CN108176329A - A kind of synthetic method of cubic boron nitride - Google Patents
A kind of synthetic method of cubic boron nitride Download PDFInfo
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- CN108176329A CN108176329A CN201711403907.2A CN201711403907A CN108176329A CN 108176329 A CN108176329 A CN 108176329A CN 201711403907 A CN201711403907 A CN 201711403907A CN 108176329 A CN108176329 A CN 108176329A
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- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/06—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
- B01J3/065—Presses for the formation of diamonds or boronitrides
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/0005—Catalytic processes under superatmospheric pressure
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- B01J2203/00—Processes utilising sub- or super atmospheric pressure
- B01J2203/06—High pressure synthesis
- B01J2203/065—Composition of the material produced
- B01J2203/066—Boronitrides
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Abstract
The present invention provides a kind of synthetic methods of cubic boron nitride, are the MgAlB using hBN as raw material14And Li3BN2Mixture for catalyst material, the synthesizing cubic boron nitride under high pressure high temperature.MgAlB used in the present invention14And Li3BN2Mixture for a kind of Novel catalyst material, improve the chemical inertness of catalyst material, further improve the conversion ratio of hBN and the quality of cBN during synthesis cBN.
Description
Technical field
The invention belongs to superhard material synthesis technical field, more particularly to a kind of synthetic method of cubic boron nitride.
Background technology
Cubic boron nitride（cBN）Thermal stability and chemistry with the high rigidity for being only second to diamond and better than diamond is lazy
Property, being used as superabrasive is made various grinding wheels and cutter, for the processing of ferrous material, has efficient, accurate, energy saving
The advantages that with automation, is particularly high-accuracy manufacture field in modern times processing and is used widely.
Up to the present, commercial scale is combined to cBN mainly using high pressure high temperature membrane by accelerant process, i.e., in high pressure high temperature item
Under part, with hexagonal boron nitride（hBN）For raw material, cBN is converted into the presence of catalyst and carries out crystal growth.Alkali metal, alkali
Earth metal and its nitride, boride, nitrogen boride are common catalyst materials, and this kind of material character is active, easily with oxygen, water
It reacts and performance is caused to deteriorate, influence the quality of the conversion ratio of hBN and the cBN of conversion.Chinese patent literature CN
100337733 C disclose a kind of cubic boron nitride and its manufacturing method, the oxidation in the patent for decrease catalyst, at it
Organic matter is added in catalyst, is covered in the surface of catalyst grains, completely cuts off the contact with oxygen or water, but this is readily incorporated other residuals
Impurity, have a great impact to the cBN intensity of synthesis.101323438 B of patent CN of same inventor disclose a kind of vertical
Square boron nitride synthetic method, the patent do catalyst using Mg-Al alloys and alkali metal, the mixture of alkaline-earth nitride, touch
Matchmaker's stability improves, and synthesis pressure temperature range is wide, but hBN conversion ratios are relatively low, and only 30% ~ 39%.
Since catalyst has vital influence to the synthesis of cBN, it is badly in need of finding new catalyst material to improve
The stability of catalyst, the conversion ratio of hBN and the quality for synthesizing cBN.
Invention content
To solve the deficiencies in the prior art, the present invention provides a kind of synthetic method of cubic boron nitride.This method
Using a kind of Novel catalyst materials synthesis cubic boron nitride, which stablizes, and has good chemical inertness,
The conversion ratio of hBN and the cBN mass of synthesis can be improved during synthesizing cubic boron nitride.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
A kind of synthetic method of cubic boron nitride is the MgAlB using hBN as raw material14And Li3BN2Mixture for catalyst material,
The synthesizing cubic boron nitride under high pressure high temperature, includes the following steps：
（1）The hBN of purity >=96% is selected as raw material, MgAlB14And Li3BN2Mixture be catalyst material；
（2）On three-dimensional material mixer be sufficiently mixed 5 ~ 8 hours after hBN raw materials and catalyst material are mixed in proportion；
（3）After mixing, mixture is pressed on a hydraulic press cylindric, is fitted into graphite heating body, is then charged into leaf
In cured stone assembling block；
（4）Assembled pyrophyllite block is put into cubic hinge press, in 4.0 ~ 5.1GPa of pressure, 1300 DEG C ~ 1800 DEG C of temperature
Under the conditions of heating synthesis 5 ~ 10 minutes；
（5）After synthesis, cBN monocrystalline is can obtain using soda acid purification processes.
As currently preferred technical solution, the hBN raw materials, MgAlB14And Li3BN2Granularity≤100 mesh.
As currently preferred technical solution, the mixed proportion of the hBN raw materials and catalyst material is, in mass ratio
Meter, hBN：MgAlB14：Li3BN2 =100:7~12:3~7。
As currently preferred technical solution, the mixed proportion of the hBN raw materials and catalyst material is, in mass ratio
Meter, hBN：MgAlB14：Li3BN2 =100:7~11:5~7。
As currently preferred technical solution, the mixed proportion of the hBN raw materials and catalyst material is, in mass ratio
Meter, hBN：MgAlB14：Li3BN2 =100:7~8.5:6~7。
Compared with prior art, beneficial effects of the present invention are：
（1）Present invention advantageously employs MgAlB14And Li3BN2Mixture for catalyst material synthesize hexagonal boron nitride, synthesis effect
Fruit is stablized, and hBN high conversion rates can reach 60% or so（At present in the method for synthesis cBN, the conversion ratio of hBN is usually less than 60%）,
It is high to synthesize cBN mass, is suitble to industrialized production.
（2）The MgAlB that the present invention uses14It is a kind of novel boride material, there is stable performance and chemical inertness；Boron
Lithium nitride（Li3BN2）It is a kind of more stable cBN synthetic catalyst materials of known performance, the mixture of two kinds of materials is as catalyst
Material improves the chemical inertness of catalyst material, further improves the conversion ratio of hBN and the quality of cBN during synthesis cBN.
Specific embodiment
The present invention provides one kind using hBN as raw material, MgAlB14And Li3BN2Mixture for catalyst material, in super-pressure height
The method of the lower synthesizing cubic boron nitride of temperature, specifically includes the following steps：
（1）The hBN of purity >=96% is selected as raw material, MgAlB14And Li3BN2Mixture be catalyst material；
（2）On three-dimensional material mixer be sufficiently mixed 5 ~ 8 hours after hBN raw materials and catalyst material are mixed in proportion；
（3）After mixing, mixture is pressed on a hydraulic press cylindric, is fitted into graphite heating body, is then charged into leaf
In cured stone assembling block；
（4）Assembled pyrophyllite block is put into cubic hinge press, in 4.0 ~ 5.1GPa of pressure, 1300 DEG C ~ 1800 DEG C of temperature
Under the conditions of heating synthesis 5 ~ 10 minutes；
（5）After synthesis, cBN monocrystalline is can obtain using soda acid purification processes.
The color of cBN monocrystalline that above-mentioned synthetic method obtains is light brown to black, and crystal is equivalance type, by sieving,
CBN monocrystalline particle size ranges between 60/70 ~ 325/400, peak value granularity be impact flexibility Ti measure after, Ti be in 50 ~ 60 it
Between, thus illustrate, cBN crystal quality prepared by synthetic method of the present invention is good.
Wherein, hBN raw materials, MgAlB in the present invention14And Li3BN2Granularity≤100 mesh, the purity of hBN raw materials >=
96%, specifically, hBN raw materials are purchased from Dandong day into the RH-A types of Science and Technology Ltd., MgAlB14And Li3BN2Commercially available lattice westerly
Agate aldrich（Shanghai）Trade Co., Ltd.HBN raw material grain sizes are thinner, are more conducive to the conversion of hBN.
In one embodiment of the invention, it counts in mass ratio, hBN：MgAlB14：Li3BN2=100:7~12:3 ~ 7,
Preferably, hBN：MgAlB14：Li3BN2=100:7~11:5 ~ 7, further preferably, hBN：MgAlB14：Li3BN2 =100:7~
8.5:6~7。
It is partly the prior art not described in preparation method of the present invention, such as the process of soda acid purification processes, not as
The innovative point of the present invention.
With reference to embodiment, the present invention is described in further detail.
Embodiment 1
In the present embodiment, the hBN of purity >=96% is selected as raw material, MgAlB14Add Li3BN2As catalyst；Raw material and catalyst
Granularity≤100 mesh, proportioning（Mass ratio）For hBN：MgAlB14：Li3BN2 =100:8.5:5；By raw material and catalyst in proportion
On three-dimensional material mixer be sufficiently mixed 6 hours after mixing；After mixing, mixture is pressed into cylinder on a hydraulic press
Shape, compact density 1.68g/cm3, it is fitted into graphite heating body, is then charged into pyrophillite assembling block；Assembled leaf is cured
Stone is put into cubic hinge press, heating synthesis 7 minutes under conditions of pressure 4.8GPa, 1500 DEG C of temperature；After synthesis, lead to
Peracid alkali purification processes obtain cBN monocrystalline, and color is in dark-brown, and cBN monocrystalline conversion ratio is 56%, and crystal is mostly equivalance type,
Particle size range is between 80/100 ~ 325/400, and for peak value granularity 120/140, impact flexibility Ti values are 54.
Embodiment 2
In the present embodiment, the hBN of purity >=96% is selected as raw material, MgAlB14Add Li3BN2As catalyst；Raw material and catalyst
Granularity≤100 mesh, proportioning（Mass ratio）For hBN：MgAlB14：Li3BN2=100:11:5；By raw material and catalyst in proportion
It carries out on three-dimensional material mixer being sufficiently mixed 7h after mixing；After mixing, mixture is pressed on a hydraulic press it is cylindric,
Compact density is 1.73g/cm3, it is fitted into graphite heating body, is then charged into pyrophillite assembling block；By assembled pyrophillite
Block is put into cubic hinge press, heating synthesis 9 minutes under conditions of pressure 5GPa, 1600 DEG C of temperature；After synthesis, by soda acid
Purification processes obtain cBN monocrystalline, and color is in black, and cBN monocrystalline conversion ratio is 50%, and crystal is mostly equivalance type, particle size range
Between 60/70 ~ 325/400, for peak value granularity 80/100, impact flexibility Ti values are 59.
Embodiment 3
In the present embodiment, the hBN of purity >=96% is selected as raw material, MgAlB14Add Li3BN2As catalyst；Raw material and catalyst
Granularity≤100 mesh, proportioning（Mass ratio）For hBN：MgAlB14：Li3BN2=100:7:6；Raw material and catalyst are mixed in proportion
It carries out on three-dimensional material mixer being sufficiently mixed 6h after conjunction；After mixing, mixture is pressed on a hydraulic press it is cylindric, into
Type density is 1.65g/cm3, it is fitted into graphite heating body, is then charged into pyrophillite assembling block；By assembled pyrophyllite block
Cubic hinge press is put into, heating synthesis 6 minutes under conditions of pressure 4.6GPa, 1480 DEG C of temperature；After synthesis, by soda acid
Purification processes obtain cBN monocrystalline, and color is in light brown, and cBN monocrystalline conversion ratio is 59%, and crystal is mostly equivalance type, granularity model
It is trapped among between 80/100 ~ 325/400, for peak value granularity 140/170, impact flexibility Ti values are 55.
Embodiment 4
In the present embodiment, the hBN of purity >=96% is selected as raw material, MgAlB14Add Li3BN2As catalyst；Raw material and catalyst
Granularity≤100 mesh, proportioning（Mass ratio）For hBN：MgAlB14：Li3BN2=100:7:6；Raw material and catalyst are mixed in proportion
It carries out on three-dimensional material mixer being sufficiently mixed 6h after conjunction；After mixing, mixture is pressed on a hydraulic press it is cylindric, into
Type density is 1.65g/cm3, it is fitted into graphite heating body, is then charged into pyrophillite assembling block；By assembled pyrophyllite block
Cubic hinge press is put into, heating synthesis 8 minutes under conditions of pressure 4.9GPa, 1500 DEG C of temperature；After synthesis, by soda acid
Purification processes obtain cBN monocrystalline, and color is in light brown, and cBN monocrystalline conversion ratio is 58%, and crystal is mostly equivalance type, granularity model
It is trapped among between 60/75 ~ 325/400, for peak value granularity 80/100, impact flexibility Ti values are 56.
Embodiment 5
In the present embodiment, the hBN of purity >=96% is selected as raw material, MgAlB14Add Li3BN2As catalyst；Raw material and catalyst
Granularity≤100 mesh, proportioning（Mass ratio）For hBN：MgAlB14：Li3BN2=100:8.5:7；By raw material and catalyst in proportion
It carries out on three-dimensional material mixer being sufficiently mixed 6h after mixing；After mixing, mixture is pressed on a hydraulic press it is cylindric,
Compact density is 1.75g/cm3, it is fitted into graphite heating body, is then charged into pyrophillite assembling block；By assembled pyrophillite
Block is put into cubic hinge press, heating synthesis 7 minutes under conditions of pressure 4.5GPa, 1450 DEG C of temperature；It, will be sour after synthesis
Alkali purification processes obtain cBN monocrystalline, and color is in light brown, and cBN monocrystalline conversion ratio is 57%, and crystal is mostly equivalance type, granularity
Range is between 80/100 ~ 325/400, and for peak value granularity 120/140, impact flexibility Ti values are 55.
Embodiment 6
In the present embodiment, the hBN of purity >=96% is selected as raw material, MgAlB14Add Li3BN2As catalyst；Raw material and catalyst
Granularity≤100 mesh, proportioning（Mass ratio）For hBN：MgAlB14：Li3BN2=100:12:3；By raw material and catalyst in proportion
It carries out on three-dimensional material mixer being sufficiently mixed 6h after mixing；After mixing, mixture is pressed on a hydraulic press it is cylindric,
Compact density is 1.73g/cm3, it is fitted into graphite heating body, is then charged into pyrophillite assembling block；By assembled pyrophillite
Block is put into cubic hinge press, heating synthesis 6 minutes under conditions of pressure 4.8GPa, 1560 DEG C of temperature；It, will be sour after synthesis
Alkali purification processes obtain cBN monocrystalline, and color is in light brown, and cBN monocrystalline conversion ratio is 57%, and crystal is mostly equivalance type, granularity
Range is between 80/100 ~ 325/400, and for peak value granularity 120/1370, impact flexibility Ti values are 53.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding without departing from the principles and spirit of the present invention can carry out these embodiments a variety of variations, modification, replace
And modification, the scope of the present invention is defined by the appended.
Claims (5)
1. a kind of synthetic method of cubic boron nitride is the MgAlB using hBN as raw material14And Li3BN2Mixture for catalyst material,
The synthesizing cubic boron nitride under high pressure high temperature, which is characterized in that include the following steps：
（1）The hBN of purity >=96% is selected as raw material, MgAlB14And Li3BN2Mixture be catalyst material；
（2）On three-dimensional material mixer be sufficiently mixed 5 ~ 8 hours after hBN raw materials and catalyst material are mixed in proportion；
（3）After mixing, mixture is pressed on a hydraulic press cylindric, is fitted into graphite heating body, is then charged into leaf
In cured stone assembling block；
（4）Assembled pyrophyllite block is put into cubic hinge press, in 4.0 ~ 5.1GPa of pressure, 1300 DEG C ~ 1800 DEG C of temperature
Under the conditions of heating synthesis 5 ~ 10 minutes；
（5）After synthesis, cBN monocrystalline is can obtain using soda acid purification processes.
2. a kind of synthetic method of cubic boron nitride according to claim 1, which is characterized in that the hBN raw materials,
MgAlB14And Li3BN2Granularity≤100 mesh.
3. a kind of synthetic method of cubic boron nitride according to claim 1, which is characterized in that the hBN raw materials and touch
The mixed proportion of catalytic material is to count in mass ratio, hBN：MgAlB14：Li3BN2 =100:7~12:3~7。
4. a kind of synthetic method of cubic boron nitride according to claim 1, which is characterized in that the hBN raw materials and touch
The mixed proportion of catalytic material is to count in mass ratio, hBN：MgAlB14：Li3BN2 =100:7~11:5~7。
5. a kind of synthetic method of cubic boron nitride according to claim 1, which is characterized in that the hBN raw materials and touch
The mixed proportion of catalytic material is to count in mass ratio, hBN：MgAlB14：Li3BN2 =100:7~8.5:6~7。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112981534A (en) * | 2021-03-12 | 2021-06-18 | 郑州中南杰特超硬材料有限公司 | Synthesis method of high-grade cubic boron nitride |
| CN113818072A (en) * | 2021-10-22 | 2021-12-21 | 郑州中南杰特超硬材料有限公司 | Hexagonal boron nitride single crystal growth method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101323438A (en) * | 2008-06-06 | 2008-12-17 | 郑州中南杰特超硬材料有限公司 | Cubic boron nitride synthetic method |
| JP2010235369A (en) * | 2009-03-31 | 2010-10-21 | Mitsubishi Materials Corp | Method of synthesizing cubic boron nitride and method of manufacturing cubic boron nitride sintered compact |
| CN103691363A (en) * | 2013-12-10 | 2014-04-02 | 太原理工大学 | Synthesis method of cubic boron nitride polycrystalline particles |
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2017
- 2017-12-22 CN CN201711403907.2A patent/CN108176329B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101323438A (en) * | 2008-06-06 | 2008-12-17 | 郑州中南杰特超硬材料有限公司 | Cubic boron nitride synthetic method |
| JP2010235369A (en) * | 2009-03-31 | 2010-10-21 | Mitsubishi Materials Corp | Method of synthesizing cubic boron nitride and method of manufacturing cubic boron nitride sintered compact |
| CN103691363A (en) * | 2013-12-10 | 2014-04-02 | 太原理工大学 | Synthesis method of cubic boron nitride polycrystalline particles |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112981534A (en) * | 2021-03-12 | 2021-06-18 | 郑州中南杰特超硬材料有限公司 | Synthesis method of high-grade cubic boron nitride |
| CN113818072A (en) * | 2021-10-22 | 2021-12-21 | 郑州中南杰特超硬材料有限公司 | Hexagonal boron nitride single crystal growth method |
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