CN110744051B - Preparation method of polycrystalline diamond compact - Google Patents
Preparation method of polycrystalline diamond compact Download PDFInfo
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- CN110744051B CN110744051B CN201911189807.3A CN201911189807A CN110744051B CN 110744051 B CN110744051 B CN 110744051B CN 201911189807 A CN201911189807 A CN 201911189807A CN 110744051 B CN110744051 B CN 110744051B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
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Abstract
The invention discloses a preparation method of a polycrystalline diamond compact, which comprises the following steps: 1) weighing diamond and a metal catalyst according to the formula of a diamond polycrystalline layer, uniformly mixing, placing in a hydrogen atmosphere, reducing at the temperature of 400-550 ℃, heating to the temperature of 550-1100 ℃ for a hydrogenation reaction to enable the metal catalyst to react to generate metal hydride, and then keeping the hydrogen atmosphere and cooling to normal temperature to obtain mixed powder of the polycrystalline layer; 2) obtaining a hard alloy matrix; 3) and placing the mixed powder of the polycrystalline layer and the hard alloy matrix in a heat-preservation pressure-transfer medium, and performing high-temperature high-pressure synthesis to obtain the polycrystalline silicon carbide. The invention carries out specific heat treatment on the diamond and the metal catalyst under the normal pressure condition, and compared with the prior conventional pretreatment process for the diamond and the metal catalyst, the invention not only simplifies the process, but also reduces the cost of pretreatment and the production cost of the polycrystalline diamond compact, and is easier for industrialization.
Description
Technical Field
The invention relates to a superhard composite material, in particular to a preparation method of a polycrystalline diamond compact.
Background
Polycrystalline diamond composite materials (polycrystalline diamond compacts) are layered composite superhard materials formed by polymerizing diamond particles and a metal catalyst (also called a binder, specifically iron, cobalt or nickel) on the surface of a hard alloy (tungsten carbide-cobalt) substrate. The polycrystalline diamond composite material has the characteristics of high hardness and good wear resistance, is widely applied to industries such as petroleum drilling, geological exploration, coal field drilling and production drill bits, machining cutters and the like, and is mainly applied to finish machining of materials such as aluminum alloy, copper alloy, titanium alloy, wood and the like in machining.
At present, the preparation method of the polycrystalline diamond compact generally comprises the steps of respectively obtaining polycrystalline layer mixed powder (or polycrystalline layer wafer) and a hard alloy matrix, and then placing the polycrystalline layer mixed powder and the hard alloy matrix in a heat-preservation pressure-transmission medium for high-temperature high-pressure synthesis. However, in the existing method for obtaining the polycrystalline layer mixed powder (or polycrystalline layer wafer), the pretreatment conditions for diamond powder and metal catalyst are harsh, and the method is embodied in that: 1) the diamond powder needs to be subjected to a series of purification treatments (such as the invention patent with the publication number of CN 103722174A), wherein the purification treatments at least comprise chemical acid-base treatment purification, after the diamond powder is mixed with a metal catalyst, the reduction treatment is needed to prevent the metal catalyst from being oxidized, and after the reduction treatment, the diamond powder needs to be stored in vacuum to prevent the metal catalyst from being oxidized again and prevent the diamond from adsorbing gas in the air; 2) the mixed powder needs to be used up in a short time after meeting air, the residual mixed powder needs to be reduced and removed again after use, and the air adsorbed in the diamond powder needs to be removed by high vacuum (the vacuum degree is as high as 1 multiplied by 10)-4Pa) and equipment with high temperature (such as L1215 III type unit horizontal vacuum atmosphere furnace, the furnace needs to continuously start a diffusion pump to pump vacuum to keep the vacuum degree in the furnace after being started, and cooling water needs to be continuously introduced during use), and the operation inevitably increases the storage and production cost of materials, on one hand, the use cost and the maintenance cost of the equipment with high vacuum and high temperature are higher, on the other hand, special heat protection is needed for heat treatment in the high vacuum equipment, and the sealing rubber gasket is prevented from being burnt out, so that the use cost is high. The existing pretreatment method not only improves the production cost of the polycrystalline diamond compact, but also increases the operation difficulty of the process, so that the further popularization and application of the polycrystalline diamond compact are limited.
Disclosure of Invention
The invention aims to provide a preparation method of a polycrystalline diamond compact with simple process and low production cost.
The preparation method of the polycrystalline diamond compact comprises the following steps:
1) weighing diamond and a metal catalyst according to the formula of a diamond polycrystalline layer, uniformly mixing, placing in a hydrogen atmosphere, reducing at the temperature of 400-550 ℃, heating to the temperature of 550-1100 ℃ for a hydrogenation reaction to enable the metal catalyst to react to generate metal hydride, and then keeping the hydrogen atmosphere and cooling to normal temperature to obtain mixed powder of the polycrystalline layer;
2) obtaining a hard alloy matrix;
3) and placing the mixed powder of the polycrystalline layer and the hard alloy matrix in a heat-preservation pressure-transfer medium, and carrying out high-temperature high-pressure synthesis to obtain the polycrystalline diamond compact.
The method of the invention comprises the steps of placing the diamond and the metal catalyst in a hydrogen atmosphere, reducing the diamond and the metal catalyst, and then heating the reduced diamond and the metal catalyst to 550-1100 ℃, so that the metal catalyst is hydrogenated to generate metal hydride MeHx(x-1-3); on the other hand, the diamond particles can absorb hydrogen in the process, so that the aim of removing gas in the air in the conventional pretreatment process is fulfilled; furthermore, the metal hydride generated in the hydrogenation process and the hydrogen adsorbed by the diamond particles are released in the form of hydrogen in the subsequent high-temperature high-pressure synthesis process, so that the metal hydride and the diamond particles which do not adsorb other gases return to the metal catalyst. The container made of metal materials (preferably zirconium and niobium) with better hydrogen adsorption can be used for containing the obtained polycrystalline layer mixed powder so as to realize the purpose of protecting the safety of the synthesis process.
In step 1) of the method, the formula of the diamond polycrystalline layer is the same as that of the prior art, and the preferable formula comprises the following components in percentage by mass: 0.1-15% of metal catalyst and the balance of diamond. The metal catalyst is the same as the prior art, and is specifically one or the combination of more than two of iron, cobalt and nickel. In the reduction, the time for the reduction is preferably 0.5 to 2 hours. The metal catalyst and the diamond are both mixed in powder form, and the particle size is selected as in the prior art, wherein the particle size of the metal catalyst is preferably 0.1-5 μm, and the particle size of the diamond is preferably 0.5-20 μm.
In step 1) of the process according to the invention, the applicant's experimental results show that it is appropriate to control the hydrogenation reaction time to between 0.5 and 2 hours when carrying out the hydrogenation.
In step 2) of the method of the present invention, the cemented carbide substrate is obtained by a conventional method, such as being prepared by a conventional method, or is directly purchased from a conventional model cemented carbide substrate, such as YG16, YG16C, YG12, YG12C, YG10 or YG 10C.
In step 3) of the method of the present invention, the heat-insulating pressure-transmitting medium and the subsequent high-temperature high-pressure synthesis are the same as those in the prior art, and specifically, the heat-insulating pressure-transmitting medium is usually pyrophyllite, and is usually placed in a shielding cup (preferably a niobium cup with a cover or a zirconium cup with a cover) and then placed in the heat-insulating pressure-transmitting medium for pressing by using a cubic hydraulic press. The technological conditions of the high-temperature high-pressure synthesis are preferably as follows: the pressure is 4.5-6.5GPa, the temperature is 1400-1750 ℃ and the time is 150-800 s.
Compared with the prior art, the method carries out specific heat treatment on the diamond and the metal catalyst under the normal pressure condition, not only simplifies the process, but also further reduces the cost of pretreatment and the production cost of the polycrystalline diamond compact because high-vacuum high-temperature equipment is not needed, and is easier to industrialize.
Detailed Description
The present invention will be better understood from the following detailed description of specific examples, which should not be construed as limiting the scope of the present invention.
Diamond powder and cubic boron nitride powder described in the following examples were subjected to conventional chemical acid-base purification treatment.
Example 1
1) Weighing 90% of diamond powder and 10% of cobalt powder according to mass percentage, uniformly mixing the diamond powder and the cobalt powder by using alcohol, drying the mixture in vacuum at the temperature of 80 ℃, placing the obtained powder in a tubular furnace, heating the powder to 450 ℃ in a hydrogen atmosphere for hydrogen reduction for 1h, then heating the powder to 700 ℃ for heat preservation for 1.5h for hydrogenation treatment, keeping the hydrogen atmosphere state, and cooling the powder to normal temperature to obtain polycrystalline layer mixed powder;
2) the cemented carbide substrate was a commercially available model YG16 having a thickness of 3 mm;
3) 3.5g of the polycrystalline layer mixed powder obtained in the step 1) is put into a niobium cup (the specification is
) Leveling the middle part, paving a hard alloy substrate with the thickness of 3mm and the model of YG16, covering a zirconium cover and compacting to obtain a front assembly block; and filling the front assembly block into a pyrophyllite die, and performing high-temperature high-pressure synthesis (the conditions of the high-temperature high-pressure synthesis process are that the pressure is 5.5GPa, the temperature is 1600 ℃, and the temperature is kept for 400s) by using a hinge type cubic tripod press to obtain the polycrystalline diamond compact.
Comparative example 1
Example 1 was repeated, except that step 1) was carried out as follows:
1) weighing 90% of diamond powder and 10% of cobalt powder according to mass percentage, placing the diamond powder and the cobalt powder in a ball milling tank for ball milling for 3 hours, then drying and screening the mixture to obtain uniformly mixed powder, heating the obtained powder to 450 ℃ in a hydrogen atmosphere for hydrogen reduction for 1 hour, placing the reduced powder in a vacuum furnace at a vacuum degree of 1 multiplied by 104And (3) carrying out high-temperature high-vacuum purification for 2h at the temperature of 1100 ℃ under Pa, and then cooling to obtain the polycrystalline layer mixed powder.
Example 2
Example 1 was repeated, except that in step 1), the hydrogen reduction was carried out at 500 ℃ for 1 h; the hydrogenation treatment was carried out at 1000 ℃ for 0.5 h.
Example 3
Example 1 was repeated, except that in step 1), the mass percentages of diamond powder and cobalt powder were 95% and 5%, respectively; the hydrotreatment was carried out at 800 ℃ for 2 h.
The wear resistance of the polycrystalline diamond compacts prepared in examples 1 to 3 and comparative example 1 was tested by the following test method: and cutting the obtained polycrystalline diamond compact into small pieces by using a wire, clamping the small pieces by using a metal clamp, and testing in a wear ratio testing machine, wherein the material to be ground is a silicon carbide grinding wheel, and the H value of the silicon carbide grinding wheel is 3.4 mm. The high-speed rotation speed of the grinding wheel is 2500 m/min. The polycrystalline layer of the composite sheet obtained in each example was ground at an angle of 45 ° against the grinding wheel while the polycrystalline layer was moved laterally. The grinding amount of the grinding wheel is not less than 25 g. The abrasion ratios of the composite sheets obtained in the respective examples were calculated and shown in table 1 below.
Table 1:
| example 1 | Comparative example 1 | Example 2 | Example 3 | |
| Wear ratio | 30.7×103 | 31.1×103 | 31.3×103 | 35.3×103 |
Claims (6)
1. A preparation method of a polycrystalline diamond compact comprises the following steps:
1) weighing diamond and a metal catalyst according to the formula of a diamond polycrystalline layer, uniformly mixing, placing in a hydrogen atmosphere, reducing at the temperature of 400-550 ℃, heating to the temperature of 550-1100 ℃ for a hydrogenation reaction to enable the metal catalyst to react to generate metal hydride, and then keeping the hydrogen atmosphere and cooling to normal temperature to obtain mixed powder of the polycrystalline layer;
2) obtaining a hard alloy matrix;
3) and placing the mixed powder of the polycrystalline layer and the hard alloy matrix in a heat-preservation pressure-transfer medium, and carrying out high-temperature high-pressure synthesis to obtain the polycrystalline diamond compact.
2. The method of claim 1, wherein: in the step 1), the formula of the diamond polycrystalline layer comprises the following components in percentage by mass: 0.1-15% of metal catalyst and the balance of diamond.
3. The method of claim 1, wherein: in the step 1), the metal catalyst is one or a combination of more than two of iron, cobalt and nickel.
4. The method of claim 1, wherein: in the step 1), the reduction time is 0.5-2 h.
5. The method of claim 1, wherein: in the step 1), the time of the hydrogenation reaction is 0.5-2 h.
6. The method of claim 1, wherein: in the step 3), the process conditions of the high-temperature high-pressure synthesis are as follows: the pressure is 4.5-6.5GPa, the temperature is 1400-1750 ℃ and the time is 150-800 s.
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| CN111974310B (en) * | 2020-09-07 | 2022-04-01 | 中国有色桂林矿产地质研究院有限公司 | Method for preparing polycrystalline diamond compact from cobalt catalyst-loaded diamond micro powder |
| CN112375932B (en) * | 2020-11-12 | 2022-01-21 | 中国有色桂林矿产地质研究院有限公司 | Graphene anti-adhesion polycrystalline diamond compact and preparation method thereof |
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