Patent Application
20180009716
The present disclosure relates to a ceramic-bonded diamond composite. More specifically, the present disclosure relates to methods of production of ceramic-bonded diamond composites composed of diamond, silicon carbide and silicon that are friable to form diamond composite particles as well as to the diamond particles, per se. Uses for such diamond composite particles include wear applications, such as grinding, cutting and dicing.
In the discussion that follows, reference is made to certain structures and/or methods. However, the following references should not be construed as an admission that these structures and/or methods constitute prior art. Applicant expressly reserves the right to demonstrate that such structures and/or methods do not qualify as prior art against the present invention.
Solid compacts comprised of diamond crystals bonded by refractory carbide or metallic phases, such as silicon carbide (SiC), are known, for example, from U.S. Pat. Nos. 4,874,398; 4,948,388; 4,985,051; 5,010,043; 5,106,393, and WO 99/12867, each of which are incorporated by reference herein in their entireties. Generally, such material is formed into a densified compact (or blank). However, the densified compact (or blank) is difficult to mechanically process, including mechanically breaking into particulate form, and the densified compact is typically either formed near net shape (see U.S. Patent Application Publication 2013/0167447, which is incorporated by reference herein in its entirety) or, if necessary, is further formed into a product shape by, for example, a cutting process, such as Electrical Discharge Machining (EDM).
Typical uses and products for these conventional compacts include dressing and truing grinding wheels; die blanks, for example, for wire stranding, bunching and compacting applications; wear parts and nozzles; and high pressure research anvils and backing plates. In general as well as in the above applications, the ceramic-bonded diamond composites are formed as a densified compact, the characteristics of which inherently limits its applications and minimizes or prevents the wear and abrasive properties of the ceramic-bonded diamond composites from being utilized in particulate form.
There is a need for an improved composite diamond material that is both friable into particulate form as well as high performing when incorporated into wear and abrasive applications. If ceramic-bonded diamond composites could be formed in particulate form rather than in a densified compact form, then numerous uses could be realized including, for example, uses as a particle embedded in a matrix or on a surface to impart abrasive and wear related properties, such as to a cutting apparatus, dicing blade, grinding wheel, saw blades and so forth.
An exemplary method to produce a ceramic-bonded diamond composite particle includes forming a diamond feedstock including a plurality of diamond grains and silicon particles and subjecting the diamond feedstock to at least one pre-consolidation process to form a granule. The method also includes forming a densified compact in a consolidation process using the granule, where the densified compact including ceramic-bonded diamond composite material, and mechanically processing the densified compact in a post-consolidation process in which a plurality of ceramic-bonded diamond composite particles are formed. The ceramic-bonded diamond composite particles include a plurality of diamond grains and silicon carbide reaction bonded to the diamond grains. A composition of the ceramic-bonded diamond composite particle includes 60-90 wt. %, preferably 70-90 wt. %, more preferably 79-81 wt. %, more preferably 80 wt. % diamond, 10-40 wt. % silicon carbide, ≦2 wt. % silicon.
Another exemplary method to produce a ceramic-bonded diamond composite particle includes forming a diamond feedstock including a plurality of diamond particles and silicon particles, mixing the diamond feedstock with a binder and a solvent to form a slurry, spraying the slurry into liquid nitrogen to form a plurality of frozen granules followed by freeze drying the frozen granule to remove the solvent from the granule or spraying the slurry into a heated chamber to remove volatile components, and heating the granule in an inert or reducing atmosphere to remove the binder from the granule. The method also includes sintering the porous granule in an inert or reducing atmosphere to form a grit of ceramic-bonded diamond composite material and mechanically processing the grit to form a plurality of ceramic-bonded diamond composite particles. The ceramic-bonded diamond composite particles include a plurality of diamond particles and silicon carbide reaction bonded to the diamond particles. A composition of the ceramic-bonded diamond composite particle includes 60-90 wt. %, preferably 70-90, more preferably 79-81 wt. %, more preferably 80 wt. % diamond, 10-40 wt. % silicon carbide, ≦2 wt. % silicon.
A further exemplary method to produce a ceramic-bonded diamond composite particle includes forming a diamond feedstock including a plurality of diamond grains and silicon particles and particles of inert material, subjecting the diamond feedstock to a consolidation process that forms a densified compact including ceramic-bonded diamond composite material from the diamond feedstock, subjecting the densified compact to a post-consolidation process in which the densified compact is mechanically processed to form a plurality of ceramic-bonded diamond composite particles, and separating particles of inert material from the plurality of ceramic-bonded diamond composite particles. The ceramic-bonded diamond composite particles include a plurality of diamond grains and silicon carbide reaction bonded to the diamond grains and a composition of the ceramic-bonded diamond composite particle includes 60-90 wt. %, preferably 79-81 wt. %, more preferably 80 wt. % diamond, 10-40 wt. % silicon carbide, ≦2 wt. % silicon. The ceramic-bonded diamond composite particle has a mesh size of 40/50 to 400/500 and a toughness index of 40 to 100.
An exemplary embodiment of a ceramic-bonded diamond composite particle include a plurality of diamond grains and silicon carbide reaction bonded to the diamond grains. A composition of the ceramic-bonded diamond composite particle includes 70-90 wt. %, preferably 79-81 wt. %, more preferably 80 wt. % diamond, 10-30 wt. % silicon carbide, ≦2 wt. % silicon.
Another exemplary embodiment of a ceramic-bonded diamond composite particle includes a plurality of ceramic-bonded diamond particles and an inert material. The ceramic-bonded diamond composite includes a plurality of diamond grains and silicon carbide reaction bonded to the diamond grains. A composition of the ceramic-bonded diamond composite is 70-90 wt. %, preferably 79-81 wt. %, more preferably 80 wt. % diamond, 10-30 wt. % silicon carbide, ≦2 wt. % silicon.
The following detailed description of preferred embodiments can be read in connection with the accompanying drawings in which like numerals designate like elements and in which:
Articles and methods of the present disclosure are directed to ceramic-bonded diamond composite particles that exhibit desirable properties. The ceramic-bonded diamond composite particles may exhibit relatively high levels of diamond content, which may contribute to the properties of the composite particles. Methods to produce a ceramic-bonded diamond composite particle according to the present disclosure include forming a diamond feedstock having a plurality of diamond grains and silicon particles and subjecting the diamond feedstock to at least one pre-consolidation process to form a granule. The granule is subjected to a consolidation process to form a densified compact. In one embodiment, the consolidation process includes a high pressure high temperature process. The resulting densified compact forms a ceramic-bonded diamond composite material. The methods also include mechanically processing the densified compact in a post-consolidation process in which a plurality of ceramic-bonded diamond composite particles are formed. The ceramic-bonded diamond composite particles include a plurality of diamond grains and silicon carbide reaction bonded to the diamond grains. A composition of the ceramic-bonded diamond composite particle includes 60-90 wt. %, preferably 70-90 wt. %, more preferably 79-81 wt. %, more preferably 80 wt. % diamond, 10-40 wt. % silicon carbide, ≦2 wt. % silicon.
The ceramic-bonded diamond composite particle 10 comprises a plurality of diamond particles bonded together by silicon carbide. Mapping of a composite particle with Energy-Dispersive X-ray spectroscopy (EDX) is shown in
In exemplary embodiments, the composition of the ceramic-bonded diamond composite particle 10 is 80 weight % (wt. %) diamond, 19 wt. % silicon carbide and 1 wt % silicon. Silicon outside the silicon carbide is present in residual amounts remaining from the manufacturing process. The constituents of the ceramic-bonded diamond composite particle 10 can be present in other suitable amounts within the following ranges: 60-90 wt. %, alternatively 70-90 wt. %, alternatively 75-90 wt. %, alternatively 79-81 wt. % or 80 wt. % diamond; 10-40 wt. % silicon carbide, alternatively ≧12 wt. % or ≧15 wt % to ≦20 wt. % or ≦25 wt. % silicon carbide; and ≦3 wt. % silicon, alternatively >0 wt. % or ≧1 wt % to ≦1 wt. % or ≦2 wt. % silicon. An exemplary composition has 85-90 wt. % diamond; 10-15 wt. % silicon carbide, and ≦2 wt. % silicon. The composition of the ceramic-bonded diamond composite can be determined by any suitable means. However, in this disclosure the compositions of ceramic-bonded diamond composite particles were determined by X-ray diffraction techniques using a Brucker AXS D8 Focus diffractometer using Cu k-alpha radiation and running Jade v.9.3.2 software, “Easy Quantitative” analysis method. The ceramic-bonded diamond composite particle 10 has a particle size (based on D50) of from 40 microns to 1000 microns.
The diamond particles can be any suitable diamond particle that is of sufficiently small size that it will mix with the other constituent raw materials prior to forming the ceramic-bonded diamond composite particle. Diamond size is measured using a Microtrac S3500 particle size analyzer running software version 10.6.2 and are reported using volume averaging. Typical sizes of the diamond particles range from 200 microns or less to 1 micron or less (based on D50). In an alternative embodiment, the diamond particles can have a bimodal size distribution. As an example, the diamond particles can have a bimodal size distribution with a first fraction having a D50 of 5 microns and a second faction having an D50 of 20 microns. Other size distributions such as tri-modal may also be used. Once the ceramic-bonded diamond composite particle is formed, the sizes of the diamond particles and any size distribution present in the raw materials are generally preserved in the formed ceramic-bonded diamond composite particle, but with a slight reduction in sizes and shift to smaller size distributions possible due to consumption of diamond and crushing that occurs in the manufacturing process.
An example of a suitable diamond grain is monocrystalline or polycrystalline diamond, i.e., diamond grains having a D50 of 100 microns or less. Another example of a suitable diamond is pitted diamond, i.e., diamond grains having a D50 of 100 microns or less, and containing more surface cutting points than a typical monocrystalline micron and polycrystalline diamond. The surface treatment in pitted diamond increases the surface area as compared to that in the untreated monocrystalline or polycrystalline diamond. Pitted diamond has increased cutting points that contribute to aggressive cutting properties. Furthermore, the higher surface area of pitted diamonds, if preserved through subsequent manufacturing, e.g., HPHT processing, may contribute to increased bonding between diamond and silicon carbide in the ceramic-bonded diamond composite particle. An example of a suitable pitted diamond is disclosed in U.S. Pat. No. 8,182,562, the entire contents of which are incorporated herein by reference, and pitted diamond is commercially available from Diamond Innovations under the trade name HYPERION™.
The ceramic-bonded diamond composite particle disclosed herein can be produced by various methods. In general, the ceramic-bonded diamond composite particle is formed by a method that includes forming a diamond feedstock, processing the diamond feedstock in a consolidation process and, optionally, one or more pre- or post-consolidation processes.
Forming the diamond feedstock includes preparing a mixture of the raw material of the ceramic-bonded diamond composite particle. In general, the diamond feedstock includes diamond particles, silicon particles and optional inert materials.
The above diamond feedstock can be used directly or can be further processed prior to introduction to the consolidation process.
An example of a consolidation process is a high pressure high temperature (HPHT) process in which a pressure of about 2000-7500 MPa and a temperature of about 800-1600° C. are maintained for time periods typically not exceeding 30 minutes. During this period, a reaction bonding process occurs in which the silicon reacts with the diamond to form silicon carbide between diamond particles. The silicon carbide acts as a reactive bond and is the structure that holds the ceramic-bonded diamond composite particle together. HPHT processes yield a densified compact with densities greater than 95% and typically approaching 100%. Other details and suitable HPHT processes are disclosed in U.S. Pat. Nos. 3,141,746; 3,745,623; 3,609,818; 3,850,591; 4,394,170; 4,403,015; 4,797,326 and 4,954,139, the entire contents of each are incorporated herein by reference.
Another example of a consolidation process is sintering at 1300-1600° C., alternatively about 1500° C., in a controlled atmosphere. Controlled atmosphere for sintering in these consolidation processes are typically an inert or reducing atmosphere, such as argon, hydrogen, nitrogen, or a mixture of argon, hydrogen and/or nitrogen or a vacuum. During sintering, the diamond particles and silicon particles from the feedstock undergo a reaction bond to form silicon carbide between diamond particles. The silicon carbide acts as a reactive bond and is the structure that holds the ceramic-bonded diamond composite particle together. Because sintering is typically done at pressures much lower than that in HPHT processes, sintering does not result in the same degree of densification as observed in HPHT processes, with typical densification of sintered material being on the order of 50-75%, alternatively about 65%.
The consolidation process can be accompanied by one or more pre- or post-consolidation processes. For example, a pre-consolidation process can incorporate pressing, such as cold isostatic pressing, to form a green body of an initial densification that is then subject to the consolidation process. In exemplary embodiments, cold isostatic pressing achieves an initial densification of approximately 50-75%, alternatively at least 65%. In another example, a debinding process can be included either with the consolidation process or as a separate pre-consolidation process. Non-limiting examples of pre- and post-consolidation processes include coating with inert materials, metal alloys or compounds; secondary heating processes to pre-densify and/or improve the strength of green bodies; freezing particles; and removing water or volatile components from particles, for example in a freeze-drying process or spray drying process.
Also in general, the ceramic-bonded diamond composite particle is formed by a method that may optionally include an additive or a processing step that reduces the number and extent of diamond to silicon carbide bonding that occurs in the consolidation process. For example, an inert material can be included in the raw material, i.e., diamond particle and silicon particle mixture, prior to consolidation to reduce the extent of reaction bonding occurring in the consolidation process by displacing reactive material with inert material. In another example, an inert or active material can be partially coated on the granules of the raw material prior to the consolidation process to inhibit or prevent reaction bonding that would otherwise occur in the consolidation process. In a further example, a binder, such as polyethylene glycol (PEG), can be incorporated into the process and can assist with formation of green bodies formed by pressing techniques.
Examples of inert materials that can be used, alone or in combination, in the disclosed methods include oxides, carbides, nitrides, aluminates, silicates, nitrates, carbonates, silica (quartz) sand and cubic boron nitride (cBN). Specific examples of inert material include Al2O3, SiO2, and SiC. When an inert material is used, the inert material has a D50 in the range of approximately 1 to 50 microns and is present in an amount of up to 10 weight percent (wt. %), alternatively 5 to 10 wt. %. It is presently believed that the inert material reduces the number and extent of reaction bonding in the densified compact. It is contemplated that the reduced network of reaction bonds results in the densified compact being friable into a plurality of ceramic-bonded diamond composite particles and having a reduced transverse rupture strength relative to a densified compact made without or below a threshold amount of inert material.
As a SiC bonded material, other active materials that form carbides can be used in addition to or in place of silicon in the ceramic bonded diamond composite. Examples of active materials include carbide forming metals such as Ti, Zr, and Cr. The addition of these active materials can result in the formation of active metal carbides other than SiC. These other carbides (TiC, ZrC, Cr2C3) can provide some binding effect but may be a lower strength bond than SiC, therefore reducing the strength of the densified compact. Active materials may be added in amounts preferably between 0 and 25% by weight. One or more of these active materials can be used.
The raw materials for the diamond feedstock can include any of the diamond material disclosed herein, including monocrystalline diamond, polycrystalline diamond, pitted diamond and combinations thereof, and silicon particles and optional silicon nitride, aluminum nitride, hexagonal boron nitride (hBN) and inert materials. Proportions of the constituents of the raw materials can be varied as variously disclosed herein to achieve a desired composition of the ceramic-bonded diamond composite particle to be produced.
Because the densified compact produced in step 120 is without inert filler materials, it has a density approaching 100% and a transverse rupture strength of over 900 MPa, mechanical processing, for example by mechanically breaking, is initially not desirable. Rather, the densified compact is first cut, for example by EDM, into smaller pieces prior to mechanical processing. Additionally or alternatively, excess material formed during the manufacture of products from densified compacts can be included with or be the sole source of densified compact comprising ceramic-bonded diamond composite material that is processed in the step of mechanically processing 130. Non-limiting examples of techniques to mechanically process the densified compact to a desired D50 size include grinding, roller milling, roll compaction milling, hammer milling, cutting, compact milling, jet milling and ball milling. Typical desired particle sizes (based on D50) range from 20 to 100 microns (μm), alternatively ≧25 μm or ≧30 μm or ≧50 μm to ≦40 μm or ≦50 μm or ≦70 μm or ≦80 μm.
The raw materials for the diamond feedstock can include any of the diamond material disclosed herein, including monocrystalline diamond, polycrystalline diamond, pitted diamond and combinations thereof, silicon particles and optional particles of silicon nitride and inert materials, such as any of the inert materials disclosed herein including, in a specific example, 5 to 10 wt. % of one or more of sand, Al2O3, SiO2 and SiC, where the inert material has a D50 of 1 to 50 microns. Proportions of the constituents of the raw materials can be varied as variously disclosed herein to achieve a desired composition of the ceramic-bonded diamond composite particle to be produced.
In contrast to the densified compact produced in the method 100 illustrated in
In the granulation steps 310 to 330, a slurry is formed and processed to form granule. The raw materials for the slurry can include any of the diamond material disclosed herein, including monocrystalline diamond, polycrystalline diamond, pitted diamond and combinations thereof, silicon particles, a solvent, and a binder. The binder can be any suitable binder that promotes the flow characteristics or spray characteristics suitable for the further processing steps while also being useful to promote sintering and green body formation as those alternative processes will be applied in the method. For example, a suitable binder can be selected from the group consisting of polyethylene glycol (PEG), polyvinyl alcohol (PVA), and paraffin wax and others. The solvent may be water, ethanol, acetone, or others chosen for compatibility with different binders and slurry processing systems. An example slurry composition includes, by weight, 66% diamond particles, 7.3% silicon powder, 1.5% PVA 4-88, 0.5% PEG 400, and 24.7% water; alternatively, the amounts and molecular weights of the binders can vary. Proportions of the constituents of the raw materials for the slurry can be varied as variously disclosed herein to achieve a desired composition of the ceramic-bonded diamond composite particle to be produced.
The slurry is processed to form a solidified granule. As identified in
The recovered granules are then processed 330 to remove water or other volatile components. In a first example process, water is removed from the recovered granule by a freeze drying process.
In the granulation steps 360 to 370, a slurry is formed and processed to form granule. The raw materials for the slurry can include any of the diamond material disclosed herein, including monocrystalline diamond, polycrystalline diamond, pitted diamond and combinations thereof, silicon particles, a solvent, and a binder. The binder can be any suitable binder that promotes the flow characteristics or spray characteristics suitable for the further processing steps while also being useful to promote sintering and green body formation as those alternative processes will be applied in the method. For example, a suitable binder can be selected from the group consisting of polyethylene glycol (PEG), polyvinyl alcohol (PVA), and wax. The solvent may be water, ethanol, acetone, or others chosen for compatibility with different binders and slurry processing systems. An example slurry composition includes, by weight, 66% diamond particles, 7.3% silicon powder, 1.5% PVA 4-88, 0.5% PEG 400, and 24.7% water. Proportions of the constituents of the raw materials for the slurry can be varied as variously disclosed herein to achieve a desired composition of the ceramic-bonded diamond composite particle to be produced.
The slurry is processed to form a solidified granule. As identified in
The granules from process 330 (
Process A 400 is shown in
Following pre-consolidation, material enters consolidation processing. For example, a consolidation process can incorporate HPHT processes that form a densified compact composed of ceramic-bonded diamond composite material 450. However, the materials, techniques and processes used prior to the consolidation process promote friability of the densified compact post-HPHT. Thus, the densified compact can be further processed to ceramic-bonded diamond composite particles by mechanically processing the densified compact to a desired D50 size 460. Non-limiting examples of techniques to mechanically process the densified compact to a desired D50 size include grinding, roller milling, roll compaction milling, hammer milling, cutting, compact milling, jet milling and ball milling. Typical desired particle sizes (based on D50) range from 20 to 100 microns (μm), alternatively ≧25 μm or ≧30 μm or ≧50 μm to ≦40 μm or ≦50 μm or ≦70 μm or ≦80 μm.
Process B 500 is shown in
Process C 600 is shown in
Following pre-consolidation, material enters consolidation processing. For example, a consolidation process can incorporate HPHT processes that form a densified compact composed of ceramic-bonded diamond composite material 640. However, the materials, techniques and processes used prior to the consolidation process promote friability of the densified compact post-HPHT. Thus, the densified compact can be further processed to ceramic-bonded diamond composite particles by mechanically processing the densified compact to a desired D50 size 650. Non-limiting examples of techniques to mechanically process the densified compact to a desired D50 size include grinding, roller milling, roll compaction milling, hammer milling, cutting, compact milling, jet milling and ball milling. Typical desired particle sizes (based on D50) range from 20 to 100 microns (μm), alternatively ≧25 μm or ≧30 μm or ≧50 μm to ≦40 μm or ≦50 μm or ≦70 μm or ≦80 μm.
Process D 700 is shown in
Process E 800 is shown in
An optional process to modify the surface of the diamond particles—either prior to forming the ceramic-bonded diamond composite particles or after forming the ceramic-bonded diamond composite particles—can be incorporated into any of the disclosed methods.
In the illustrated method 900, one optional surface modification process is to modify the surface morphology of diamond particles 910. Modifying the surface morphology of diamond particles can occur prior to forming or processing the granules as in any of the first process steps in Processes A to E. Air oxidation or graphitization methods can be used to achieve the surface modification. For example, a method of making granules may comprise the steps of treating a plurality of diamond particles at a pre-determined temperature, such as from about 550° C. to about 900° C., at a pre-set atmosphere, such as flowing air or flowing oxygen, such that diamond particles form nano-scale or sub-micron surface texture. In another example, diamond can be coated with nickel or nickel alloy via an electroless coating method. The weight percentage of Ni or Ni alloy can vary from 5% to 60%. The coated diamond can be subjected to elevated heat treatment in a temperature range from 550° C. to 1000° C. under inert atmospheres or flowing forming gas which contains 2-5% hydrogen and 95-98% nitrogen. The dwell time for the heat treatment can be from 30 minutes to 10 hours to enable the diamond surface to convert back to graphite. As a result, the surface morphology of the diamond can be modified due to the back conversion and very rough surface textures exposed after cleaning out of the graphite.
In a specific example, surface oxidation of the diamond particles having a D50 of 21.3 microns was conducted in a heated environment with flowing air (moisture content less than 1%). 30 grams of the diamond particles was loaded into a 10″×4″ sized quartz crucible and distributed to evenly cover the entire bottom area of the crucible. The crucible was then inserted into the center of a tube furnace. The two ends of the furnace were sealed using flanges incorporating inlet and outlet ports. The inlet port was connected to a gas cylinder by a plastic tube and the outlet port was connected to a ventilation hood using a plastic tube. A regulator was equipped at the gas cylinder to control the air flow. A 5 PSI pressure air flow was pre-adjusted and supplied during the entire experiment. The power was turned on at a heater control unit and the temperature was set at 700° C. with a ramp rate of 15° C. per minute. The dwell time for this experiment was controlled for 1 hour. The heater power was shut off after the dwell time. The diamond particles were allowed to cool in the furnace for several hours under flowing air to a temperature of 100° C. The air flow was turned off and the seal flange at the outlet side opened and the crucible removed. The diamond particles were collected and weighed. In this experiment, the weight loss was around 10%. The oxidized diamond particles were further characterized using SEM. A SEM image of the surface oxidized diamond particle is shown in
In the illustrated method 900, granules are formed using the (optionally modified) diamond particles and silicon 920. These granules are then processed under HPHT conditions to form a densified compact composed of ceramic-bonded diamond composite material 930 and then mechanically processed to a desired particle size 940. Processing into the granules, HPHT processing and mechanical processing can be by any of the methods disclosed herein in Processes A to E for such processes.
In the illustrated method 900, another optional surface modification process 950 can occur on the ceramic-bonded diamond composite particle after the particles are formed in the mechanical processing step as in any of the Processes A to E. In this optional process 950, the surface of the particle can be textured by exposure to one or more chemicals or chemical solutions that will preferentially dissolve or otherwise erode portions of the particle to increase the surface area or porosity of the particle, which is beneficial in that the increased surface area or porosity in the produced particle increases in the number of cutting points and contributes to aggressive cutting properties for the particle. Leaching is an example of this optional surface modification process 950. Examples of suitable leaching process include contacting or submerging a portion or all of the particle in a solution comprising one or more acids, such as sulfuric acid and nitric acid, or in a caustic solution, such as sodium hydroxide or potassium hydroxide or a mixture of both. For ceramic-bonded diamond composite particles having an average diameter of 40 to 100 microns, the particles can be submerged in a leaching solution for up to 72 hours at room temperature (or shorter period of time at elevated temperatures and/or pressures).
For example, unreacted silicon (or other active material) and unreacted carbon can be dissolved in the leaching process, which results in micropores on the surface. In a sulfuric acid and nitric acid solution with a combination ratio of 1:1, leaching can take up to 72 hours at room temperature. In the same solution, at elevated temperature of 200° C., leaching can take about 1-5 hours. In either sodium hydroxide or potassium hydroxide or both at a ratio of 1:1, which is a molten caustic mixture, leaching can take about less than 1 hour at a temperature of 300° C. Recovery of the diamond composite particles can include rinsing in deionized water for multiple cycles in order to remove residual acids or caustic chemicals.
An optional coating step can be incorporated into any of the disclosed methods.
In each of the methods disclosed herein, after the densified compact is mechanically broken to the desired particle size, the inert material can be separated and the resulting ceramic-bonded diamond composite particles can be collected for further use, for example, for further use in manufacturing products for wear applications, particularly where high thermal stability is desirable. Examples of such products include grinding wheels, saw blades, dicing blades, lapping compounds, polishing compounds.
It should be noted that the raw materials, in particular, the raw materials present in the consolidation process, are not contemplated to include cobalt or other refractory metals that are known to promote diamond-to-diamond bonding under HPHT processing conditions. Further, the diamond-to-diamond bonding is relatively stronger than the reaction bonded silicon carbide and would, therefore, be more likely to remain intact than the otherwise friable reaction bonded silicon carbide.
A quantitative measure of the contribution to the friability of the densified compact of inert material and the disclosed processing can be determined based on measuring the transverse rupture strength (TRS) (reported on a force per unit area basis) of the densified compact. Compacts from each of the processes 100, 200 and A-E were manufactured as disclosed herein. TRS was measured using an Instron 5800R universal testing machine and a 3-point bending test on a test bar (prepared from the densified compacts) measuring 30 mm length×3 mm height×4 mm width performed at room temperature, using a crosshead displacement rate of 2.54 mm/min and a test fixture span of 20 mm, and load versus crosshead displacement recorded. The highest point of the load-displacement curve was used to calculate the TRS by the following relationship:
TRS=1.5*[(P*I)/(h2*b)]
where P=maximum load, I is the test fixture span, h is the test bar height, and b is the test bar width. The values for TRS for various processes disclosed herein are reported in Table 1.
The toughness of the diamond composite particles, as measured by a standard friability test, may be a factor in abrasion performance. The friability test involves ball milling a quantity of product under controlled conditions and sieving the residue to measure the particle size reduction of the product. The toughness index (TI) is measured at room temperature and a score of 100 is the highest toughness of the crystal. In many cases the tougher the crystal, the longer the life of the crystal in a grinding or machining or dicing tool and, therefore, the longer the life of the tool. This leads to less tool wear and, ultimately, lower overall tool cost.
The ceramic diamond composite particles may be graded by size according to ASTM specification EI 1-09, entitled “Standard Specification for Wire Cloth and Sieves for Testing Purposes.” Table 2 lists toughness index data of the ceramic diamond composite particles in a size range from mesh size 40/50 (D50 of 400 micron) to mesh size 400/500 (D50 of 35 micron). The ceramic diamond composite particles were made by the various process disclosed herein, as indicated in the header to each column. Thus, for, example, ceramic diamond composite particles made from process 100 were made by crushing and milling HPHT sintered composite blanks without inert material followed by sieving into various mesh sizes. The diamond composite particles made by process 100 possess toughness index values of up to 95, indicating they are the toughest among other methods described herein.
Although the present invention has been described in connection with preferred embodiments thereof, it will be appreciated by those skilled in the art that additions, deletions, modifications, and substitutions not specifically described may be made without department from the spirit and scope of the invention as defined in the appended claims.
| Filing Document | Filing Date | Country | Kind |
|---|---|---|---|
| PCT/US2016/015332 | 1/28/2016 | WO | 00 |
| Number | Date | Country | |
|---|---|---|---|
| 62108628 | Jan 2015 | US |
