CN112239362A - Preparation method of single-phase polycrystalline cubic boron nitride sintered body - Google Patents
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Abstract
The invention belongs to a method for preparing a single-phase pure cubic boron nitride polycrystalline sintered body by using cubic boron nitride micro powder as an initial raw material, which has good heat resistance and high hardness. The method comprises the steps of 1, cubic boron nitride powder is preferably selected, 2, prepressing and forming, 3, vacuum heat treatment, 4, pyrophyllite synthesis block assembly, 5, high-temperature and high-pressure sintering and the like, and the preparation of the single-phase pure cubic boron nitride polycrystal is completed. The method has strong operability, and can be finished by one-time sintering on the conventional cubic boron nitride polycrystalline sintering machine, so that the performances of wear resistance, heat resistance, hardness and the like of the single-phase cubic boron nitride polycrystalline sintering body are greatly improved. The method of the invention provides an effective way for preparing the superhard cutter material.
Description
Technical Field
The invention belongs to the field of manufacturing of cutting tool materials, and particularly relates to a preparation method of a single-phase cubic boron nitride polycrystalline sintered body which does not need a binder, has good heat resistance and high hardness.
Background
The superhard material has irreplaceable effect in national economic construction and national defense industry, is called national strategic material, and the superhard material and the product thereof are listed as one of the national strategic emerging industries. Among them, the sintered body of the superhard material has occupied an absolute specific gravity in industrial applications. How to prepare a high-performance superhard material sintered body and obtain the superhard material sintered body with excellent comprehensive performances such as high compactness, thermal stability, hardness and the like is a difficult problem which troubles the field and a key problem to be solved urgently.
As a green environment-friendly high-performance structural material, the cubic boron nitride polycrystal fully reflects the requirements of modern manufacturing industry on the material by the excellent performances of super wear resistance, corrosion resistance, high temperature resistance and the like. The cubic boron nitride polycrystalline cutter is particularly suitable for hard cutting, rough and finish machining of various ferrous metals, and even turning instead of grinding. Not only improves the drawing processing efficiency, but also greatly reduces the processing cost, and mainly cuts various quenched steels, tool steels, die steels, bearing steels (HRC45-70), chilled cast irons, high-chromium cast irons, nickel-based and cobalt-based high-temperature alloys, various difficult-to-process grey cast irons, other difficult-to-process black materials and the like. Because the hardness of the cubic boron nitride is far higher than that of ceramics and hard alloy, the service life of the prepared cutter is several times that of the ceramic cutter and the hard alloy cutter. Under the large background of efficient machining, efficient cutters such as cubic boron nitride polycrystallization and the like are widely accepted by the market and gradually replace the traditional cutters, so that the domestic huge demand for cubic boron nitride polycrystallization for metal cutting is bound to exist.
At present, the existing cubic boron nitride polycrystalline sintered body is a high-performance structural material, wherein independent cubic boron nitride particles are bonded by a binder (sintering aid) under the conditions of high temperature and high pressure, so that the whole cubic boron nitride layer is sintered into a high-strength cubic boron nitride polycrystalline. The cubic boron nitride polycrystalline material has obvious differences in synthesis conditions and product performance due to different manufacturing methods and sintering mechanisms, and what is important to explain here is that: because of the addition of the binder in the sintering system, mechanical properties such as hardness and the like are greatly reduced, heat resistance is greatly influenced, and the service life of a product is reduced due to the fact that the binder with different components is doped, and the product is formed by large residual thermal stress caused by different thermal expansion coefficients, so that the binder is not used, the development of single-phase cubic boron nitride polycrystal has great advantages in service performance, and the cutting performance and the service life of the cubic boron nitride polycrystal are greatly improved. Based on this, there is an urgent need for a method for preparing a polycrystalline sintered body of boron nitride having advantages in terms of high wear resistance, hardness, and high-temperature resistance.
Disclosure of Invention
The invention aims to provide a preparation method of a single-phase cubic boron nitride polycrystalline sintered body, which does not adopt a binder, does not need the addition of various nitrogen mixtures, and has simple process and strong operability.
The technical scheme of the invention is as follows:
a preparation method of a single-phase polycrystalline sintered cubic boron nitride body comprises the following steps:
firstly, submicron and nano cubic boron nitride micro powder is used as an initial raw material, then sorting and purification treatment are carried out, the purity of the cubic boron nitride reaches 99.9 wt%, the crystal form is complete, the corners are not damaged and passivated, the particle uniformity is good, and the average particle size of the selected submicron and nano cubic boron nitride micro powder is 50nm-10 mu m;
secondly, putting the pure cubic boron nitride powder which is selected in the step one and is not added with the binder into a molybdenum cup for assembly, wherein the molybdenum cup is used as an anti-pollution packaging device, the wall thickness is 0.08-0.2 mm, and the original micro powder material can be hermetically packaged;
and thirdly, the molybdenum cup assembled in the second step is subjected to prepressing molding, vacuum purification treatment, pyrophyllite synthesis block fitting assembly and high-temperature high-pressure sintering to complete the preparation of the single-phase cubic boron nitride polycrystal.
The method comprises the following steps that firstly, the cubic boron nitride micro powder in the neutral direction is a high-purity cubic phase.
The processes of pre-pressing forming, vacuum heat treatment, pyrophyllite synthesis block fitting assembly and high-temperature high-pressure sintering are that the molybdenum cup assembled in the second step is pre-pressed and formed under the pressure of more than 30MPa, the molybdenum cup is placed into a graphite tube external member after heat treatment for 1-2 hours at the temperature of 700 ℃ in vacuum, all the parts are placed into the pyrophyllite synthesis block together, high-temperature high-pressure sintering is carried out on a cubic press, the sintering conditions are 7-8GPa, 1800 and 1900 ℃ plus materials, the sintering heat preservation time is 5-10min, and finally the submicron and nano pure cubic boron nitride polycrystalline sintering body with excellent performance is obtained.
The invention has the beneficial effects that:
1. the method for preparing the cubic boron nitride polycrystalline powder selects the submicron and nanometer cubic boron nitride single crystal micro-powder raw materials with good crystal form uniformity and high purity, does not adopt any binder, does not need the addition of various nitrogen mixtures and other substances, has excellent performances of high heat resistance, high wear resistance, hardness and the like, and obviously improves the heat resistance (higher than 1300 ℃); the hardness is more than 50 GPa.
2. The method has strong operability, reduces the negative influence of uneven powder mixing or introduced impurities, and has simple process and good repeatability. Can be directly finished on the existing production press equipment without secondary pressurization ultrahigh pressure. The method of the invention provides an effective way for preparing the superhard cutter material.
3. The synthesized cubic boron nitride polycrystalline product has high stability, and can be suitable for the fields of rough machining and precision machining of materials such as chilled cast iron, heat-resistant alloy, quenched steel and the like.
Drawings
FIG. 1 is an assembled sectional view of a pyrophyllite composite block fitting of the present invention. The composite material comprises a pure cubic boron nitride micro-powder raw material 1 with a molybdenum cup, an insulating sheet 2, a heating pipe 3, a graphite sheet 4, a copper sheet 5, a conductive steel cap 6 and a pyrophyllite synthetic block 7.
Detailed Description
The single-phase boron nitride polycrystalline sintered body is obtained through long-term research by the inventor and long-term experiments. The method adopts high-quality submicron and nanoscale cubic boron nitride micro powder as a raw material, and synthesizes the boron nitride polycrystalline sintered body through the processes of pre-pressing forming, vacuum heat treatment and high-temperature high-pressure sintering.
Example 1:
1) submicron cubic boron nitride micro powder is adopted as a raw material, then sorting and purifying treatment is carried out, the micro powder with purity of 99.9 wt%, complete crystal form, undamaged corners and unpassivated particles and good particle uniformity is preferred, and the average particle size of the selected submicron cubic boron nitride micro powder is 50 nm.
2) 3 g of pure cubic boron nitride micro powder selected in the step 1) is put into a molybdenum cup with the diameter of 16mm and the wall thickness of 0.2mm for assembly, so that the powder can be hermetically packaged to prevent pollution.
3) Pre-pressing and molding the molybdenum cup assembled in the step 2) under 40MPa, carrying out heat treatment at 700 ℃ for 1h through vacuum purification, then placing the molybdenum cup into a graphite tube 3, and finally placing the components 4-6 into a pyrophyllite synthetic block 7 together, wherein the size of the pyrophyllite synthetic block 7 is 32.5mm multiplied by 32.5mm, the diameter of a synthetic cavity is 18mm, and the inner diameter of the graphite tube 3 is 16mm and the height is 17 mm. Sintering the pyrophyllite synthesized block at high temperature and high pressure on a cubic press, wherein the sintering conditions are 7.5GPa and 1850 ℃, slowly cooling to room temperature after sintering and heat preservation time is 5min, and releasing pressure to obtain a phi 14mm multiplied by 5mm single-phase cubic boron nitride polycrystalline sintered body.
Example 2:
1) submicron cubic boron nitride micro powder is adopted as a raw material, then sorting and purifying treatment is carried out, the micro powder with purity of 99.9 wt%, complete crystal form, undamaged corners, non-passivation and good particle uniformity is preferably selected, and the average particle size of the selected submicron cubic boron nitride micro powder is 1-2 μm.
2) 3 g of pure cubic boron nitride micro powder selected in the step 1) is put into a molybdenum cup with the diameter of 16mm and the wall thickness of 0.08mm for assembly, so that the powder can be hermetically packaged to prevent pollution.
3) Pre-pressing and molding the molybdenum cup assembled in the step 2) under 40MPa, performing heat treatment at 700 ℃ for 1.5h through vacuum purification, putting the molybdenum cup into a graphite tube 3, and finally putting the components 4-6 into a pyrophyllite synthetic block 7 together, wherein the size of the pyrophyllite synthetic block 7 is 32.5mm multiplied by 32.5mm, the diameter of a synthetic cavity is 18mm, and the inner diameter and the height of the graphite tube 3 are 16mm and 17 mm. And (3) sintering the pyrophyllite synthesized block at high temperature and high pressure on a cubic press under the sintering conditions of 7GPa and 1800 ℃, slowly cooling to room temperature after sintering and heat preservation time of 5min, and releasing pressure to obtain the phi 14mm multiplied by 5mm single-phase cubic boron nitride polycrystalline sintered body.
Example 3:
1) submicron cubic boron nitride micro powder is adopted as a raw material, then sorting and purifying treatment is carried out, the micro powder with purity of 99.9 wt%, complete crystal form, undamaged corners, non-passivation and good particle uniformity is preferably selected, and the average particle size of the selected submicron cubic boron nitride micro powder is 10 mu m.
2) 3 g of pure cubic boron nitride micro powder selected in the step 1) is put into a molybdenum cup with the diameter of 16mm and the wall thickness of 0.1mm for assembly, so that the powder can be hermetically packaged to prevent pollution.
3) Pre-pressing and molding the molybdenum cup assembled in the step 2) under 40MPa, performing heat treatment at 700 ℃ for 2h through vacuum purification, then placing the molybdenum cup into a graphite tube 3, and finally placing the components 4-6 into a pyrophyllite synthetic block 7 together, wherein the size of the pyrophyllite synthetic block 7 is 32.5mm multiplied by 32.5mm, the diameter of a synthetic cavity is 18mm, and the inner diameter of the graphite tube 3 is 16mm and the height is 17 mm. Sintering the pyrophyllite synthesized block at high temperature and high pressure on a cubic press, wherein the sintering conditions are 8GPa and 1900 ℃, the temperature is slowly reduced to room temperature after the sintering heat preservation time is 10min, and the single-phase cubic boron nitride polycrystalline sintered body with phi 14mm multiplied by 5mm is obtained after pressure relief.
The application finishes one-time sintering on the existing cubic bench press, and the performances of wear resistance, heat resistance, hardness and the like of the single-phase cubic boron nitride polycrystalline sintered body are greatly improved. The method of the invention provides an effective way for preparing the superhard cutter material. Compared with the prior art, the cubic boron nitride polycrystalline sintered body disclosed by the patent adopts cubic boron nitride instead of hexagonal boron nitride as an initial raw material, so that the problem that hexagonal-to-cubic phase transformation is insufficient to influence the performance of finally forming a polycrystalline is avoided, more rigorous sintering conditions are not needed, and the sintering conditions are smaller than those of hexagonal sintered polycrystalline. It is also advantageous in view of operability.
The synthesis principle is as follows: the method adopts the optimized cubic boron nitride nano and submicron particles as undamaged particles with high crystallization and high cleanliness, and the surfaces of the particles have higher sintering activity due to the fact that raw materials are packaged in a molybdenum cup and subjected to vacuum heat treatment, so that bonding between boron nitride can be formed under the conditions of high pressure and high temperature, a net structure is formed, and the particles have high strength and high wear resistance and have more excellent mechanical properties than a polycrystalline material added with a binder. Such as heat resistance, hardness and wear resistance. Meanwhile, due to the selection of raw materials and vacuum packaging heat treatment, the sintering conditions are not very harsh.
Compared with the prior art, the cubic boron nitride polycrystalline sintered body synthesized by the method has good technical performance indexes, is simple in process operation and good in repeatability, can keep the hardness close to that of a cubic boron nitride single crystal, reaches the hardness of more than 50GPa, is higher than that of a common polycrystalline (30GPa) with a binder, and has the heat resistance of more than 1300 ℃.
Claims (3)
1. A preparation method of a single-phase polycrystalline sintered cubic boron nitride body is characterized by comprising the following steps: the method comprises the following steps:
firstly, submicron and nano cubic boron nitride micro powder is used as an initial raw material, then sorting and purification treatment are carried out, the purity of the cubic boron nitride reaches 99.9 wt%, the crystal form is complete, the corners are not damaged and passivated, the particle uniformity is good, and the average particle size of the selected submicron and nano cubic boron nitride micro powder is 50nm-10 mu m;
secondly, putting the pure cubic boron nitride powder which is selected in the step one and is not added with the binder into a molybdenum cup for assembly, wherein the molybdenum cup is used as an anti-pollution packaging device, the wall thickness is 0.08-0.2 mm, and the original micro powder material can be hermetically packaged;
and thirdly, the molybdenum cup assembled in the second step is subjected to prepressing molding, vacuum purification treatment, pyrophyllite synthesis block fitting assembly and high-temperature high-pressure sintering to complete the preparation of the single-phase cubic boron nitride polycrystal.
2. The method for preparing a single-phase polycrystalline sintered body of cubic boron nitride according to claim 1, wherein: the method comprises the following steps that firstly, the cubic boron nitride micro powder in the neutral direction is a high-purity cubic phase.
3. The method for preparing a single-phase polycrystalline sintered body of cubic boron nitride according to claim 1, wherein: the processes of pre-pressing forming, vacuum heat treatment, pyrophyllite synthesis block fitting assembly and high-temperature high-pressure sintering are that the molybdenum cup assembled in the second step is pre-pressed and formed under the pressure of more than 30MPa, the molybdenum cup is placed into a graphite tube external member after heat treatment for 1-2 hours at the temperature of 700 ℃ in vacuum, all the parts are placed into the pyrophyllite synthesis block together, high-temperature high-pressure sintering is carried out on a cubic press, the sintering conditions are 7-8GPa, 1800 and 1900 ℃ plus materials, the sintering heat preservation time is 5-10min, and finally the submicron and nano pure cubic boron nitride polycrystalline sintering body with excellent performance is obtained.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103526295A (en) * | 2013-10-15 | 2014-01-22 | 寇自力 | High-purity high-hardness polycrystalline cubic boron nitride block material and preparation method thereof |
| CN106699190A (en) * | 2017-01-03 | 2017-05-24 | 吉林师范大学 | Method for preparing polycrystalline sintered body by using cubic boron nitride single crystal bioblast as initial raw material |
| CN109650900A (en) * | 2018-12-19 | 2019-04-19 | 郑州中南杰特超硬材料有限公司 | A kind of synthetic method of pure phase polycrystal cubic boron nitride cylinder |
| CN110342943A (en) * | 2019-07-18 | 2019-10-18 | 燕山大学 | The method and its application of binder free plycrystalline diamond boron nitride bulk are synthesized under industrial stresses |
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Patent Citations (4)
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| CN103526295A (en) * | 2013-10-15 | 2014-01-22 | 寇自力 | High-purity high-hardness polycrystalline cubic boron nitride block material and preparation method thereof |
| CN106699190A (en) * | 2017-01-03 | 2017-05-24 | 吉林师范大学 | Method for preparing polycrystalline sintered body by using cubic boron nitride single crystal bioblast as initial raw material |
| CN109650900A (en) * | 2018-12-19 | 2019-04-19 | 郑州中南杰特超硬材料有限公司 | A kind of synthetic method of pure phase polycrystal cubic boron nitride cylinder |
| CN110342943A (en) * | 2019-07-18 | 2019-10-18 | 燕山大学 | The method and its application of binder free plycrystalline diamond boron nitride bulk are synthesized under industrial stresses |
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