CN103924288B - Use the cubic boron nitride monocrystal micropowder preparation method and application of magnesio composite catalyst - Google Patents
Use the cubic boron nitride monocrystal micropowder preparation method and application of magnesio composite catalyst Download PDFInfo
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Abstract
The invention discloses a kind of cubic boron nitride monocrystal micropowder preparation method using magnesio composite catalyst, first, selection magnesio catalyst Mg3N2Making composite catalyst with the mixture of Mg, hBN powder is raw material；Weigh composite catalyst respectively and hBN powder puts into mix homogeneously in Vacuum mixer；Second, mixed uniformly composite catalyst and hBN powder are taken out, on forcing press, pre-molding is cylindrical synthesis bar, synthesis bar is assembled into Synthetic block, and puts into insulation in thermostatic drying chamber；3rd, Synthetic block is placed in the high pressure chest of cubic hinge press and carries out High Temperature High Pressure compound experiment, the 4th, High Temperature High Pressure is synthesized the sample broke obtained；Decontamination, obtains pure cBN monocrystalline micropowder after drying.The invention also discloses the application of this cBN monocrystalline micropowder.The cBN monocrystalline micropowder that the present invention produces, product crystal formation is irregular, has more rib cutting edge of a knife or a sword, good thermal stability, and self-sharpening is good, and grinding efficiency is high, may be machined and makes the product such as abrasive pastes, polishing agent.
Description
Technical field
The present invention relates to a kind of synthetic technology belonging to superhard material, a kind of cube nitridation using magnesio composite catalyst
Boron single crystal micropowder preparation method and application.
Background technology
Cubic boron nitride (cBN) is the superhard material of the synthetic not yet found in nature.Owing to cBN only has
Inferior to the high rigidity of diamond, the heat stability higher than diamond and high-temperature oxidation resistance, the most not with iron family element
The feature such as react, and can be made into grinding tool, cutter etc., have that grinding is sharp, working (machining) efficiency is high, machined surface quality is excellent,
Machining accuracy height, length in service life, energy-conservation and improve the advantages such as environment, be particularly well-suited to high-speed steel, heat resisting steel, rustless steel,
The accurate grinding processing of the material that the hardness such as thermo-sensitive material are high, toughness is big, elevated temperature strength is high, pyroconductivity is low.CBN monocrystalline
Micropowder refer to granularity < the cBN single crystal grain of 54 μm, has the advantages such as refractoriness height, Heat stability is good, wearability be good,
Can be applicable to the fine grinding of high request, essence is thrown or mirror finish, and in the production of high-grade abrasive pastes and Metallographic Analysis.
In the prior art, commercial production cBN monocrystalline micropowder mainly the most first synthesis cBN monocrystalline abrasive particle, then through pulverizing, whole
Shape processes, and uses special process to produce.CBN monocrystalline abrasive particle many employings Li and Ca synthesized by this method
And its nitride is catalyst material.Li and Ca is active noble metal, preserves and synthesizing nitride all has certain difficulty
Degree, relatively costly, synthesis technique is complex, and the product impurity content produced is higher, intensity is relatively low.
The prior art close with the present invention is entitled " to use Mg3N2And CaH2The method of synthesizing cubic boron nitride " patent
Application (patent No. 201010211951.5, Authorization Notice No. CN101869817A).This method is with Mg3N2For catalyst,
CaH2For additive.Wherein CaH2Corrosivity is strong, is the chemical substance of a kind of instability, and chemical reactivity is the highest, meets
Water or malaria easily react, and generate hydroxide, release hydrogen and can cause burning.Therefore, this side is used
Method synthesis cBN monocrystalline, it is necessary to paying special attention to preservation and the enforcement of High Temperature High Pressure synthesis technique of sample, technological process is the most multiple
Miscellaneous.And the cBN monocrystal conversion ratio that produced of this synthetic method relatively low be 30～40%, crystal grain size is relatively big,
Granularity, about 100 mesh, is not suitable for industrial mass manufacture cBN monocrystalline micropowder.
Summary of the invention
It is an object of the invention to as overcoming above-mentioned the deficiencies in the prior art, it is provided that a kind of cube nitridation using magnesio composite catalyst
Boron single crystal micropowder preparation method and application, magnesio catalyst Mg3N2With the mixture of Mg as composite catalyst, with rough six sides
Boron nitride (hBN) is that (rough hBN refers to synthesis, purity relatively low (referring generally to 90%～95%) in reacting furnace to raw material
HBN powder without high temperature refinement treatment.Refine and refer to be placed in vacuum drying oven, at high temperature rough hBN
(1400～2000 DEG C) remove hydrone, low boiling impurity, B2O3Deng, make the process technique that hBN purity improves), suitable
When synthesis pressure and at a temperature of synthesize the cBN monocrystalline micropowder that intensity is high, conversion ratio is high.The cBN monocrystalline micropowder produced,
Product crystal formation is irregular, has more rib cutting edge of a knife or a sword, good thermal stability, and self-sharpening is good, and grinding efficiency is high, may be machined to make and grinds
The mill product such as cream, polishing agent.
For achieving the above object, the present invention uses following technical proposals:
A kind of cubic boron nitride monocrystal micropowder preparation method using magnesio composite catalyst, including:
The first step, selects magnesio catalyst Mg3N2Making composite catalyst with the mixture of Mg, selecting purity is 90%～95%
HBN powder is raw material；It is 10～25: 75～90 on electronic balance, to weigh Mg and Mg respectively in mass ratio3N2, and put into
Mortar is uniformly mixed to form composite catalyst with spoon；
Second step, in mass ratio 10～20: 80～90 weigh composite catalyst and hBN powder on electronic balance respectively, and put
Enter in the Vacuum mixer at the uniform velocity rotated and mix, until mix homogeneously；
3rd step, takes out uniform mixed composite catalyst and hBN powder, and on frame type hydraulic press, pre-molding is close
Real cylinder synthesis bar, a size ofh=30mm；
4th step, the cylinder after pre-molding is synthesized bar and pyrophyllite block, graphite-pipe, pyrophillite ring, white clouds stone ring,
Graphite flake and conductive steel cap are assembled into pre-synthesis block；
5th step, puts into the pre-synthesis block assembled with 100～120 DEG C of preheatings in thermostatic drying chamber, and is incubated 10min；
6th step, is placed in the Synthetic block assembled in the high pressure chest of cubic hinge press and carries out High Temperature High Pressure compound experiment, synthesis
Temperature is 1300～1600 DEG C, and synthesis pressure is 3.8～5.5GPa, and generated time is 6～15min；
7th step, the sample broke that High Temperature High Pressure synthesis obtains is become diameter, and < the fritter bar of 5mm, puts into fritter bar
In beaker, add deionized water 500ml and boil 30min, to remove sample remaining hBN and sample after High Temperature High Pressure synthesizes
The pyrophillite powder of product surface attachment；
8th step, slowly outwells the solution after decocting in water in beaker, and adds 300ml aqueous slkali NaOH or KOH, boils
40min, with deionized water rinsing after filtering off the solution after soda boiling, to remove the hBN of residual；
9th step, adds 300ml Solution H Cl or HNO in beaker3, boil 40min, after the solution after acid being boiled filters off
Again with deionized water rinsing, to remove the graphite and metal impurities remained in the sample；
Tenth step, the cBN single crystal samples after processing is placed in the baking oven of 120～150 DEG C and is dried 6h, obtains pure after drying
CBN monocrystalline micropowder；The conversion ratio of cBN monocrystalline micro powder product is 50%～55%, and granularity is at 270 mesh～600 mesh.
The application of a kind of cubic boron nitride monocrystal micropowder using magnesio composite catalyst to prepare, adds the cBN monocrystalline micropowder of preparation
Work makes abrasive pastes or polishing agent product, is applied to optical glass producing, high technology ceramics or optical mould high accuracy grinding and polishing
In.
The present invention passes through magnesio catalyst Mg and Mg3N2Rationally being combined of catalyst, has obtained good being combined of a kind of synthetic effect
Catalyst, compensate for the deficiency using magnesio catalyst synthesis cBN monocrystalline conversion ratio relatively low, simplifies the production of cBN monocrystalline micropowder
Technique, reduces synthesis cost, and economic and social benefits are preferable.
Using the synthetic method in the present invention, the cBN monocrystalline corner angle of synthesis are sharp, have good thermal stability, self-sharpening good,
Grinding efficiency advantages of higher, may be machined and make the product such as abrasive pastes, polishing agent, is applied to optical glass producing, accurate pottery
In the high accuracy grinding and polishing such as porcelain and optical mould, rubbing down effect of product can be improved, improve Grinding Quality and precision, reduce
Mechanical loss, improves service life.
Accompanying drawing explanation
Fig. 1-Fig. 7 is respectively the product experiment effect figure of embodiment 1-7.
Detailed description of the invention
The present invention is further described with embodiment below in conjunction with the accompanying drawings.
Embodiment 1:
The first step, selects magnesio catalyst Mg3N2Making composite catalyst with the mixture of Mg, selecting purity is the hBN of 90%
Powder is raw material；It is on electronic balance respectively to weigh Mg and Mg at 10: 90 in mass ratio3N2, and put into medication in mortar
Spoon is uniformly mixed to form composite catalyst；
Second step, in mass ratio 10: 90 weigh composite catalyst and hBN powder on electronic balance respectively, and put at the uniform velocity
The Vacuum mixer rotated mixes, until mix homogeneously；
3rd step, takes out uniform mixed composite catalyst and hBN powder, and on frame-type forcing press, pre-molding is circle
Cylindricality synthesis bar；
4th step, the cylinder after pre-molding is synthesized bar and pyrophyllite block, graphite-pipe, pyrophillite ring, white clouds stone ring,
Graphite flake and conductive steel cap are assembled into pre-synthesis block；
5th step, puts into the pre-synthesis block assembled with 100 DEG C of preheatings in thermostatic drying chamber, and is incubated 10min；
6th step, is placed in the Synthetic block assembled in the high pressure chest of cubic hinge press and carries out High Temperature High Pressure compound experiment, synthesis
Temperature is 1600 DEG C, and synthesis pressure is 3.8GPa, and generated time is 6min；
7th step, becomes diameter < the fritter bar of 5mm by the sample broke that High Temperature High Pressure synthesis obtains.Fritter bar is put into
In beaker, add deionized water 500ml and boil 30min, to remove sample remaining hBN and sample after High Temperature High Pressure synthesizes
The pyrophillite powder of product surface attachment；
8th step, slowly outwells the solution after decocting in water in beaker, and adds 300ml aqueous slkali NaOH or KOH, boils
40min, with deionized water rinsing after filtering off the solution after soda boiling, to remove the hBN of residual；
9th step, adds 300ml Solution H Cl or HNO in beaker3, boil 40min, after the solution after acid being boiled filters off
Again with deionized water rinsing, to remove the graphite and metal impurities remained in the sample；
Tenth step, the cBN single crystal samples after processing is placed in the baking oven of 120 DEG C and is dried 6h, obtains pure cBN after drying
Monocrystalline micropowder；The conversion ratio of cBN monocrystalline micro powder product is 50%, and granularity is at 270 mesh～600 mesh.As it is shown in figure 1, synthesis
CBN monocrystalline corner angle sharp, there is good thermal stability, self-sharpening is good, grinding efficiency is high.
The cBN monocrystalline micropowder of preparation is processed into abrasive pastes or polishing agent product, is applied to optical glass producing, accurate pottery
In porcelain or optical mould high accuracy grinding and polishing.
Embodiment 2:
The first step, selects magnesio catalyst Mg3N2Making composite catalyst with the mixture of Mg, selecting purity is the hBN of 91%
Powder is raw material；It is on electronic balance respectively to weigh Mg and Mg at 15: 85 in mass ratio3N2, and put into medication in mortar
Spoon is uniformly mixed to form composite catalyst；
Second step, in mass ratio 10: 90 weigh composite catalyst and hBN powder on electronic balance respectively, and put at the uniform velocity
The Vacuum mixer rotated mixes, until mix homogeneously；
3rd step, takes out uniform mixed composite catalyst and hBN powder, and on frame-type forcing press, pre-molding is circle
Cylindricality synthesis bar；
4th step, the cylinder after pre-molding is synthesized bar and pyrophyllite block, graphite-pipe, pyrophillite ring, white clouds stone ring,
Graphite flake and conductive steel cap are assembled into pre-synthesis block；
5th step, puts into the pre-synthesis block assembled with 110 DEG C of preheatings in thermostatic drying chamber, and is incubated 10min；
6th step, is placed in the Synthetic block assembled in the high pressure chest of cubic hinge press and carries out High Temperature High Pressure compound experiment, synthesis
Temperature is 1550 DEG C, and synthesis pressure is 4.2GPa, and generated time is 7min；
7th step, becomes diameter < the fritter bar of 5mm by the sample broke that High Temperature High Pressure synthesis obtains.Fritter bar is put into
In beaker, add deionized water 500ml and boil 30min, to remove sample remaining hBN and sample after High Temperature High Pressure synthesizes
The pyrophillite powder of product surface attachment；
8th step, slowly outwells the solution after decocting in water in beaker, and adds 300ml aqueous slkali NaOH or KOH, boils
40min, with deionized water rinsing after filtering off the solution after soda boiling, to remove the hBN of residual；
9th step, adds 300ml Solution H Cl or HNO in beaker3, boil 40min, after the solution after acid being boiled filters off
Again with deionized water rinsing, to remove the graphite and metal impurities remained in the sample；
Tenth step, the cBN single crystal samples after processing is placed in the baking oven of 130 DEG C and is dried 6h, obtains pure cBN after drying
Monocrystalline micropowder；The conversion ratio of cBN monocrystalline micro powder product is 51%, and granularity is at 270 mesh～600 mesh.As in figure 2 it is shown, synthesis
CBN monocrystalline corner angle sharp, there is good thermal stability, self-sharpening is good, grinding efficiency is high.
The cBN monocrystalline micropowder of preparation is processed into abrasive pastes or polishing agent product, is applied to optical glass producing, accurate pottery
In porcelain or optical mould high accuracy grinding and polishing.
Embodiment 3:
The first step, selects magnesio catalyst Mg3N2Making composite catalyst with the mixture of Mg, selecting purity is the hBN of 92%
Powder is raw material；It is on electronic balance respectively to weigh Mg and Mg at 20: 80 in mass ratio3N2, and put into medication in mortar
Spoon is uniformly mixed to form composite catalyst；
Second step, in mass ratio 10: 90 weigh composite catalyst and hBN powder on electronic balance respectively, and put at the uniform velocity
The Vacuum mixer rotated mixes, until mix homogeneously；
3rd step, takes out uniform mixed composite catalyst and hBN powder, and on frame-type forcing press, pre-molding is circle
Cylindricality synthesis bar；
4th step, the cylinder after pre-molding is synthesized bar and pyrophyllite block, graphite-pipe, pyrophillite ring, white clouds stone ring,
Graphite flake and conductive steel cap are assembled into pre-synthesis block；
5th step, puts into the pre-synthesis block assembled with 120 DEG C of preheatings in thermostatic drying chamber, and is incubated 10min；
6th step, is placed in the Synthetic block assembled in the high pressure chest of cubic hinge press and carries out High Temperature High Pressure compound experiment, synthesis
Temperature is 1510 DEG C, and synthesis pressure is 4.5GPa, and generated time is 8min；
7th step, becomes diameter < the fritter bar of 5mm by the sample broke that High Temperature High Pressure synthesis obtains.Fritter bar is put into
In beaker, add deionized water 500ml and boil 30min, to remove sample remaining hBN and sample after High Temperature High Pressure synthesizes
The pyrophillite powder of product surface attachment；
8th step, slowly outwells the solution after decocting in water in beaker, and adds 300ml aqueous slkali NaOH or KOH, boils
40min, with deionized water rinsing after filtering off the solution after soda boiling, to remove the hBN of residual；
9th step, adds 300ml Solution H Cl or HNO in beaker3, boil 40min, after the solution after acid being boiled filters off
Again with deionized water rinsing, to remove the graphite and metal impurities remained in the sample；
Tenth step, the cBN single crystal samples after processing is placed in the baking oven of 140 DEG C and is dried 6h, obtains pure cBN after drying
Monocrystalline micropowder；The conversion ratio of cBN monocrystalline micro powder product is 52%, and granularity is at 270 mesh～600 mesh.As it is shown on figure 3, synthesis
CBN monocrystalline corner angle sharp, there is good thermal stability, self-sharpening is good, grinding efficiency is high.
The cBN monocrystalline micropowder of preparation is processed into abrasive pastes or polishing agent product, is applied to optical glass producing, accurate pottery
In porcelain or optical mould high accuracy grinding and polishing.
Embodiment 4:
The first step, selects magnesio catalyst Mg3N2Making composite catalyst with the mixture of Mg, selecting purity is the hBN of 93%
Powder is raw material；It is on electronic balance respectively to weigh Mg and Mg at 25: 75 in mass ratio3N2, and put into medication in mortar
Spoon is uniformly mixed to form composite catalyst；
Second step, in mass ratio 10: 90 weigh composite catalyst and hBN powder on electronic balance respectively, and put at the uniform velocity
The Vacuum mixer rotated mixes, until mix homogeneously；
3rd step, takes out uniform mixed composite catalyst and hBN powder, and on frame-type forcing press, pre-molding is circle
Cylindricality synthesis bar；
4th step, the cylinder after pre-molding is synthesized bar and pyrophyllite block, graphite-pipe, pyrophillite ring, white clouds stone ring,
Graphite flake and conductive steel cap are assembled into pre-synthesis block；
5th step, puts into the pre-synthesis block assembled with 105 DEG C of preheatings in thermostatic drying chamber, and is incubated 10min；
6th step, is placed in the Synthetic block assembled in the high pressure chest of cubic hinge press and carries out High Temperature High Pressure compound experiment, synthesis
Temperature is 1470 DEG C, and synthesis pressure is 4.7GPa, and generated time is 9min；
7th step, becomes diameter < the fritter bar of 5mm by the sample broke that High Temperature High Pressure synthesis obtains.Fritter bar is put into
In beaker, add deionized water 500ml and boil 30min, to remove sample remaining hBN and sample after High Temperature High Pressure synthesizes
The pyrophillite powder of product surface attachment；
8th step, slowly outwells the solution after decocting in water in beaker, and adds 300ml aqueous slkali NaOH or KOH, boils
40min, with deionized water rinsing after filtering off the solution after soda boiling, to remove the hBN of residual；
9th step, adds 300ml Solution H Cl or HNO in beaker3, boil 40min, after the solution after acid being boiled filters off
Again with deionized water rinsing, to remove the graphite and metal impurities remained in the sample；
Tenth step, the cBN single crystal samples after processing is placed in the baking oven of 150 DEG C and is dried 6h, obtains pure cBN after drying
Monocrystalline micropowder；The conversion ratio of cBN monocrystalline micro powder product is 53%, and granularity is at 270 mesh～600 mesh.As shown in Figure 4, synthesis
CBN monocrystalline corner angle sharp, there is good thermal stability, self-sharpening is good, grinding efficiency is high.
The cBN monocrystalline micropowder of preparation is processed into abrasive pastes or polishing agent product, is applied to optical glass producing, accurate pottery
In porcelain or optical mould high accuracy grinding and polishing.
Example 5:
The first step, selects magnesio catalyst Mg3N2Making composite catalyst with the mixture of Mg, selecting purity is the hBN of 94%
Powder is raw material；It is on electronic balance respectively to weigh Mg and Mg at 15: 85 in mass ratio3N2, and put into medication in mortar
Spoon is uniformly mixed to form composite catalyst；
Second step, in mass ratio 15: 85 weigh composite catalyst and hBN powder on electronic balance respectively, and put at the uniform velocity
The Vacuum mixer rotated mixes, until mix homogeneously；
3rd step, takes out uniform mixed composite catalyst and hBN powder, and on frame-type forcing press, pre-molding is circle
Cylindricality synthesis bar；
4th step, the cylinder after pre-molding is synthesized bar and pyrophyllite block, graphite-pipe, pyrophillite ring, white clouds stone ring,
Graphite flake and conductive steel cap are assembled into pre-synthesis block；
5th step, puts into the pre-synthesis block assembled with 115 DEG C of preheatings in thermostatic drying chamber, and is incubated 10min；
6th step, is placed in the Synthetic block assembled in the high pressure chest of cubic hinge press and carries out High Temperature High Pressure compound experiment, synthesis
Temperature is 1420 DEG C, and synthesis pressure is 4.9GPa, and generated time is 10min；
7th step, becomes diameter < the fritter bar of 5mm by the sample broke that High Temperature High Pressure synthesis obtains.Fritter bar is put into
In beaker, add deionized water 500ml and boil 30min, to remove sample remaining hBN and sample after High Temperature High Pressure synthesizes
The pyrophillite powder of product surface attachment；
8th step, slowly outwells the solution after decocting in water in beaker, and adds 300ml aqueous slkali NaOH or KOH, boils
40min, with deionized water rinsing after filtering off the solution after soda boiling, to remove the hBN of residual；
9th step, adds 300ml Solution H Cl or HNO in beaker3, boil 40min, after the solution after acid being boiled filters off
Again with deionized water rinsing, to remove the graphite and metal impurities remained in the sample；
Tenth step, the cBN single crystal samples after processing is placed in the baking oven of 140 DEG C and is dried 6h, obtains pure cBN after drying
Monocrystalline micropowder；The conversion ratio of cBN monocrystalline micro powder product is 55%, and granularity is at 270 mesh～600 mesh.As it is shown in figure 5, synthesis
CBN monocrystalline corner angle sharp, there is good thermal stability, self-sharpening is good, grinding efficiency is high.
The cBN monocrystalline micropowder of preparation is processed into abrasive pastes or polishing agent product, is applied to optical glass producing, accurate pottery
In porcelain or optical mould high accuracy grinding and polishing.
Embodiment 6:
The first step, selects magnesio catalyst Mg3N2Making composite catalyst with the mixture of Mg, selecting purity is the hBN of 94%
Powder is raw material；It is on electronic balance respectively to weigh Mg and Mg at 20: 80 in mass ratio3N2, and put into medication in mortar
Spoon is uniformly mixed to form composite catalyst；
Second step, in mass ratio 15: 85 weigh composite catalyst and hBN powder on electronic balance respectively, and put at the uniform velocity
The Vacuum mixer rotated mixes, until mix homogeneously；
3rd step, takes out uniform mixed composite catalyst and hBN powder, and on frame-type forcing press, pre-molding is circle
Cylindricality synthesis bar；
4th step, the cylinder after pre-molding is synthesized bar and pyrophyllite block, graphite-pipe, pyrophillite ring, white clouds stone ring,
Graphite flake and conductive steel cap are assembled into pre-synthesis block；
5th step, puts into the pre-synthesis block assembled with 120 DEG C of preheatings in thermostatic drying chamber, and is incubated 10min；
6th step, is placed in the Synthetic block assembled in the high pressure chest of cubic hinge press and carries out High Temperature High Pressure compound experiment, synthesis
Temperature is 1360 DEG C, and synthesis pressure is 5.52GPa, and generated time is 12min；
7th step, becomes diameter < the fritter bar of 5mm by the sample broke that High Temperature High Pressure synthesis obtains.Fritter bar is put into
In beaker, add deionized water 500ml and boil 30min, to remove sample remaining hBN and sample after High Temperature High Pressure synthesizes
The pyrophillite powder of product surface attachment；
8th step, slowly outwells the solution after decocting in water in beaker, and adds 300ml aqueous slkali NaOH or KOH, boils
40min, with deionized water rinsing after filtering off the solution after soda boiling, to remove the hBN of residual；
9th step, adds 300ml Solution H Cl or HNO in beaker3, boil 40min, after the solution after acid being boiled filters off
Again with deionized water rinsing, to remove the graphite and metal impurities remained in the sample；
Tenth step, the cBN single crystal samples after processing is placed in the baking oven of 125 DEG C and is dried 6h, obtains pure cBN after drying
Monocrystalline micropowder；The conversion ratio of cBN monocrystalline micro powder product is 54%, and granularity is at 270 mesh～600 mesh.As shown in Figure 6, synthesis
CBN monocrystalline corner angle sharp, there is good thermal stability, self-sharpening is good, grinding efficiency is high.
The cBN monocrystalline micropowder of preparation is processed into abrasive pastes or polishing agent product, is applied to optical glass producing, accurate pottery
In porcelain or optical mould high accuracy grinding and polishing.
Embodiment 7:
The first step, selects magnesio catalyst Mg3N2Making composite catalyst with the mixture of Mg, selecting purity is the hBN of 95%
Powder is raw material；It is on electronic balance respectively to weigh Mg and Mg at 25: 75 in mass ratio3N2, and put into medication in mortar
Spoon is uniformly mixed to form composite catalyst；
Second step, in mass ratio 15: 85 weigh composite catalyst and hBN powder on electronic balance respectively, and put at the uniform velocity
The Vacuum mixer rotated mixes, until mix homogeneously；
3rd step, takes out uniform mixed composite catalyst and hBN powder, and on frame-type forcing press, pre-molding is circle
Cylindricality synthesis bar；
4th step, the cylinder after pre-molding is synthesized bar and pyrophyllite block, graphite-pipe, pyrophillite ring, white clouds stone ring,
Graphite flake and conductive steel cap are assembled into pre-synthesis block；
5th step, puts into the pre-synthesis block assembled with 110 DEG C of preheatings in thermostatic drying chamber, and is incubated 10min；
6th step, is placed in the Synthetic block assembled in the high pressure chest of cubic hinge press and carries out High Temperature High Pressure compound experiment, synthesis
Temperature is 1300 DEG C, and synthesis pressure is 5.5GPa, and generated time is 15min；
7th step, becomes diameter < the fritter bar of 5mm by the sample broke that High Temperature High Pressure synthesis obtains.Fritter bar is put into
In beaker, add deionized water 500ml and boil 30min, to remove sample remaining hBN and sample after High Temperature High Pressure synthesizes
The pyrophillite powder of product surface attachment；
8th step, slowly outwells the solution after decocting in water in beaker, and adds 300ml aqueous slkali NaOH or KOH, boils
40min, with deionized water rinsing after filtering off the solution after soda boiling, to remove the hBN of residual；
9th step, adds 300ml Solution H Cl or HNO in beaker3, boil 40min, after the solution after acid being boiled filters off
Again with deionized water rinsing, to remove the graphite and metal impurities remained in the sample；
Tenth step, the cBN single crystal samples after processing is placed in the baking oven of 140 DEG C and is dried 6h, obtains pure cBN after drying
Monocrystalline micropowder；The conversion ratio of cBN monocrystalline micro powder product is 55%, and granularity is at 270 mesh～600 mesh.As it is shown in fig. 7, synthesis
CBN monocrystalline corner angle sharp, there is good thermal stability, self-sharpening is good, grinding efficiency is high.
The cBN monocrystalline micropowder of preparation is processed into abrasive pastes or polishing agent product, is applied to optical glass producing, accurate pottery
In porcelain or optical mould high accuracy grinding and polishing.
Although the detailed description of the invention of the present invention is described by the above-mentioned accompanying drawing that combines, but not to scope
Limiting, one of ordinary skill in the art should be understood that, on the basis of technical scheme, those skilled in the art are not required to
Various amendments that creative work to be paid can be made or deformation are still within protection scope of the present invention.
Claims (2)
1. use a cubic boron nitride monocrystal micropowder preparation method for magnesio composite catalyst, it is characterized in that, specifically comprise the following steps that
The first step, selects magnesio catalyst Mg3N2Making composite catalyst with the mixture of Mg, selecting purity is 90%～95%
HBN powder is raw material；It is 10～25: 75～90 on electronic balance, to weigh Mg and Mg respectively in mass ratio3N2, and put into
Mortar is uniformly mixed to form composite catalyst with spoon；
Second step, in mass ratio 10～20: 80～90 weigh composite catalyst and hBN powder on electronic balance respectively, and put
Enter in the Vacuum mixer at the uniform velocity rotated and mix, until mix homogeneously；
3rd step, takes out uniform mixed composite catalyst and hBN powder, and on frame-type forcing press, pre-molding is circle
Cylinder synthesis bar；
4th step, the cylinder after pre-molding is synthesized bar and pyrophyllite block, graphite-pipe, pyrophillite ring, white clouds stone ring,
Graphite flake and conductive steel cap are assembled into pre-synthesis block；
5th step, puts into the pre-synthesis block assembled with 100～120 DEG C of preheatings in thermostatic drying chamber, and is incubated 10min；
6th step, is placed in the Synthetic block assembled in the high pressure chest of cubic hinge press and carries out High Temperature High Pressure compound experiment, synthesis
Temperature is 1300～1600 DEG C, and synthesis pressure is 3.8～5.5GPa, and generated time is 6～15min；
7th step, becomes the sample broke that High Temperature High Pressure synthesis obtains the fritter bar of diameter ＜ 5mm, is put into by fritter bar
In beaker, add deionized water 500ml and boil 30min, to remove sample remaining hBN and sample after High Temperature High Pressure synthesizes
The pyrophillite powder of product surface attachment；
8th step, slowly outwells the solution after decocting in water in beaker, and adds 300ml aqueous slkali NaOH or KOH, boils
40min, with deionized water rinsing after filtering off the solution after soda boiling, to remove the hBN of residual；
9th step, adds 300ml Solution H Cl or HNO in beaker3, boil 40min, after the solution after acid being boiled filters off
Again with deionized water rinsing, to remove the graphite and metal impurities remained in the sample；
Tenth step, the cBN single crystal samples after processing is placed in the baking oven of 120～150 DEG C and is dried 6h, obtains pure after drying
CBN monocrystalline micropowder；The conversion ratio of cBN monocrystalline micro powder product is 50%～55%, and granularity is at 270 mesh～600 mesh.
2. use the cubic boron nitride monocrystal micropowder preparation method of magnesio composite catalyst as claimed in claim 1, it is characterized in that, will
The cBN monocrystalline micropowder of preparation is processed into abrasive pastes or polishing agent product, is applied to optical glass producing, high technology ceramics or light
Learn in mould high accuracy grinding and polishing.
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