CN115044978B - Preparation method of large-particle CBN - Google Patents
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- CN115044978B CN115044978B CN202210798418.6A CN202210798418A CN115044978B CN 115044978 B CN115044978 B CN 115044978B CN 202210798418 A CN202210798418 A CN 202210798418A CN 115044978 B CN115044978 B CN 115044978B
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
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- C30B29/10—Inorganic compounds or compositions
- C30B29/38—Nitrides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/10—Single-crystal growth directly from the solid state by solid state reactions or multi-phase diffusion
Abstract
The invention relates to a preparation method of large-particle CBN, which comprises the following steps: step 1): and (3) catalyst preparation: the catalyst is LiCoN; step 2): and (3) batching: mixing 8-15 parts of LiNaN and 85-92 parts of HBN materials according to the weight part ratio; step 3): cold isostatic pressing: sealing the materials mixed in the previous step, and performing isostatic pressing on a cold isostatic pressing machine under the pressure of 290-310 Mpa; step 4): crushing, sieving and pressing; step 5): and (3) assembling: filling the round bar stock formed in the previous step into a pyrophyllite block mechanism to form a synthetic block; step 6): synthesizing at high temperature and high pressure; step 7): chemical treatment; step 8): drying; step 9): screening; step 10): checking; step 11): packaging and warehousing; the invention has the advantages of high conversion rate, large formed particles, long service life, suitability for industrial production and simple process.
Description
Technical Field
The invention belongs to the technical field of cubic boron nitride, and particularly relates to a preparation method of large-particle CBN.
Background
Cubic boron nitride is extremely hard, has microhardness HV 7200-9800, is an insulator but is an excellent heat conductor, is also called cubic boron nitride, c-BN, beta-BN or z-BN (named as Zinc Blende (Zinc Blende) crystal structure), is a widely used industrial drilling and grinding tool, and Cubic Boron Nitride (CBN) is a superhard material with hardness which is only inferior to that of diamond, has many excellent characteristics of diamond, has higher thermal stability and chemical inertness to iron group metals and alloys thereof, is used as engineering materials, has been widely applied to the ferrous metal and alloy material processing industry, is also applied to a series of high-tech fields by virtue of excellent thermal, electrical, optical, acoustic and other properties, becomes a functional material with development prospect, and has low conversion rate, usually about 40-55%, extremely low individual synthesis rate, low raw material utilization rate, small formed particles and low grade influence on service life; therefore, it is very necessary to provide a large-particle CBN preparation method which has high conversion rate, large particle formation, long service life, suitability for industrial production, and simple process.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the large-particle CBN preparation method which has the advantages of high conversion rate, large formed particles, long service life, suitability for industrial production and simple process.
The technical scheme of the invention is as follows: the preparation method of the large-particle CBN comprises the following steps:
step 1): and (3) catalyst preparation: the catalyst is LiCoN;
step 2): and (3) batching: mixing 2-15 parts of LiNaN and 85-98 parts of HBN materials according to the weight part ratio;
step 3): cold isostatic pressing: sealing the materials mixed in the previous step, and performing isostatic pressing on a cold isostatic pressing machine under the pressure of 290-310 Mpa;
step 4): crushing, sieving and pressing the column: crushing the material formed by the pressing in the previous step, sieving, weighing the powder with set quality, putting the powder into a round die with the diameter of 46mm and the height of 62mm, and prepressing the powder into round bars with the height of 62mm on a hydraulic press;
step 5): and (3) assembling: filling the round bar stock formed in the previous step into a pyrophyllite block mechanism to form a synthetic block;
step 6): high-temperature high-pressure synthesis: putting the synthetic block formed in the previous step into a high-pressure cavity of a hexahedral top press, pressurizing to 4-6GPa, heating to 1300-1500 ℃ for 3-10h until the sample of the synthetic block is obtained;
step 7): chemical treatment: knocking and crushing a high-pressure synthetic block sample obtained by high-temperature high-pressure synthesis, putting the crushed material into a container, adding deionized water, boiling in water for 30min, stopping heating, precipitating at the bottom of the container due to high density of CBN monocrystal, filtering out the solution in the container, and flushing 3-5 times by adopting the deionized water; then collecting CBN at the bottom of the container, putting the CBN into a strong alkali solution, boiling for 20-40min, and washing with deionized water;
step 8): and (3) drying: after the steps, collecting CBN at the bottom of the container, putting the CBN into a strong acid solution, boiling for 20-40min, repeatedly flushing with deionized water, and then putting the obtained CBN into a baking oven at 130-160 ℃ for baking for 4h to obtain CBN crystals;
step 9): screening;
step 10): and (3) checking: observing the color of the CBN single crystal by adopting OM, observing the surface morphology of the CBN single crystal by adopting SEM, and measuring the static pressure intensity of the CBN single crystal by using an intensity measuring instrument;
step 11): packaging and warehousing.
The synthetic route of LiCoN is as follows: (1) 3Ca+2NH 3 →3CaH 2 +N 2 ②6CaH 2 +6Li+6NH 3 →6LiCaN+15H 2 。
The specific steps of the step 2 are as follows: and mixing LiCoN and HBN materials according to parts by weight, and putting the mixture into a vacuumized mixer for mixing for 1-3 hours.
The number of cold isostatic pressing times in the step 3 is 2-4.
The cold isostatic press in the step 3 adopts a frame type cold isostatic press.
The density of the round bar stock pre-pressed in the step 4 is 1.2-2.0 g/cm.
The hexahedral top press in the step 6 adopts a hexahedral top press with a cylinder diameter of phi 500mm, and the synthetic cavity is phi 40mm.
The strong alkali solution in the step 7 is NAOH solution or KOH solution.
The strong acid solution in the step 8 is a king water solution.
And in the step 9, a standard vibration screening machine is adopted for screening.
The invention has the following advantages: when the catalyst is used, liCoN high-quality catalyst is adopted, dynamic conditions are met, stable thermodynamic conditions, namely stable P-T conditions are met at stable high temperature, HBN is dissolved by the catalyst in a molten state, CBN crystals are separated out, crystal nuclei grow gradually under proper high temperature and high pressure conditions, and the CBN prepared by the method is monocrystalline, perfect in crystal form, prismatic in most of the crystal forms and small in quantity of flat crystals; the high-temperature high-pressure synthesis step of the invention determines the P-T region of the coarse-grain high-grade CBN; the high-temperature high-pressure synthesis step adopts a hexahedral top press with a phi 500mm cylinder diameter, a synthesis cavity is phi 40mm, in a nucleation stage, pressure, power and time parameters are adjusted to form crystal nucleus 'sparse but not thin', the pressure is increased and the power is reduced in a growth stage, the stability of pressure and temperature in the cavity is achieved, the shape of a generated CBN crystal is perfect, the synthesis time is greatly longer than the conventional CBN synthesis time, and the CBN single crystal with complete synthesis crystal form and large particles is obtained, the conversion rate is 70%, the static pressure intensity is higher, and the method is suitable for industrial production; the invention has the advantages of high conversion rate, large formed particles, long service life, suitability for industrial production and simple process.
Drawings
FIG. 1 is a schematic diagram of the pyrophyllite block mechanism of the large-particle CBN preparation method.
FIG. 2 shows the P-T region of high grade coarse particle CBN production of large particle CBN production.
Fig. 3 is a schematic diagram of a pressure power process curve of a large particle CBN preparation method.
Fig. 4 is a schematic SEM diagram one of synthesized coarse-size CBN crystals of the large-particle CBN preparation method.
Fig. 5 is a SEM schematic of synthesized coarse-size CBN crystals of the large-particle CBN preparation method, fig. two.
Fig. 6 is a SEM schematic of synthesized coarse-size CBN crystals of the large-particle CBN preparation method, three.
Fig. 7 is a SEM schematic of synthesized coarse-size CBN crystals of the large-particle CBN preparation method, fourth.
In the figure: 1. the device comprises a conductive steel ring 2, a conductive sheet 3, a regulating sheet 4, a graphite heating container 5, a sample 6, a composite liner tube 7 and a pressure transmission medium.
Detailed Description
The invention is further illustrated below with reference to examples.
Example 1
The preparation method of the large-particle CBN comprises the following steps:
step 1): and (3) catalyst preparation: the catalyst is LiCoN;
step 2): and (3) batching: mixing 4 parts of LiNaN and 88 parts of HBN materials according to the weight part ratio;
step 3): cold isostatic pressing: sealing the materials mixed in the previous step, and performing isostatic pressing on a cold isostatic pressing machine at the pressure of 290;
step 4): crushing, sieving and pressing the column: crushing the material formed by the pressing in the previous step, sieving, weighing the powder with set quality, putting the powder into a round die with the diameter of 46mm and the height of 62mm, and prepressing the powder into round bars with the height of 62mm on a hydraulic press;
step 5): and (3) assembling: filling the round bar stock formed in the previous step into a pyrophyllite block mechanism to form a synthetic block;
step 6): high-temperature high-pressure synthesis: loading the synthetic block formed in the previous step into a high-pressure cavity of a hexahedral top press, pressurizing to 4GPa, heating to 1300 ℃ for 3 hours until a sample of the synthetic block is obtained;
step 7): chemical treatment: knocking and crushing a high-pressure synthetic block sample obtained by high-temperature high-pressure synthesis, putting the crushed material into a container, adding deionized water, boiling in water for 30min, stopping heating, precipitating at the bottom of the container due to high density of CBN monocrystal, filtering out the solution in the container, and flushing 3-5 times by adopting the deionized water; then collecting CBN at the bottom of the container, putting the CBN into a strong alkali solution, boiling for 20-40min, and washing with deionized water;
step 8): and (3) drying: after the steps, collecting CBN at the bottom of the container, putting the CBN into a strong acid solution, boiling for 20-40min, repeatedly flushing with deionized water, and then putting the obtained CBN into a baking oven at 130-160 ℃ for baking for 4h to obtain CBN crystals;
step 9): screening;
step 10): and (3) checking: observing the color of the CBN single crystal by adopting OM, observing the surface morphology of the CBN single crystal by adopting SEM, and measuring the static pressure intensity of the CBN single crystal by using an intensity measuring instrument;
step 11): packaging and warehousing.
The CBN single crystal prepared in the embodiment has perfect crystal form and complete crystal form, and the granularity reaches 30/40, wherein the obtained CBN single crystal is single crystal, has perfect crystal form and prismatic surface, is mostly isosceles crystal, has a small amount of flat crystal, and has the conversion rate of 69.2%.
Example 2
The preparation method of the large-particle CBN comprises the following steps:
step 1): and (3) catalyst preparation: the catalyst is LiCoN;
step 2): and (3) batching: mixing 15 parts of LiNaN and 98 parts of HBN materials according to the weight part ratio;
step 3): cold isostatic pressing: sealing the materials mixed in the previous step, and performing isostatic pressing on a cold isostatic pressing machine under the pressure of 310 Mpa;
step 4): crushing, sieving and pressing the column: crushing the material formed by the pressing in the previous step, sieving, weighing the powder with set quality, putting the powder into a round die with the diameter of 46mm and the height of 62mm, and prepressing the powder into round bars with the height of 62mm on a hydraulic press;
step 5): and (3) assembling: filling the round bar stock formed in the previous step into a pyrophyllite block mechanism to form a synthetic block;
step 6): high-temperature high-pressure synthesis: loading the synthetic block formed in the previous step into a high-pressure cavity of a hexahedral top press, pressurizing to 5GPa, heating to 1500 ℃ for 5 hours, and waiting until a sample of the synthetic block is pressed at the high pressure;
step 7): chemical treatment: knocking and crushing a high-pressure synthetic block sample obtained by high-temperature high-pressure synthesis, putting the crushed material into a container, adding deionized water, boiling in water for 30min, stopping heating, precipitating at the bottom of the container due to high density of CBN monocrystal, filtering out the solution in the container, and flushing 3-5 times by adopting the deionized water; then collecting CBN at the bottom of the container, putting the CBN into a strong alkali solution, boiling for 20-40min, and washing with deionized water;
step 8): and (3) drying: after the steps, collecting CBN at the bottom of the container, putting the CBN into a strong acid solution, boiling for 20-40min, repeatedly flushing with deionized water, and then putting the obtained CBN into a baking oven at 130-160 ℃ for baking for 4h to obtain CBN crystals;
step 9): screening;
step 10): and (3) checking: observing the color of the CBN single crystal by adopting OM, observing the surface morphology of the CBN single crystal by adopting SEM, and measuring the static pressure intensity of the CBN single crystal by using an intensity measuring instrument;
step 11): packaging and warehousing.
The CBN single crystal prepared in the embodiment has perfect crystal form and complete crystal form, and the granularity reaches 30/40, wherein the obtained CBN single crystal is single crystal, has perfect crystal form and prismatic surface, is mostly isosceles crystal, has a small amount of flat crystal and has a conversion rate of 70%.
Example 3
The preparation method of the large-particle CBN is characterized by comprising the following steps: it comprises the following steps:
step 1): and (3) catalyst preparation: the catalyst is LiCoN;
step 2): and (3) batching: mixing 10 parts of LiCoN and 90 parts of HBN materials according to the weight part ratio;
step 3): cold isostatic pressing: sealing the materials mixed in the previous step, and performing isostatic pressing on a cold isostatic pressing machine at 300 Mpa;
step 4): crushing, sieving and pressing the column: crushing the material formed by the pressing in the previous step, sieving, weighing the powder with set quality, putting the powder into a round die with the diameter of 46mm and the height of 62mm, and prepressing the powder into round bars with the height of 62mm on a hydraulic press;
step 5): and (3) assembling: filling the round bar stock formed in the previous step into a pyrophyllite block mechanism to form a synthetic block;
step 6): high-temperature high-pressure synthesis: loading the synthetic block formed in the previous step into a high-pressure cavity of a hexahedral top press, pressurizing to 6GPa, heating to 1400 ℃ for 7h, and waiting until a sample of the synthetic block is pressed at the high pressure;
step 7): chemical treatment: knocking and crushing a high-pressure synthetic block sample obtained by high-temperature high-pressure synthesis, putting the crushed material into a container, adding deionized water, boiling in water for 30min, stopping heating, precipitating at the bottom of the container due to high density of CBN monocrystal, filtering out the solution in the container, and flushing 3-5 times by adopting the deionized water; then collecting CBN at the bottom of the container, putting the CBN into a strong alkali solution, boiling for 20-40min, and washing with deionized water;
step 8): and (3) drying: after the steps, collecting CBN at the bottom of the container, putting the CBN into a strong acid solution, boiling for 20-40min, repeatedly flushing with deionized water, and then putting the obtained CBN into a baking oven at 130-160 ℃ for baking for 4h to obtain CBN crystals;
step 9): screening;
step 10): and (3) checking: observing the color of the CBN single crystal by adopting OM, observing the surface morphology of the CBN single crystal by adopting SEM, and measuring the static pressure intensity of the CBN single crystal by using an intensity measuring instrument;
step 11): packaging and warehousing.
The CBN single crystal prepared in the embodiment has perfect crystal form and complete crystal form, and the granularity reaches 30/40, wherein the obtained CBN single crystal is single crystal, has perfect crystal form and prismatic surface, is mostly isosceles crystal, has a small amount of flat crystal and has the conversion rate of 69%.
Example 4
The preparation method of the large-particle CBN is characterized by comprising the following steps: it comprises the following steps:
step 1): and (3) catalyst preparation: the catalyst is LiCoN;
step 2): and (3) batching: mixing 8 parts of LiCoN and 91 parts of HBN materials according to the weight part ratio;
step 3): cold isostatic pressing: sealing the materials mixed in the previous step, and performing isostatic pressing on a cold isostatic pressing machine at 300 Mpa;
step 4): crushing, sieving and pressing the column: crushing the material formed by the pressing in the previous step, sieving, weighing the powder with set quality, putting the powder into a round die with the diameter of 46mm and the height of 62mm, and prepressing the powder into round bars with the height of 62mm on a hydraulic press;
step 5): and (3) assembling: filling the round bar stock formed in the previous step into a pyrophyllite block mechanism to form a synthetic block;
step 6): high-temperature high-pressure synthesis: loading the synthetic block formed in the previous step into a high-pressure cavity of a hexahedral top press, pressurizing to 6GPa, heating to 1300 ℃ for 10 hours until a sample of the synthetic block is obtained;
step 7): chemical treatment: knocking and crushing a high-pressure synthetic block sample obtained by high-temperature high-pressure synthesis, putting the crushed material into a container, adding deionized water, boiling in water for 30min, stopping heating, precipitating at the bottom of the container due to high density of CBN monocrystal, filtering out the solution in the container, and flushing 3-5 times by adopting the deionized water; then collecting CBN at the bottom of the container, putting the CBN into a strong alkali solution, boiling for 20-40min, and washing with deionized water;
step 8): and (3) drying: after the steps, collecting CBN at the bottom of the container, putting the CBN into a strong acid solution, boiling for 20-40min, repeatedly flushing with deionized water, and then putting the obtained CBN into a baking oven at 130-160 ℃ for baking for 4h to obtain CBN crystals;
step 9): screening;
step 10): and (3) checking: observing the color of the CBN single crystal by adopting OM, observing the surface morphology of the CBN single crystal by adopting SEM, and measuring the static pressure intensity of the CBN single crystal by using an intensity measuring instrument;
step 11): packaging and warehousing.
The CBN single crystal prepared in the embodiment has perfect crystal form and complete crystal form, and the granularity reaches 30/40, wherein the obtained CBN single crystal is single crystal, has perfect crystal form and prismatic surface, is mostly isosceles crystal, has a small amount of flat crystal and has a conversion rate of 58.4%.
Example 5
The preparation method of the large-particle CBN is characterized by comprising the following steps: it comprises the following steps:
step 1): and (3) catalyst preparation: the catalyst is LiCoN;
step 2): and (3) batching: mixing 15 parts of LiNaN and 85 parts of HBN materials according to the weight part ratio;
step 3): cold isostatic pressing: sealing the materials mixed in the previous step, and performing isostatic pressing on a cold isostatic pressing machine under the pressure of 310 Mpa;
step 4): crushing, sieving and pressing the column: crushing the material formed by the pressing in the previous step, sieving, weighing the powder with set quality, putting the powder into a round die with the diameter of 46mm and the height of 62mm, and prepressing the powder into round bars with the height of 62mm on a hydraulic press;
step 5): and (3) assembling: filling the round bar stock formed in the previous step into a pyrophyllite block mechanism to form a synthetic block;
step 6): high-temperature high-pressure synthesis: loading the synthetic block formed in the previous step into a high-pressure cavity of a hexahedral top press, pressurizing to 5GPa, heating to 1600 ℃ for 5 hours, and waiting until a sample of the synthetic block is pressed at the high pressure;
step 7): chemical treatment: knocking and crushing a high-pressure synthetic block sample obtained by high-temperature high-pressure synthesis, putting the crushed material into a container, adding deionized water, boiling in water for 30min, stopping heating, precipitating at the bottom of the container due to high density of CBN monocrystal, filtering out the solution in the container, and flushing 3-5 times by adopting the deionized water; then collecting CBN at the bottom of the container, putting the CBN into a strong alkali solution, boiling for 20-40min, and washing with deionized water;
step 8): and (3) drying: after the steps, collecting CBN at the bottom of the container, putting the CBN into a strong acid solution, boiling for 20-40min, repeatedly flushing with deionized water, and then putting the obtained CBN into a baking oven at 130-160 ℃ for baking for 4h to obtain CBN crystals;
step 9): screening;
step 10): and (3) checking: observing the color of the CBN single crystal by adopting OM, observing the surface morphology of the CBN single crystal by adopting SEM, and measuring the static pressure intensity of the CBN single crystal by using an intensity measuring instrument;
step 11): packaging and warehousing.
The CBN single crystal prepared in the embodiment has perfect crystal form and complete crystal form, and the granularity reaches 30/40, wherein the obtained CBN single crystal is single crystal, has perfect crystal form and prismatic surface, is mostly isosceles crystal, has a small amount of flat crystal, and has the conversion rate of 69.5%.
To further illustrate the performance of the present invention, specific effect data is provided below.
1. CBN synthesis results for the present invention.
TABLE 1 CBN synthesis results
2. The CBN particle size distribution is relevant to the present invention.
TABLE 2 CBN particle size distribution
3. 100 grains are extracted for static pressure intensity detection.
TABLE 3 static pressure intensity test results of CBN
Note that: the granularity intensity of 30/40 and 40/50 has no national standard prescribed value.
Claims (10)
1. The preparation method of the large-particle CBN is characterized by comprising the following steps: it comprises the following steps:
step 1): and (3) catalyst preparation: the catalyst is LiCoN;
step 2): and (3) batching: mixing 2-15 parts of LiNaN and 85-98 parts of HBN materials according to the weight part ratio;
step 3): cold isostatic pressing: sealing the materials mixed in the previous step, and performing isostatic pressing on a cold isostatic pressing machine under the pressure of 290-310 Mpa;
step 4): crushing, sieving and pressing the column: crushing the material formed by the pressing in the previous step, sieving, weighing the powder with set quality, putting the powder into a round die with the diameter of 46mm and the height of 62mm, and prepressing the powder into round bars with the height of 62mm on a hydraulic press;
step 5): and (3) assembling: filling the round bar stock formed in the previous step into a pyrophyllite block mechanism to form a synthetic block;
step 6): high-temperature high-pressure synthesis: putting the synthetic block formed in the previous step into a high-pressure cavity of a hexahedral top press, pressurizing to 4-6GPa, heating to 1300-1500 ℃ for 3-10h to obtain a high-pressure synthetic block sample;
step 7): chemical treatment: knocking and crushing a high-pressure synthetic block sample obtained by high-temperature high-pressure synthesis, putting the crushed material into a container, adding deionized water, boiling in water for 30min, stopping heating, precipitating at the bottom of the container due to high density of CBN monocrystal, filtering out the solution in the container, and flushing 3-5 times by adopting the deionized water; then collecting CBN at the bottom of the container, putting the CBN into a strong alkali solution, boiling for 20-40min, and washing with deionized water;
step 8): and (3) drying: after the steps, collecting CBN at the bottom of the container, putting the CBN into a strong acid solution, boiling for 20-40min, repeatedly flushing with deionized water, and then putting the obtained CBN into a baking oven at 130-160 ℃ for baking for 4h to obtain CBN crystals;
step 9): screening;
step 10): and (3) checking: observing the color of the CBN single crystal by adopting OM, observing the surface morphology of the CBN single crystal by adopting SEM, and measuring the static pressure intensity of the CBN single crystal by using an intensity measuring instrument;
step 11): packaging and warehousing.
2. The method for preparing large-particle CBN according to claim 1, wherein: the synthetic route of LiCoN is as follows: (1) 3Ca+2NH 3 →3CaH 2 +N 2 ②6CaH 2 +6Li+6NH 3 →6LiCaN+15H 2 。
3. The method for preparing large-particle CBN according to claim 1, wherein: the specific steps of the step 2 are as follows: and mixing LiCoN and HBN materials according to parts by weight, and putting the mixture into a vacuumized mixer for mixing for 1-3 hours.
4. The method for preparing large-particle CBN according to claim 1, wherein: the number of cold isostatic pressing times in the step 3 is 2-4.
5. A method of preparing large particle CBN as claimed in claim 3, wherein: the cold isostatic press in the step 3 adopts a frame type cold isostatic press.
6. The method for preparing large-particle CBN according to claim 1, wherein: the density of the round bar stock pre-pressed in the step 4 is 1.2-2.0 g/cm.
7. The method for preparing large-particle CBN according to claim 1, wherein: the hexahedral top press in the step 6 adopts a hexahedral top press with a cylinder diameter of phi 500mm, and the synthetic cavity is phi 40mm.
8. The method for preparing large-particle CBN according to claim 1, wherein: the strong alkali solution in the step 7 is NaOH solution or KOH solution.
9. The method for preparing large-particle CBN according to claim 1, wherein: the strong acid solution in the step 8 is a king water solution.
10. The method for preparing large-particle CBN according to claim 1, wherein: and in the step 9, a standard vibration screening machine is adopted for screening.
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| EP2177585B1 (en) * | 2003-08-20 | 2014-11-26 | Showa Denko K.K. | Cubic boron nitride, method for producing cubic boron nitride, grinding wheel with cubic boron nitride, and sintered cubic boron nitride compact |
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| CN101062766A (en) * | 2007-05-18 | 2007-10-31 | 河南中南工业有限责任公司 | Method for synthesizing coarse-grain degree cubic boron nitride |
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