CN113831127A - Preparation method of polycrystalline cubic boron nitride diamond composite material - Google Patents

Preparation method of polycrystalline cubic boron nitride diamond composite material Download PDF

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CN113831127A
CN113831127A CN202111115556.1A CN202111115556A CN113831127A CN 113831127 A CN113831127 A CN 113831127A CN 202111115556 A CN202111115556 A CN 202111115556A CN 113831127 A CN113831127 A CN 113831127A
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diamond
boron nitride
cubic boron
composite material
polycrystalline
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王永凯
张相法
位星
王大鹏
刘红伟
薛磊
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Zhengzhou Zhongnan Jete Superabrasives Co ltd
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    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/52Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/583Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on boron nitride
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    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64Burning or sintering processes
    • C04B35/645Pressure sintering
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567Treatment time
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    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C26/00Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
    • C22C2026/003Cubic boron nitrides only

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Abstract

The invention provides a preparation method of a polycrystalline cubic boron nitride diamond composite material. The preparation method of the polycrystalline cubic boron nitride diamond composite material comprises the following steps: s1, selecting materials: (1) selecting ammonia borane with the purity of 99.9 percent and the size of 1-5 mu m and diamond with the size of 100-500 mu m as initial raw materials; (2) the ammonia borane accounts for 30-100 parts by weight, and the diamond accounts for 10-80 parts by weight. The preparation method of the polycrystalline cubic boron nitride diamond composite material provided by the invention prepares the binderless polycrystalline diamond/cubic boron nitride sintered body composite material through in-situ reaction, can ensure that cubic boron nitride and diamond are uniformly distributed in a polycrystalline sintered body, ensures the consistency of the microstructure of the polycrystalline sintered body, directly forms bonding through the cubic boron nitride and the diamond, is compact in combination, has slightly low pressure condition required by synthesis, and is convenient for large-scale industrial production.

Description

Preparation method of polycrystalline cubic boron nitride diamond composite material
Technical Field
The invention belongs to the technical field of diamond composite materials, and particularly relates to a preparation method of a polycrystalline cubic boron nitride diamond composite material.
Background
The diamond composite material is a special material widely used, usually, a certain proportion of diamond particles are added into a matrix material, the diamond particles are embedded in the matrix to be used as hard particles and wear-resistant phases, the performance of the diamond composite material mainly depends on the performance of diamond and the performance of the matrix material used for embedding the diamond particles, and the matrix material can be metal, alloy, resin, ceramic, rubber and the like. A tool made of an alloy matrix/diamond composite material is usually selected when cutting and grinding hard natural materials or artificial building materials and drilling hard rock strates, but the natural materials or the artificial building materials and rock strates have the characteristics of high hardness, high strength, strong grindability and the like, so that diamond falling caused by over-quick abrasion of the diamond composite material matrix is often caused in the use process, the tool fails, the use efficiency is lower, and in order to improve the processing efficiency of the hard materials and the drilling efficiency of the hard rock strates, a high-performance diamond tool matrix material is selected as an important way, in the related technology, a polycrystalline cubic boron nitride/diamond composite material is disclosed and consists of polycrystalline cubic boron nitride, diamond particles and a bonding agent 8, the composite material of the invention innovatively takes the polycrystalline cubic boron nitride as the matrix material of the diamond composite material, the hardness and the wear resistance of the matrix of the composite material are obviously improved, the composite material is applied to a diamond tool and can improve the processing efficiency of the hard material and the drilling efficiency of a hard rock stratum, the cubic boron nitride micro powder, the diamond particles and the bonding agent powder are prepared by adopting a high-temperature high-pressure sintering process, the polycrystalline cubic boron nitride is adopted as the matrix material of the diamond composite material, the diamond is embedded in the matrix material and is used as a hard mass point and a wear-resistant phase, the structure of the composite material is compact, the matrix has higher hardness, wear resistance and comprehensive performance, and the diamond tool made of the composite material can improve the processing efficiency of the hard material and the drilling efficiency of the hard rock stratum.
However, the above-mentioned structure has disadvantages that the above-mentioned structure is made of a binder, the synthesis pressure condition required is high, it is inconvenient for mass industrial production, and cubic boron nitride and diamond cannot be uniformly distributed in a polycrystalline sintered body, which results in loose bonding.
Therefore, there is a need to provide a new method for preparing polycrystalline cubic boron nitride diamond composite material to solve the above technical problems.
Disclosure of Invention
The invention solves the technical problem of providing a preparation method of a polycrystalline cubic boron nitride diamond composite material which can prepare binderless polycrystalline diamond/cubic boron nitride sintered body composite material through in-situ reaction, can ensure that cubic boron nitride and diamond are uniformly distributed in a polycrystalline sintered body, ensures the consistency of the microstructure of the polycrystalline sintered body, directly forms bonding through the cubic boron nitride and the diamond, is compactly bonded, has slightly low pressure condition required by synthesis, and is convenient for large-scale industrial production.
In order to solve the technical problem, the preparation method of the polycrystalline cubic boron nitride diamond composite material provided by the invention comprises the following steps:
s1, selecting materials:
(1) selecting ammonia borane with the purity of 99.9 percent and the size of 1-5 mu m and diamond with the size of 100-500 mu m as initial raw materials;
(2) ammonia borane in 30-100 weight portions and diamond in 10-80 weight portions;
s2, preparation process:
(1) putting the initial raw materials into a three-dimensional mixer according to a certain mass ratio, and mixing for 2-6 h;
(2) placing the mixed powder body on a hydraulic press to be pressed into a column body, wherein the pressure is 5-15MPa, and the time is 10-20 min;
(3) placing the obtained column body in a vacuum environment at the temperature of 300-600 ℃ for vacuum treatment, and naturally cooling after the vacuum treatment for 2-4 hours;
(4) and (3) putting the cylinder subjected to high-temperature vacuum treatment in the step (3) into a pyrophyllite synthetic block, and then putting the pyrophyllite synthetic block into a cubic press for high-temperature high-pressure synthesis.
As a further scheme of the invention, the synthetic pressure of the cubic press is 7-10 GPa, the temperature is 1800-2300 ℃, and the time is 3-8 min.
As a further aspect of the present invention, S3, the molding process:
(1) and (3) taking out the material prepared in the step (4), performing acid-base post-treatment and the like, and removing surface impurities to obtain the binderless polycrystalline diamond/cubic boron nitride sintered body composite material.
Compared with the prior art, the preparation method of the polycrystalline cubic boron nitride diamond composite material provided by the invention has the following beneficial effects:
1. with ammonia borane (NH)3BH3) The diamond micro powder is used as an initial material, and the binderless polycrystalline diamond/cubic boron nitride sintered body composite material is prepared through in-situ reaction, so that cubic boron nitride and diamond can be uniformly distributed in a polycrystalline sintered body, the consistency of the microstructure of the polycrystalline sintered body is ensured, the cubic boron nitride and the diamond are directly bonded, the bonding is compact, and meanwhile, the pressure condition required by synthesis is slightly low, so that the large-scale industrial production is facilitated;
2. by adjusting the mass ratio of the initial materials, the content of cubic boron nitride and diamond can be regulated, so that the binderless polycrystalline diamond/cubic boron nitride sintered body composite material with different properties can be prepared.
Detailed Description
The preparation method of the polycrystalline cubic boron nitride diamond composite material comprises the following steps:
s1, selecting materials:
(1) selecting ammonia borane with the purity of 99.9 percent and the size of 1-5 mu m and diamond with the size of 100-500 mu m as initial raw materials;
(2) ammonia borane in 30-100 weight portions and diamond in 10-80 weight portions;
s2, preparation process:
(1) putting the initial raw materials into a three-dimensional mixer according to a certain mass ratio, and mixing for 2-6 h;
(2) placing the mixed powder body on a hydraulic press to be pressed into a column body, wherein the pressure is 5-15MPa, and the time is 10-20 min;
(3) placing the obtained column body in a vacuum environment at the temperature of 300-600 ℃ for vacuum treatment, and naturally cooling after the vacuum treatment for 2-4 hours;
(4) and (3) putting the cylinder subjected to high-temperature vacuum treatment in the step (3) into a pyrophyllite synthetic block, and then putting the pyrophyllite synthetic block into a cubic press for high-temperature high-pressure synthesis.
2. The method of producing a polycrystalline cubic boron nitride diamond composite material according to claim 1, characterized in that: the synthetic pressure of the cubic press is 7-10 GPa, the temperature is 1800-2300 ℃, and the time is 3-8 min.
3. The method of producing a polycrystalline cubic boron nitride diamond composite material according to claim 1, characterized in that: s3, molding:
(1) and (3) taking out the material prepared in the step (4), performing acid-base post-treatment and the like, and removing surface impurities to obtain the binderless polycrystalline diamond/cubic boron nitride sintered body composite material.
The preparation method of the polycrystalline cubic boron nitride diamond composite material provided by the invention has the working principle that:
NH3BH3decomposition reaction is carried out under heating condition to generate BN and release H2, and the reaction chemical formula is as follows: NH (NH)3BH3→BN+3H2And the product BN is converted into cubic boron nitride at ultrahigh pressure and high temperature and is bonded with diamond to obtain the binderless polycrystalline diamond/cubic boron nitride sintered body.
Example 1:
the preparation method of the polycrystalline cubic boron nitride diamond composite material comprises the following steps:
(1) putting 100 parts by weight of ammonia borane with the purity of 99.9 percent and the size of 5 mu m and 80 parts by weight of diamond into a three-dimensional mixer for mixing treatment for 6 hours;
(2) placing the mixed powder body on a hydraulic press to be pressed into a column body, wherein the pressure is 15MPa and the time is 20 min;
(3) placing the pressed cylinder in a vacuum environment at the temperature of 600 ℃ for vacuum treatment, and naturally cooling after vacuum treatment for 4 hours;
(4) filling the cylinder subjected to high-temperature vacuum treatment in the step (3) into a pyrophyllite synthetic block, and then placing the pyrophyllite synthetic block into a cubic press for high-temperature high-pressure synthesis, wherein the synthesis pressure of the cubic press is 10GPa, the temperature is 2300 ℃, and the time is 8 min;
(5) and (3) taking out the material prepared in the step (4), performing acid-base post-treatment and the like, and removing surface impurities to obtain the binderless polycrystalline diamond/cubic boron nitride sintered body composite material.
The working principle is as follows: NH (NH)3BH3Decomposition reaction is carried out under heating condition to generate BN and release H2, and the reaction chemical formula is as follows: NH (NH)3BH3→BN+3H2And the product BN is converted into cubic boron nitride at ultrahigh pressure and high temperature and is bonded with diamond to obtain the binderless polycrystalline diamond/cubic boron nitride sintered body.
Example 2:
the preparation method of the polycrystalline cubic boron nitride diamond composite material comprises the following steps:
(1) putting 50 parts by weight of ammonia borane with the purity of 99.9 percent and the size of 3 mu m and 30 parts by weight of diamond with the size of 250 mu m into a three-dimensional mixer for mixing treatment for 4 hours;
(2) placing the mixed powder body on a hydraulic press to be pressed into a column body, wherein the pressure is 10MPa and the time is 15 min;
(3) placing the pressed cylinder in a vacuum environment at the temperature of 450 ℃ for vacuum treatment, and naturally cooling after the vacuum treatment for 3 hours;
(4) filling the cylinder subjected to high-temperature vacuum treatment in the step (3) into a pyrophyllite synthetic block, and then placing the pyrophyllite synthetic block into a cubic press for high-temperature high-pressure synthesis, wherein the synthesis pressure of the cubic press is 8.5GPa, the temperature is 2000 ℃, and the time is 5 min;
(5) and (3) taking out the material prepared in the step (4), performing acid-base post-treatment and the like, and removing surface impurities to obtain the binderless polycrystalline diamond/cubic boron nitride sintered body composite material.
The working principle is as follows: NH (NH)3BH3Decomposition reaction under heating condition to generate BN and release H2The reaction chemical formula is as follows: NH (NH)3BH3→BN+3H2And the product BN is converted into cubic boron nitride at ultrahigh pressure and high temperature and is bonded with diamond to obtain the binderless polycrystalline diamond/cubic boron nitride sintered body.
Example 3:
the preparation method of the polycrystalline cubic boron nitride diamond composite material comprises the following steps: (1) putting ammonia borane with the purity of 99.9 percent, the size of 1 mu m and the weight of 30 parts and diamond with the size of 100 mu m and the weight of 10 parts into a three-dimensional mixer for mixing treatment for 2 hours;
(2) placing the mixed powder body on a hydraulic press to be pressed into a column body, wherein the pressure is 5MPa and the time is 10 min;
(3) placing the pressed cylinder in a vacuum environment at the temperature of 300 ℃ for vacuum treatment, and naturally cooling after the vacuum treatment for 2 hours;
(4) filling the cylinder subjected to high-temperature vacuum treatment in the step (3) into a pyrophyllite synthetic block, and then placing the pyrophyllite synthetic block into a cubic press for high-temperature high-pressure synthesis, wherein the synthesis pressure of the cubic press is 7GPa, the temperature is 1800 ℃ and the time is 3 min;
(5) and (3) taking out the material prepared in the step (4), performing acid-base post-treatment and the like, and removing surface impurities to obtain the binderless polycrystalline diamond/cubic boron nitride sintered body composite material.
The working principle is as follows: NH (NH)3BH3Decomposition reaction is carried out under heating condition to generate BN and release H2, and the reaction chemical formula is as follows: NH (NH)3BH3→BN+3H2The product BN is converted into cubic boron nitride at ultrahigh pressure and high temperature and is bonded with diamond to obtain the binderless polycrystalA diamond/cubic boron nitride sintered body.

Claims (3)

1. The preparation method of the polycrystalline cubic boron nitride diamond composite material is characterized by comprising the following steps:
s1, selecting materials:
(1) selecting ammonia borane with the purity of 99.9 percent and the size of 1-5 mu m and diamond with the size of 100-500 mu m as initial raw materials;
(2) ammonia borane in 30-100 weight portions and diamond in 10-80 weight portions;
s2, preparation process:
(1) putting the initial raw materials into a three-dimensional mixer according to a certain mass ratio, and mixing for 2-6 h;
(2) placing the mixed powder body on a hydraulic press to be pressed into a column body, wherein the pressure is 5-15MPa, and the time is 10-20 min;
(3) placing the obtained column body in a vacuum environment at the temperature of 300-600 ℃ for vacuum treatment, and naturally cooling after the vacuum treatment for 2-4 hours;
(4) and (3) putting the cylinder subjected to high-temperature vacuum treatment in the step (3) into a pyrophyllite synthetic block, and then putting the pyrophyllite synthetic block into a cubic press for high-temperature high-pressure synthesis.
2. The method of producing a polycrystalline cubic boron nitride diamond composite material according to claim 1, characterized in that: the synthetic pressure of the cubic press is 7-10 GPa, the temperature is 1800-2300 ℃, and the time is 3-8 min.
3. The method of producing a polycrystalline cubic boron nitride diamond composite material according to claim 1, characterized in that: s3, molding:
(1) and (3) taking out the material prepared in the step (4), performing acid-base post-treatment and the like, and removing surface impurities to obtain the binderless polycrystalline diamond/cubic boron nitride sintered body composite material.
CN202111115556.1A 2021-09-23 2021-09-23 Preparation method of polycrystalline cubic boron nitride diamond composite material Pending CN113831127A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115259659A (en) * 2022-08-09 2022-11-01 深圳市正离子科技有限公司 Germanium-containing jade article and preparation process thereof

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