalline diamond table.
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(27) Referring to
(28) In
(29) Leached PDC cutter 100 may be used without further treatment. However, cavities 90 may also be wholly or partially filed with a backfill material 140 to result in backfilled PDC cutter 130, as shown in
(30) Substrate 30 may be any substrate suitable for use in a PDC cutter. In particular, it may be a conventional substrate, such as a tungsten carbide substrate. Substrate 30 may include a sintering aid that catalyzes the formation of diamond-diamond bonds, allowing diamond grains 40 to form polycrystalline diamond table 60 in the HTHP process. The sintering aid may also be located with diamond grains 40, both in substrate 30 and diamond grains 40, or in any other location that allows it to catalyze the formation of diamond-diamond bonds during the HTHP process. The sintering aid may also assist in bonding diamond table 60 to substrate 30 and in forming substrate 30 if it is not in final form before the HTHP process. Any one or combination of sintering aids may be used. Suitable sintering aids include Group VIII metals, such as Co, nickel (Ni), iron (Fe), or copper (Cu), and their alloys.
(31) Diamond grains 40 may be any suitable diamond grains, including diamond grains of substantially uniform grain sizes, diamond grains of mixed grain sizes, or mixtures thereof located in different areas of what will become polycrystalline diamond table 60 after it is formed.
(32) Acid-labile leach-enhancing material 50 may be any material that is able to remain at least partially intact during the HTHP process and then be dissolved by acid more readily than at least one sintering aid because it is more acid-labile in the acid than the sintering aid. The purpose of acid-labile leach-enhancing material 50 is to be removed by acid prior to or during leaching, thereby forming cavities 90, which provide greater surface area of polycrystalline diamond table 90 in contact with a leaching fluid. Accordingly, acid-labile leach-enhancing material 50 may be dissolved by acid more readily than all sintering aids, when more than one sintering aid is present, because it is more acid-labile in the acid than any of the sintering aids.
(33) Suitable acid-labile leach-enhancing materials 50 include W, halfnium (Hf), and vanadium (V), metal-coated W, Hf, or V, such as Ni or Co-coated W, Hf, or V, and other metals or alloys, ceramics, and glasses.
(34) In order to remain at least partially intact during the HTHP process, suitable acid-labile leach-enhancing materials 50 may have limited ability to dissolve into or otherwise enter diamond grains 40 during an HTHP process. They may also be able to retain their general shape during such a process. Thus, at least a portion of the acid-labile leach-enhancing material 50 will typically have a melting point above the temperature of the HTHP process. Acid-labile leach-enhancing materials 50 may have sufficient ductility to cause them to elongate during an HTHP process, thereby further increasing leaching surface area provided by cavities 90.
(35) Acid-labile leach-enhancing materials 50 may be removed by a pre-leaching acid prior to leaching polycrystalline diamond table 60. A pre-leaching acid may be able to remove at least 80 wt %, at least 90 wt %, at least 95 wt %, or at least 99 wt % of acid-labile leach-enhancing materials 50 when incubated at 20° C. for 1 day. The pre-leaching acid may also remove no more than 10 wt % of the sintering aid from polycrystalline diamond table 60a when incubated at 20° C. for 1 day, although in most instances, removal of sintering aid during pre-leaching is not a problem and may actually be a benefit, such that it is not a concern of more than 10 wt % sintering aid is removed by the pre-leaching acid.
(36) Hydrofluoric acid (HF) is an example of one suitable pre-leaching acid for use with a W-containing acid-labile leach-enhancing material 50.
(37) Leaching may then be conducted with any suitable leaching agent able to dissolve at least one sintering aid and remove it from polycrystalline diamond table 60. For instance, nitric and sulfuric acids and mixtures thereof are often used as the leaching agent for Co and Co-based sintering aids. Leached agents enter polycrystalline diamond via a surface in contact with the leaching agent and leached sintering aid exits with such a surface. The surface area of a polycrystalline diamond table available to contact the leaching agent may be referred to as the leaching surface area. Cavities 90 increase the leaching surface area of polycrystalline diamond table 60. In particular, cavities 90 increase the leaching surface area inside polycrystalline diamond table 60.
(38) In
(39) Although
(40) In addition, although
(41) Acid-labile leach-enhancing material 50 may be in the form of microstructures or nanostructures, or a mixture thereof. Microstructures generally have an average largest linear dimension of at least 1 μm and less than 1000 μm, less than 500 μm, or less than 100 μm. Nanostructures generally have an average largest linear dimension of at least 1 nm and less than 1000 nm, less than 500 nm, or less than 100 nm. Microstructures may be better able to increase leaching surface area than nanostructures, but microstructures may cause greater decreases in mechanical strength of polycrystalline diamond table 60 than do nanostructures. Due to the tendency of microstructures to decrease mechanical strength of polycrystalline diamond table 60 more than nanostructures, it may be possible to include more acid-labile leach-enhancing material 50 by overall volume when it is in the form of nanostructures. Thus, the total available leaching surface area may still be similar to that obtained using microstructures.
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(44) The benefits of both microstructures and nanostructures of acid-labile leach-enhancing material 50 may be achieved by using a mixture of both. The proportions of microstructures to nanostructures by number in the mixture may be between 5:1 and 1:5, in particular between 2:1 and 1:2.
(45) Acid-labile leach-enhancing material 50, whether in the form of microstructures, nanostructures, or a mixture, may be evenly distributed within diamond grains 40 so that cavities 90 are evenly distributed within polycrystalline diamond table 60 or a portion thereof. This even distribution may increase the mechanical stability of polycrystalline diamond table 60, particularly if cavities 90 are not backfilled.
(46) Although
(47) Acid-labile leach-enhancing material 50 may be oriented in diamond grains 40 and subsequently in polycrystalline diamond table 60 in a particular pattern or manner. For instance, elongated microstructures of acid-labile leach-enhancing material 50, such as those of
(48) In addition because fractures in the polycrystalline diamond table during PDC use tend to run along boundaries between leached and unleached regions, acid-labile leach-enhancing material 50 may be oriented in a particular pattern or manner to direct the location of such boundaries and thus the likely location of fractures, which may lead to improved PDC life.
(49) Acid-labile leach-enhancing material 50 may be oriented using any of a variety of methods. For instance, if acid-labile leach-enhancing material 50 contains a magnetic component, such as a Co, Ni, or Fe coating on W as shown in
(50) Acid-labile leach-enhancing material 50 may also be directed to particular regions of diamond grains 40 and ultimately polycrystalline diamond table 60 using a magnetic or electric field, or by vibrating sintering assembly 10.
(51) As shown in
(52) Acid-labile leach-enhancing material 50 may be grown on or with template 150. It may also be 3-D printed using additive manufacturing on or with template 150.
(53) Rather than using a separate template 150, acid-labile leach-enhancing material 50 may also simply be adhered to or grown on can 20.
(54) Regardless of the template 150 used or whether the acid-labile leach-enhancing material 50 is grown on can 20, after removal and leaching, a leached polycrystalline diamond table 60b similar to that of
(55) Pre-formed structures of acid-labile leach-enhancing material 50 may also be used within diamond grains 40 prior to sintering, resulting in cavities 90 with a particular orientation in polycrystalline diamond table 60. For instance, as shown in
(56) Although a mesh may be formed having either a micro- or nano-sized diameter of its component strands, nano-sized strands may be more effective.
(57) A mesh of acid-labile leach-enhancing material 50 results in an interconnected grid or a plurality of interconnected grids of cavities 90. However, acid-labile leach-enhancing material 50 may also form an interconnected grid or plurality of interconnected grids of cavities 90 in other manners. For instance, microstructures and nanostructures may be arranged such that they occasionally touch one another, which produces connected cavities 90. This may be particularly effective when a combination of both microstructures 50a and nanostructures 50b of acid-labile leach-enhancing material are used, as shown in
(58) Multiple ways of orienting or directing acid-labile leach-enhancing material 50 may be employed to produce the same PDC cutter. For instance, elongated nanostructures of acid-labile leach-enhancing material 50 having polarizable terminal moieties, such as those shown in
(59) More than one type of acid-labile leach-enhancing material 50 may be used to form a single PDC cutter. These multiples types of material may be mixed together uniformly or in different proportions, then placed in diamond grains 40. Alternatively, the different types of materials may be localized to different regions of diamond grains 40. For instance, a first, more acid-labile leach-enhancing material 50c may be placed around the circumference of the chamber containing diamond grains 40, while a second less acid-labile leach-enhancing material 50d may be placed in a central portion of the chamber, as shown in
(60) Although the acid-labile leach-enhancing material 50 of
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(64) In addition to the sintering assemblies and PDC cutters described in
(65) A substrate and polycrystalline diamond power with acid-labile leach-enhancing material are combined in a can to form a sintering assembly that is subjected to an HTHP process that forms a sintered PDC cutter with an unleached polycrystalline diamond table in which the acid-labile leach-enhancing material remains at least partially intact. The unleached polycrystalline diamond is then placed in a pre-leaching agent that removes at least a portion of the acid-labile leach-enhancing material to form cavities in the polycrystalline diamond table of the sintered PDC cutter. The PDC cutter is then placed in a leaching agent that removes a sintering aid from the polycrystalline diamond table to form a leached polycrystalline diamond table in a leached PDC cutter. The leached polycrystalline diamond table may still have leached and unleached portions. In particular, it may have a leached portion extending to a leaching depth from a surface, and an unleached portion adjacent the substrate. The cavities remain in the leached polycrystalline diamond table after leaching, but they may be backfilled with a backfill material to produce a backfilled PDC cutter.
(66) When conventional leaching methods are used, the rate of leaching slows down as leaching progresses to greater depths within the PDC cutter. Thus, the rate of leaching also slows down as total leaching time increases. This effect is illustrated conceptually by the “Conventional Leaching” line in the graph of
(67) A PDC cutter as described herein or formed using the methods described herein may be incorporated into an industrial device, such as an earth-boring drill bit, as illustrated in
(68) Bit body 220 may include a plurality of blades 230 extending therefrom. Bit body 220 may be formed from steel, a steel alloy, a matrix material, a metal-matrix composite, or other suitable bit body material desired strength, toughness and machinability. Bit body 220 may be formed to have desired wear and erosion properties. PDC cutters 210 may be located in gage region 240, or in a non-gage region, or both.
(69) Drilling action associated with drill bit 200 may occur as bit body 220 is rotated relative to the bottom of a wellbore in response to rotation of an associated drill string. At least some PDC cutters 210 disposed on associated blades 230 may contact adjacent portions of a downhole formation during drilling. These PDC cutters 210 may be oriented such that their polycrystalline diamond tables contact the formation.
(70) The present disclosure provides an embodiment A relating to an unleached PDC including a substrate and an unleached polycrystalline diamond table including an acid-labile leach-enhancing material and a sintering aid.
(71) The present disclosure provides an embodiment B relating to a leached PDC including a substrate and a leached polycrystalline diamond table including a plurality of microstructure or nanostructure cavities, or a mixture thereof.
(72) The present disclosure provides an embodiment C relating to a drill bit including a bit body and the PDC of embodiment B.
(73) The present disclosure provides an embodiment D relating to a PDC sintering assembly including a substrate, polycrystalline diamond grains, a sintering aid, microstructures or nanostructures or a mixture thereof of acid-labile leach-enhancing material disposed in the polycrystalline diamond grains, and a can in which the substrate, polycrystalline diamond grains, sintering aid and acid-labile leach-enhancing material are disposed.
(74) The present disclosure further provides an embodiment E relating to a method of forming a leached PDC by placing a substrate, polycrystalline diamond grains containing microstructures, nanostructures, or a mixture of both of an acid-labile leach-enhancing material, and a sintering aid in a can to form a sintering assembly, performing an HTHP process on the sintering assembly to produce a sintered PDC with a polycrystalline diamond table containing the acid-labile leaching boost material, removing at least a part of the acid-labile leach-enhancing material from the polycrystalline diamond table, and leaching the polycrystalline diamond table to remove at least a part of the sintering aid.
(75) In addition, embodiments A, B, C, D and E may be used in conjunction with one another and the following additional elements, which may also be combined with one another unless clearly mutually exclusive, and which method elements may be used to obtain devices and which device elements may result from methods: i) the acid-labile leach-enhancing material may be more labile in an acid than the sintering aid; ii) the acid-labile leach-enhancing material may be in the form of a microstructure; ii) the acid-labile leach-enhancing material may be in the form of a nanostructure; iii) the acid-labile leach-enhancing material may be in the form of a mixture of microstructures and nanostructures; iv) the acid-labile leach-enhancing material may be in a dog bone structure; v) the acid-labile leach-enhancing material may be coated with a magnetic material; vi) the acid-labile leach-enhancing material may have a polarizable moiety; vii) the acid-labile leach-enhancing material may be may be part of a template; vii) the acid-labile leach-enhancing material may be part of a mesh; viii) the acid-labile leach-enhancing material may be adhered to the can; the acid-labile leach-enhancing material may be oriented in a pattern in the polycrystalline diamond table; ix) the acid-labile leach-enhancing material may be may include W; x) the acid-labile leach-enhancing material may define a plurality of cavities within the polycrystalline diamond table that increase the leaching surface area of the polycrystalline diamond table after removal of the acid-labile leach-enhancing material; xi) the polycrystalline diamond table may include a plurality of both microstructure and nanostructure cavities; xii) the microstructure or nanostructure cavities, or both, form at least one interconnected grid of cavities; xiii) the microstructure or nanostructure cavities may increase the leaching surface area of the polycrystalline diamond table; ix) the cavities may include a backfill material; x) the leached polycrystalline diamond may include a leached region surrounding the plurality of cavities and an unleached region; xi) the substrate may include the sintering aid; xii)
(76) Although only exemplary embodiments of the invention are specifically described above, it will be appreciated that modifications and variations of these examples are possible without departing from the spirit and intended scope of the invention. For instance, the use of PDCs on other industrial devices may be determined by reference to the drill bit example.