IE85364B1 - Thermally stable diamond bonded materials and compacts - Google Patents

Abstract

ABSTRACT Thermally stable diamond bonded materials and compacts include a diamond body having a thermally stable region and a PCD region, and a substrate integrally joined to the body. The thermally stable region has a microstructure comprising a plurality of diamond grains bonded together by a reaction with a reactant material. The PCD region extends from the thermally stable region and has a microstructure of bonded together diamond grains and a metal solvent catalyst disposed interstitially between the bonded diamond grains. The compact is formed by subjecting the diamond grains, reactant material, and metal solvent catalyst to a first temperature and pressure condition to form the thermally stable region, and then to a second higher temperature condition to both form the PCD region and bond the body to a desired substrate.

Description

TIIERMALLY STABLE DIAMOND BONDED MATERIALS AND COMPACTS FIELD OF THE INVENTION This invention generally relates to diamond bonded materials and, more specifically, diamond bonded materials and compacts formed therefrom that are specially designed to provide improved thermal stability when compared to conventional polycrystalline diamond materials.

BACKGROUND OF THE INVENTION Polycrystalline diamond (PCD) materials and PCD elements formed therefrom are well known in the art. Conventional PCD is formed by combining diamond grains with a suitable solvent catalyst material to form a mixture. The mixture is subjected to processing conditions of extremely high pressure/high temperature, where the solvent catalyst material promotes desired intercrystalline diamond-to-diamond bonding between the grains, thereby forming a PCD structure.

The resulting PCD structure produces enhanced properties of wear resistance and hardness, making PCD materials extremely useful in aggressive wear and cutting applications where high levels of wear resistance and hardness are desired.

Solvent catalyst materials that are typically used for forming conventional PCD include metals from Group VIII of the Periodic table, with cobalt (Co) being the most common.

Conventional PCD can comprise from 85 to 95% by volume diamond and a remaining amount of the solvent catalyst material. The solvent catalyst material is present in the microstructure of the PCD material within interstices that exist between the bonded together diamond grains.

A problem known to exist with such conventional PCD materials is thermal degradation due to differential themial expansion characteristics between the interstitial solvent catalyst material and the intercrystalline bonded diamond. Such differential thermal expansion is known to occur at temperatures of about 400°C, causing ruptures to occur in the diamond-to- diamond bonding, and resulting in the formation of cracks and chips in the PCD structure.

Another problem known to exist with conventional PCD materials is also related to the presence of the solvent catalyst material in the interstitial regions and the adherence of the solvent catalyst to the diamond crystals to cause another tom of thermal degradation. Specifically, the solvent catalyst material is known to cause an undesired catalyzed phase transformation in diamond (converting it to carbon monoxide, carbon dioxide, or graphite) with increasing temperature, thereby limiting practical use of the PCD material to about 750°C.

Attempts at addressing such unwanted forms of thermal degradation in PCD are knovm in the art. Generally, these attempts have involved the formation of a PCD body having an improved degree of thermal stability when compared to the conventional PCD material discussed above. One known technique of producing a thermally stable PCD body involves at least a two-stage process of first fonning a conventional sintered PCD body, by combining diamond grains and a cobalt solvent catalyst material and subjecting the same to high pressure/high temperature process, and then removing the solvent catalyst material therefrom.

This method, which is fairly time consuming, produces a resulting PCD body that is substantially free of the solvent catalyst material, and is therefore promoted as providing a PCD body having improved thermal stability. However, the resulting thermally stable PCD body typically does not include a metallic substrate attached thereto by solvent catalyst infiltration from such substrate due to the solvent catalyst removal process. The thermally stable PCD body also has a coefficient of thennal expansion that is sufficiently different from that of conventional substrate materials (such as WC-Co and the like) that are typically infiltrated or otherwise attached to the PCD body to provide a PCD compact that adapts the PCD body for use in many desirable applications. This difference in thermal expansion between the thermally stable PCD body and the substrate, and the poor wetability of the thermally stable PCD body diamond surface makes it very difficult to bond the thermally stable PCD body to conventionally used substrates, thereby requiring that the PCD body itself be attached or mounted directly to a device for use.

However, since such conventional thermally stable PCD body is devoid of a metallic substrate, it cannot (e.g., when configured for use as a drill bit cutter) be attached to a drill bit by conventional brazing process. The use of such thermally stable PCD body in this particular application necessitates that the PCD body itself be mounted to the drill bit by mechanical or interference fit during manufacturing of the drill bit, which is labor intensive, time consuming, and which does not provide a most secure method of attachment.

Additionally, because such conventional thermally stable PCD body no longer includes the solvent catalyst material, it is known to be relatively brittle and have poor impact strength, thereby limiting its use to less extreme or severe applications and making such thermally stable PCD bodies generally unsuited for use in aggressive applications such as subterranean drilling and the like. it is, therefore, desired that a diamond material be developed that has improved thermal stability when compared to conventional PCD materials. It is also desired that a diamond compact be developed that includes a thermally stable diamond material bonded to a suitable substrate to facilitate attachment of the compact to an application device by conventional method such as welding or brazing and the like. It is further desired that such thermally stable diamond material and compact formed therefrom have improved properties of hardness/toughness and impact strength when compared to conventional thermally stable PCD material described abcwe, and PCD compacts formed therefrom. it is further desired that such a product can be manufactured at reasonable cost without requiring excessive mamfacturing times and without the use of exotic materials or techniques.

SUMMARY OF THE INVENTION A lirst aspect of the invention provides a thermally stable diamond bonded compact comprising: a diamond bonded body comprising; a thermally stable region extending a distance below a diamond bonded body surface, the thermally stable region having a material microstructure comprising a plurality of diamond grains bonded together by a reaction product of the diamond grains and a reactant; a polycrystalline diamond region extending a depth from the thermally stable region and having a material microstructure comprising intercrystallinc bonded together diamond grains and a metal solvent catalyst disposal within interstitial regions between the intererystalline bonded together diamond grains; and a metallic substrate attached to the polycrystalline diamond region; wherein the reactant is selected from the group of materials capable of reacting with the diamond at a temperature below the melting temperature of the metal solvent catalyst.

A second aspect of the invention provides a method for makinga thermally stable diamond bonded compact comprising a diamond bonded body attached to a substrate, the method comprising the steps of: combining a volume ofdiamond grains to form a mixture; placing a first intiltrant material adjacent a portion of the mixture; placing a metallic substrate adjacent another portion of the mixture; infiltrating a first region ofthe mixture at a first temperature and pressure condition, wherein during the first temperature and pressure condition the first infiltrant reacts with and bonds together the diamond grains to form a thermally stable diamond bonded region of the diamond bonded body; infiltrating a second region of the mixture at a second temperature condition that is higher than the first temperature condition, wherein during the second temperature condition a second infiltrant provided from the metallic substrate melts and infiltrates the second region to form a polycrystalline diamond region of the diamond bonded body, wherein the first and second regions are bonded together; and forming an attachment between the polycrystalline diamond region of the diamond bonded body and the substrate during the step of forming the polycrystalline diamond region.

Thermally stable diamond bonded materials and compacts formed therefrom according to principles of this invention have improved thermal stability when compared to conventional PCD materials, and include a suitable substrate to facilitate attachment of the compact to an application device by corventional method sudr as welding or brazing andthe like. Thermally stable diamond materials and compacts formed therefrom have improved properties of hardness/toughness and impactstrength when compared to conventional thermally stable PCD material described above, and PCD compacts formed therefrom.

BRIEF DESCRIPTION OF THE DRAWINGS These and other features and advantages of the present invention will be appreciated as the same becomes better understood by reference to the following detailed description when considered in connection with the accompanying drawings wherein: FIG. 1 is schematic view taken from a thermally stable region of a diamond bonded material of this invention; FIG. 2 is a perspective View of a thermally stable diamond bonded compact of this invention comprising a diamond bonded body and a substrate bonded thereto; FIGS. 3A and 3B are cross-sectional schematic \news of the thermally stable diamond bonded compacts of FIG. 2; FIG. 4 is a perspective side view of an insert, for use in a roller cone or a hammer drill bit, comprising the thermally stable diamond bonded compact of FIGS. 3A and 3B; FIG. 5 is a perspective side view of a roller cone drill bit comprising a number of the inserts of FIG. 4; FIG. 6 is a perspective side view of a percussion or hammer bit comprising a number ofinserts of FIG. 4; FIG. 7 is a schematic perspective side view of a diamond shear cutter comprising the thermally stable diamond bonded compact of FIGS. 3A and 3B; and FIG. 8 is a perspective side view of a drag bit comprising a number of the shear cutters of FIG. 7.

DETAILED DESCRIPTION Thermally stable diamond bonded materials and compacts of this invention are specifically engineered having a diamond bonded body comprising a thermally stable diamond bonded region, thereby providing improved thermal stability when compared to conventional PC D materials. As used herein, the term PCD is used to refer to polycrystalline diamond that has been formed, at high pressure/high temperature (HPHT) conditions, through the use of a metal solvent catalyst, such as those metals included in Group VIII of the Periodic table. The thermally stable diamond bonded region in diamond bonded bodies of this invention, is not referred to as being PCD because, unlike conventional PCD and thermally stable PCD, it is not formed by the removal of a metal solvent catalyst.

Thermally stable diamond bonded materials and compacts of this invention also include a region comprising conventional PCD, i.e., intercrystalline bonded diamond formed using a metal solvent catalyst, thereby providing properties of hardness/toughness and impact strength that are superior to conventional thermally stable PCD materials that have been rendered thermally stable by having substantially all of the solvent catalyst material removed. Such PCD region also enables thennally stable diamond bonded materials of this invention to be permanently attached to a substrate by virtue of the presence of such metal solvent catalyst, thereby enabling thermally stable diamond bonded compacts of this invention to be attached to cutting or wear devices, e. g., drill bits when the diamond compact is configured as a cutter, by conventional means such as by brazing and the like.

Thermally stable diamond bonded materials and compacts of this invention are formed during a single HPHT process to produce a desired thermally stable diamond bonded material in one region of the body, while also providing PCD in another region to provide a permanent attachment between the diamond bonded body and a desired substrate.

FIG. 1 illustrates a region of a thermally stable diamond bonded material 10 of this invention having a material microstructure comprising the following material phases. A first material phase 12 comprises intercrystalline bonded diamond that is formed by the bonding together of adjacent diamond grains at HPHT. A second material phase 14 is disposed interstitially between bonded together diamond grains and comprises a reaction product of a preselected material with the diamond that functions to bond the diamond grains together. Accordingly, the material microstructurc of this region comprises a distribution of both intercrystalline bonded diamond, and diamond grains that are bonded together by reaction with the preselected bonding agent.

Diamond grains useful for forming thermally stable diamond bonded materials of this invention include synthetic diamond powders having an average diameter grain size in the range of from submicrometer in size to 100 micrometers, and more preferably in the range of from about 5 to 80 micrometers. The diamond powder can contain grains having a mono or multi-modal size distribution. In an example embodiment, the diamond powder has an average particle grain sized of approximately 20 micrometers. In the event that diamond powders are used having differently sized grains, the diamond grains are mixed together by conventional process, such as by ball or attrittor milling for as much time as necessary to ensure good uniform distribution.

The diamond grain powder is preferably cleaned, to enhance the sinterability of the powder by treatment at high temperature, in a vacuum or reducing atmosphere. The diamond powder mixture is loaded into a desired container for placement within a suitable HPHT consolidation and sintering device. In an example embodiment where the diamond bonded body is to be attached to 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 and includes a metal solvent catalyst that is capable of infiltrating into the adjacent diamond powder mixture during processing. Suitable metal solvent catalyst materials include those metals selected from Group VIII elements of the Periodic table. A particularly preferred metal solvent catalyst is cobalt (Co).

The substrate material can be selected from the group of materials conventionally used as substrate materials for forming conventional PCD compacts. In a preferred embodiment, the substrate material comprises cemented tungsten carbide (WC-Co).

It is desired that a predetermined region of the diamond bonded body formed during the consolidation and sintering process become thermally stable. It is further desired that a predetermined region of the diamond body formed during the same process also form a desired attachment with the substrate. In an example embodiment, the predetermined region to become thermally stable is one that will form the wear or cutting surface of the final product.

In a first invention embodiment, a suitable first or initial stage infiltrant is disposed adjacent a surface portion of the predetermined region of the diamond powder to become thermally stable. The first infiltrant can be selected from those materials having a melting temperature that is below the melting temperature of the metal solvent catalyst in the substrate, that are capable of infiltrating the diamond powder mixture upon melting during processing, and that are capable of bonding together the diamond grains. In an example embodiment, the first infiltrant actually participates in the bonding process, forming a reaction product that bonds the diamond grains together.

In a preferred first embodiment, the first infiltrant is a silicon material that is provided in a form suitable for placement and use within the consolidation and sintering device. In an example embodiment, the silicon material can be provided in the fonn of a silicon metal foil or powder, or in the form of a compacted green powder. The first infiltrant is positioned within the device adjacent the surface of the predetermined region of the diamond powder to become thermally stable. In an example embodiment, the first infiltrant is positioned adjacent the diamond powder during assembly of the container prior to its placement into the HPI-IT consolidation and sintering device.

The device is then activated to subject the container to a desired HPHT condition to effect consolidation and sintering. In an example embodiment, the device is controlled so that the container is subjected to a HPHT process where the applied pressure and temperature is first held at a suitable intermediate level for a period of time sufficient to melt the first infiltrant, c.g., a silicon material, and allow the first infiltrant to infiltrate into the diamond powder mixture and react with and bond together the diamond grains. In such example embodiment, the intermediate level can be at a pressure of approximately 5500 MPa, and at a temperature of from 1l50°C to l300°C. It is to be understood that the particular intermediate pressure and temperatures presented above are based on using a silicon metal first infiltrant and a specific type and volume of diamond powder. Accordingly, pressures and/or temperatures other than those noted above may be useful for other types of infiltrants and/or other types and Volumes of diamond powder.

The use of temperatures below this range may not be well suited for the intermediate level, when silicon metal is chosen as the first infiltrant, because at lower temperatures the silicon metal may not melt, and thus not infiltrate into the diamond mixture as desired. Using a temperature above this range may not be desired for the intermediate level because, although the first infiltrant will melt and infiltrate into the diamond powder mixture, such higher temperature may also cause a second stage infiltrant, ie, the metal solvent catalyst in the substrate (e.g., cobalt), to melt and infiltrate the diamond grains at the same time.

Infiltration of the metal solvent catalyst prior to or at the same time as infiltration of the first infiltrant, e. g., silicon metal, is not desired because it can initiate unwanted conventional diamond sintering throughout the diamond body. Such conventional diamond sintering operates to inhibit infiltration into the diamond mixture by the first stage infiltrant, thereby preventing reaction of the first infiltrant with the diamond grains to preclude fomiation of the desired thermally stable diamond region.

I)uring this intennediate stage of processing, the first infiltrant melts and infiltrates into the adjacent surface of the diamond mixture. In the case where the first infiltrant is a silicon metal, it then reacts with the diamond grains to form silicon carbide (SiC) between the diamond particles in the adjacent region of the compact. In such example embodiment, where silicon is provided as the selected first infiltrant, it is desired that the intermediate level of processing be held for a period of time of from 2 to 20 minutes. This time period must be sufficient to melt all of the silicon, allow the melted silicon to infiltrate the diamond powder, and allow the infiltrated silicon to react with the diamond to fonn the desired SiC, thereby bonding the diamond particles together. It is desired that substantially all of the silicon infiltrant be reacted, as silicon metal is known to be brittle and any residual unreacted silicon metal in the diamond can have a deleterious effect on the final properties of the resulting thermally stable diamond bonded compact.

While particular intennediate level pressures, temperatures and times have been provided, it is to be understood that one or more of these process variables may change depending on such factors as the type and amount of infiltrant and/or diamond powder that is selected. A key point, however, is that the temperature for the intermediate level be below the melting temperature of the second stage infiltrant, ie., the metal solvent catalyst in the substrate, to permit the first stage infiltrant to infiltrate and react with the diamond powder prior to melting and infiltration of the metal solvent catalyst.

In an example embodiment, where the thermally stable diamond bonded compact being fomied according to this invention will be embodied as a diamond cutter, the first infiltrant is provided in the form of a silicon metal foil that is positioned adjacent what will be a working or cutting surface of the to—be-fonned diamond bonded body, and the silicon infiltrates the diamond body a desired depth from the working surface, thereby providing a desired thermally stable diamond bonded region extending the desired depth from the working surface. In such example embodiment, the silicon may infiltrate the diamond powder a depth from the working surface of from 1 to 1,000 micrometers, and preferably at least 10 micrometers. In an example embodiment, the silicon may infiltrate the diamond powder a depth from the working surface of from about 20 to 500 micrometers.

A key feature of thermally stable diamond bonded materials and compacts of this invention is that the thermally stable region of the diamond body is formed in a single process step without the presence or assistance of a conventional metal solvent catalyst, such as cobalt, and without the need for subsequent processing to remove the metal solvent catalyst. Rather, the thermally stable region is formed by the infiltration and reaction of a first stage infiltrant, such as silicon, into the diamond powder during H PHT processing to produce a bonded reaction product between the diamond grains.

After the desired time has passed during the intermediate level, the consolidation and sintering process is continued by increasing the temperature to a range of from about l350°C to 1500°C. The pressure for this secondary processing step is preferably maintained at the same level as noted above for the intermediate level. At this temperature, the second stage infiltrant in the fomi of the metal solvent catalyst component in the substrate melts and infiltrates into an adjacent region of the diamond powder mixture, thereby sintering the adjacent diamond grains in this region by conventional method to form conventional PCD in this region, and forming a desired attachment or bond between the PCD region of the diamond bonded body and the substrate.

While a particular temperature range for this secondary phase of processing has been provided, it is to be understood that such secondary processing temperature can and will vary depending on such factors as the type and/or amount of metal solvent catalyst used in the substrate, as well as the type and/or amount of diamond powder used to form the diamond bonded body.

In the example embodiment discussed above, where the diamond bonded compact is configured for use as a cutter, the region of the compact body that is secondarily infiltrated with the metal solvent catalyst component from the substrate is positioned adjacent a surface of the diamond mixture opposite from the working surface, and it is desired that the metal solvent catalyst infiltration depth be sufficient to provide a secure bonded attachment between the substrate and diamond bonded body.

During this secondary or final phase of the HPHT processing, the metal solvent catalyst, e,g., cobalt, infiltrates between the diamond grains in the region of the diamond powder adjacent the substrate to provide highly localized catalysis for the rapid creation of strong bonds between the diamond grains or crystals, i.e., producing intercrystalline bonded diamond or conventional PCD. As these bonds are formed, the cobalt moves into and remains disposed within interstitial regions between the intercrystalline bonded diamond.

While there may be some possibility that, during this secondary phase of processing, the metal solvent catalyst from the substrate may infiltrate into the diamond powder to a point where it passes into the thermally stable region of the diamond bonded body, there is no indication that reactions between the metal solvent catalyst and any unreacted infiltrant, e.g., silicon, or reactions between the metal solvent catalyst and the infiltrant reaction product, e.g., silicon carbide, takes place or if it does has had any deleterious effect on the final properties of the diamond bonded body.

As noted above, when the first stage infiltrant selected for fonning the thermal stable diamond region is silicon, the infiltrated silicone forms a reaction phase with the diamond grains, crystals or particles in the diamond bonded phase according to the reaction: Si + C = SiC This reaction between silicon and carbon present in the diamond grains, crystals or particles is desired as the reaction product; namely, silicon carbide is a ceramic material that has a coefficient of thermal expansion that is similar to diamond. At the interface within the diamond bonded body between the thermally stable diamond bonded region and the PCD region, where both cobalt and silicon carbide may be present, reactions such as the following may take place: Co + 2SiC = CoSi; + 2C, lhis, however, is not a concern and may be advantageous as CoSi2 is also known to be a thennally stable compound.

Additionally, if the Co and SiC do not end up reacting together at the boundary or interface between the two regions, the presence of the silicon carbide adjacent the PCD region operates to minimize or dilute the otherwise large difference in the coefficient of thermal expansion that would otherwise exist between the intercrystalline diamond and the cobalt phases in PCD region.

Thus, the formation of silicon carbide within the silicon-infiltrated region of the diamond bonded body operates to minimize the development of thennal stress in that region and at the boundary between the Si and Co infiltrated regions, thereby improving the overall thermal stability of the entire diamond bonded body.

As noted above, the first stage infiltrant operates to provide a thermally stable diamond bonded region through the fonnation of a reaction product that actually forms a bond with diamond crystals. While a certain amount of diamond—to-diamond bonding can also occur within this thermally stable diamond region without the benefit of the second stage solvent—catalyst infiltrant, it is theorized that such direct diamond—to-diamond bonding represents a minority of the diamond bonding that occurs in this region. In an example embodiment, where the first stage infrltrant being used is silicon, it is believed that greater than about 75 percent, and more preferably 85 percent or more, ofthe diamond bonding occurring in the thennally stable region is provided by reaction of the diamond grains or particles with the first stage infiltrant.

While ideally, it is desired that all of the diamond bonding in the thermally stable region be provided by reaction with the first stage infiltrant, any amount of diamond-to-diamond bonding occurring in the themially stable region occurs without the presence or use of a metal solvent catalyst, thus the resulting diamond bonded region is one having a degree of thermal stability that is superior to conventional PCD.

It is to be understood that the amount of the first stage infrltrant used during processing can and will vary depending on such factors as the size of the diamond grains that are used, the volume of diamond grains and region/volume of desired thermal stability, the amount and/or type of the first stage infiltrant material itself, in addition to the particular application for the resulting diamond bonded compact. Additionally, the amount of the first stage infiltrant used must be precisely determined for the purpose of infiltrating and reacting with a desired volume of the diamond powder to provide a desired thermally stable diamond region, e.g., a desired thermally stable diamond depth.

For example, using an excessive amount of the first stage infiltrant, e.g., silicon, to react with the diamond powder during intermediate stage processing can result in excess infiltrant being present during secondary or final processing when the second stage metal solvent catalyst infrltrant e.g., cobalt, in the substrates melts, infiltrates, and facilitates conventional diamond sintering adjacent the substrate. Excess first stage infiltrant present during this secondary phase of processing can remain unreacted as a brittle silicon phase or can react with the metal solvent catalyst material to form cobalt disilicide (CoSiz) at the boundary between the two regions.

In addition to silicon, the thermally stable region of first embodiment diamond bonded materials and compacts of this invention can be fomied from other types of first stage materials. Such materials must be capable of melting or of reacting with diamond in the solid state during processing of the diamond bonded materials at a temperature that is below the melting temperature of the metal solvent catalyst component in the metallic substrate. Additionally, such first stage material must, upon reacting with the diamond, form a compound having a coefficient of thermal expansion that is relatively closer to that of diamond than that of the metal solvent catalyst.

It is also desired that the compound fonned by reaction with diamond be capable of bonding with the diamond and must possess significantly high-strength characteristics.

In an example embodiment, the source of silicon that is used for initial infiltration is provided in the form of a silicon metal disk. As noted above, the amount of silicon that is used can influence the depth of infiltration as well as the resulting types of silicon compounds that can be fonned. In an example embodiment, where the volume of the diamond bonded body to become thennally stable is within the range of from about 50 to 400 cubic mm, it is desired that the amount of silicon infiltrant be in the range of from about l0 to 80 milligrams. In a preferred embodiment, where the desired silicon infiltration volume is approximately 100 cubic mm, the amount of silicon infiltrant to be used is approximately 23 milligrams.

A second embodiment thermally stable diamond bonded compact of this invention can be formed by mixing diamond powder together with a preselected material capable of participating in solid state reactions with the diamond powder. 'lhus, unlike the first embodiment described above, the preselected materials useful for forming the thermally stable region in this second embodiment is provided in situ with the diamond powder and is not positioned adjacent a surface of the diamond powder as an initial infiltrant.

Suitable preselected materials useful for forming second embodiment thermally stable diamond bonded compacts include those compounds or materials capable of forming a bond with the diamond grains, have a coefficient of thermal expansion that is relatively closer to that of the diamond grains than that of a conventional metal solvent catalyst, that is capable of reacting with the diamond at a temperature that is below that of the melting temperature of the metal solvent catalyst contained in the substrate, and that is capable of fonning an attachment with an adjacent diamond region in the diamond body.

Example preselected materials useful for fonning the second invention embodiment include ceramic materials such as TiC, A1203, Si3N4 and the like. These ceramic materials are known to bond with the diamond grains to form a diamond~ceramic microstructure. In an example embodiment, the volume percent of diamond grains in this mixture is in the range of from about 50 to volume percent. Again, a key feature of this second embodiment of the invention is the ability to form both a thermally stable diamond region and a conventional PCD region in the diamond body during a single HPHT process.

Since the preselected material used to bond the diamond grains together in this second embodiment is mixed together with the diamond grains, the solid state reaction of these materials during HPHT processing operates to form thermally stable diamond within the entire region of the diamond body that was formally occupied by the diamond mixture. In other words, conventional PCD is not fomied within this region.

To accommodate attachment of a desired substrate to the thermally stable region of the diamond body, second embodiments of this invention further include use of a green-state diamond grain material disposed adjacent the diamond grain mixture. The green-state diamond grain material may or may not include a metal solvent catalyst. Additionally the green—state diamond grain material can be provided in the form of a single layer of material or in the form of multiple layers of materials. Each layer may include the same or different diamond grain size, diamond volume, and may or may not include the use of a solvent catalyst. In an example embodiment, the green-state diamond grain material can be provided in the form of one or more layers of conventional diamond tape.

Thus, second embodiment thermally stable diamond compacts of this invention are formed by mixing together diamond grains, as described above, with the desired preselected material for reacting with the diamond grains as noted above. The mixture can be cleaned in the manner noted above and loaded into a desired container for placement within the HPHT device. The green- state diamond graincontaining material is positioned adjacent the mixture. In an example embodiment where the diamond bonded body is to be attached to a substrate, a substrate material as noted above is positioned adjacent the green-state diamond grain-containing material.

The container is placed in the HPHT device and the device is activated to affect consolidation and sintering. Like the process described above of forming the first invention embodiment, the device is controlled so that the container and its contents is subjected to a IIPHT condition wherein the pressure and/or temperature is first held at a suitable intermediate level for a period of time sufiicient to cause the desired solid state reaction to occur within the mixture of diamond grains and the preselected material. Subsequently, the HPHT condition is changed to a different pressure and/or temperature. At this subsequent HPHT condition, any solvent catalyst in the green-state diamond grain material melts and facilitates diamond-diamond bonding to form conventional PCD within this region. Also, the two adjacent diamond regions will become attached to one another, and the solvent catalyst in the substrate will melt and infiltrate the adjacent green« state material to form a desired attachment or bond between the PCD region of the diamond body and the substrate.

In this second embodiment, the intermediate HPHT process conditions are such that will cause the diamond grains and preselected material mixture to undergo solid state reactions to fomr a thermally stable diamond-ceramic phase. The specific pressure and temperature for this intermediate HPHT condition can and will vary depending on the particular nature of the preselected material that is used to react with the diamond grains. Again, a key processing point here is that the temperature at this intermediate HPHT condition be below the melting point of any solvent catalyst present in the adjacent green—state diamond material, and present in the substrate, to ensure formation of the thermally stable diamond region prior to the melting and infiltration of the solvent catalyst.

In an example embodiment where the preselected material is A1203, and the diamond powder used is the same as that described above for the first invention embodiment, the intermediate HPHT process can be conducted at a pressure of approximately 5500 MPa, and at a temperature of from l250°C to l300°C. The intermediate level of HPHT processing can be held for a period of time of from about 10 to 60 minutes to facilitate plastic deformation and filling of the voids between the diamond grains by the ceramic powder and initiation of solid state reactions of the ceramic with the diamond particles. Again, it is to be understood that the intermediate HPHT conditions provided above are based on using A1203 as the preselected material and a specific size and volume of diamond powder. Accordingly, pressure and/or temperatures other than those noted above may be useful for other types of preselected materials and/or other types and/or volumes of diamond powder.

Once the intermediate level HPHT processing has been completed, the HPHT process is changed to facilitate further consolidation and sintering by increasing the temperature to a point where any solvent catalyst present in the green-state material region, and the solvent catalyst in the substrate, melts. When the solvent catalyst is cobalt, the temperature is increased to about 1350°C to l500°C. The pressure at this subsequent HPHT process condition is maintained at the same level as noted above for the intermediate HPHT process condition.

As noted above, at this temperature all or a portion of the green-state diamond material becomes PCD. In the event that the green-state diamond material itself includes a solvent catalyst, then the entire region occupied by the green-state diamond becomes PCD. If the green-stale ... . _...... . .rr

Claims (16)

1. Claims I. A thermally stable diamond bonded compact comprising: a diamond bonded body comprising; a thermally stable region extending a distance below a diamond bonded body surface, the thermally stable region having a material microstructure comprising a plurality ofdiamond grains bonded together by a reaction product of the diamond grains and a reactant; a polycrystalline diamond region extending a depth from the thermally stable region and having a material microstructure comprising intererystalline bonded together diamond grains and a metal solvent catalyst disposed within interstitial regions between the intercrystalline bonded together diamond grains; and a metallic substrate attached to the polycrystalline diamond region; wherein the reactant is selected from the group of materials capable of reacting with the diamond at a temperature below the melting temperature ofthe metal solvent catalyst.

2. The compact as recited in claim 1 wherein the thermally stable region is substantially free of a metal solvent catalyst used to form the polycrystalline diamond region.

3. The compact as recited in claim 1 wherein the reaction product has a coefficient ofthermal expansion that is closer to the intercrystalline bonded diamond than to the metal solvent catalyst.

4. The compact as recited in claim 1 wherein the reactant has a melting temperature that is below the melting temperature ofthe metal solvent catalyst.

5. The compact as recited in claim 1 wherein the thermally stable region extends a depth below the diamond bonded body surface of from about 20 to 500 micrometers. 23

6. The compact as recited in claim 1 wherein greater than about 75 percent of the diamonds bonded in the thermally stable region are bonded together by the reaction product of the diamond grains and the reactant. 5

7. The compact as recited in claim 1 wherein the reactant comprises silicon.

8. A method for making a thermally stable diamond bonded compact comprising a diamond bonded body attached to a substrate, the method comprising the steps of: combining a volume ofdiamond grains to form a mixture; 10 placing a first infiltrant material adjacent a portion of the mixture; placing a metallic substrate adjacent another portion of the mixture; infiltrating a first region of the mixture at a first temperature and pressure condition, wherein during the first temperature and pressure condition the first intiltrant reacts with and bonds together the diamond grains to form a thermally stable diamond bonded region ofthe diamond l5 bonded body; infiltrating a second region ofthe mixture at a second temperature condition that is higher than the first temperature condition, wherein during the second temperature condition a second intiltrant provided from the metallic substrate melts and infiltrates the second region to form a polycrystalline diamond region of the diamond bonded body, wherein the first and second regions are 20 bonded together; and forming an attachment between the polycrystalline diamond region of the diamond bonded body and the substrate during the step of forming the polycrystalline diamond region.

9. The method as recited in claim 8 wherein during the step ofinfiltrating the 25 second region, the second infiltrant is a metal solvent catalyst. l().

10. The method as recited in claim 8 wherein during the process of infiltrating the second region, the second infiltrant is disposed within interstitial regions between intercrystalline bonded together diamond grains present in the polycrystalline diamond region, and wherein the 30 reaction product formed between the diamond gains and the first infiltrant in the thermally stable region has a coellicient ofthermal expansion that is closer to the intercrystalline bonded together diamond than to the second infiltrant.

11. l l. The method as recited in claim 8, wherein the first infiltrant has a melting temperature that is lower than that of the second infiltrant.

12. I2. The method as recited in claim 8 wherein the mixture is substantially free of metal solvent catalyst.

13. l3. The method as recited in claim 8 wherein the steps of infiltrating the lirst region and infiltrating the second region are conducted at the same pressure condition.

14. The method as recited in claim 8 wherein the volume ofdiamond used to form the thermally stable diamond bonded region is from about 50 to 400 cubic millimeters. and the amount of the lirst inliltrant is from about l0 to 80 milligrams.

15. The method as recited in claim 8 wherein the first infiltrant comprises silicon.

l6. The method as recited in claim 8 wherein the steps of infiltrating take place within a high pressure/high temperature device, and wherein during the steps of infiltrating, the mixture is not removed from the device. TOMKINS & CO.