CN113956848A - Processing method of cubic boron nitride micro powder - Google Patents
Processing method of cubic boron nitride micro powder Download PDFInfo
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- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 238000003672 processing method Methods 0.000 title claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 99
- 239000012535 impurity Substances 0.000 claims abstract description 40
- 229910052582 BN Inorganic materials 0.000 claims abstract description 34
- 238000007493 shaping process Methods 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000001514 detection method Methods 0.000 claims abstract description 13
- 238000004806 packaging method and process Methods 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims description 42
- 238000011282 treatment Methods 0.000 claims description 33
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 238000001816 cooling Methods 0.000 claims description 23
- 239000002253 acid Substances 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 230000007935 neutral effect Effects 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 15
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 10
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000011521 glass Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 229910017604 nitric acid Inorganic materials 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 238000010306 acid treatment Methods 0.000 claims description 8
- 239000003513 alkali Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 2
- 238000004643 material aging Methods 0.000 claims 1
- 238000000227 grinding Methods 0.000 abstract description 13
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 230000007547 defect Effects 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 abstract description 2
- 238000003754 machining Methods 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 4
- 239000013077 target material Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 3
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010902 jet-milling Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000002505 iron Chemical class 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
- C01B21/0648—After-treatment, e.g. grinding, purification
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C19/00—Other disintegrating devices or methods
- B02C19/06—Jet mills
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C23/00—Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
- B02C23/08—Separating or sorting of material, associated with crushing or disintegrating
- B02C23/14—Separating or sorting of material, associated with crushing or disintegrating with more than one separator
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1409—Abrasive particles per se
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/60—Compounds characterised by their crystallite size
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/38—Particle morphology extending in three dimensions cube-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- Chemical & Material Sciences (AREA)
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Abstract
The application belongs to the technical field of superhard material processing and manufacturing, and particularly relates to a processing method of cubic boron nitride micro powder. The method takes cubic boron nitride with 40-80 meshes as a raw material and comprises the operation steps of airflow crushing, shaping, impurity removal, sorting, detection, packaging and the like. The cubic boron nitride micro powder obtained by the processing method of the cubic boron nitride micro powder has the product characteristics of high purity, concentrated granularity and regular crystal form, can better overcome the defects of high production cost, low yield, long time consumption and the like when the cubic boron nitride micro powder is prepared by directly using a cubic press, and has better technical significance for processing and manufacturing related high-precision grinding tools.
Description
Technical Field
The application belongs to the technical field of superhard material processing and manufacturing, and particularly relates to a processing method of cubic boron nitride micro powder.
Background
Cubic boron nitride is used as an artificially synthesized superhard material and has wide application in the industries of machining and the like. In production, the cubic boron nitride is synthesized by hexagonal boron nitride and a catalyst at high temperature and high pressure. It has very high hardness, thermal stability and chemical inertness, its hardness is second to diamond, but its thermal stability is far higher than diamond, and it also has greater chemical stability to iron series metal elements.
In application, the grinding tool using the cubic boron nitride as the raw material has excellent grinding performance, can be used for grinding various materials and has better grinding quality. However, as the requirement for the quality of industrial machining is increased, especially as the machining technology of high-precision machine tools is rapidly developed, the requirement for the machining precision is higher and higher, and thus the requirement for grinding tools is higher. In the actual process of preparing the grinding tool taking the cubic boron nitride as the raw material, the diameter of the cubic boron nitride particles has direct influence on the processing performance of the related grinding tool, so that how to adjust the particle size of the cubic boron nitride particles has important technical significance on the preparation of the related grinding tool.
Disclosure of Invention
The application aims to provide a processing method of cubic boron nitride micro powder, thereby laying a certain technical foundation for adjusting the grain size of cubic boron nitride and further processing and manufacturing related grinding tools.
The technical solution adopted in the present application is detailed as follows.
A processing method of cubic boron nitride micro powder comprises the following steps:
(I) air flow crushing
Crushing a cubic boron nitride raw material with 40-80 meshes by adopting an airflow crushing mode, and further sequentially dividing the obtained airflow crushed material into a first-level material, a second-level material, a third-level material and other different levels according to the thickness degree of the particle size, so that the subsequent processing is facilitated;
during the air flow crushing, for example, a Shandong Dali heavy AB30 air flow crusher (the device is a material dry-method superfine crushing device combining a fluidized bed type air flow crusher and a self-flow-dividing classification technology) can be used for related operations; based on the target granularity output rate index, the corresponding airflow crushing process parameters are referred as: the crushing pressure is controlled to be 0.4-0.7MPa, and the internal negative pressure is controlled to be 0.02-0.07 MPa;
when the materials are classified after the airflow is broken, the three-stage classification method can be designed according to the following reference: primary D50 of 25-35 μm, secondary D50 of 6-16 μm, and tertiary D50 of 1-4 μm, wherein the D50 value represents the median of particle size detection of materials;
(II) reshaping and impurity removal
Performing popular shaping treatment on the air inflow of the airflow crushing material in the step (I) (when the shaping treatment is performed, materials of different grades can be respectively treated), so that the particle shape of the airflow crushing material is closer to a round shape (similar to a round shape);
the principle of the airflow shaping process is as follows: the drying air flow blows the materials in the cavity through a nozzle (for example, a Laval nozzle is adopted), and the particle shapes of the materials are closer to a quasi-circular shape through mutual rotation, collision and friction among the materials;
the parameters of the gas flow shaping process are referred to as: shaping under 0.2-0.6Mpa for 30-70 min;
the shaped material is further subjected to impurity removal treatment (in the production process, a small amount of metal or metal and nonmetal oxide, a small amount of carbon and the like can be doped into the cubic boron nitride micro powder); the impurity removal process comprises the steps of carrying out mixed acid impurity removal, mixed alkali impurity removal and secondary acid treatment on the materials (the impurity removal treatment process operation can be carried out in sequence or adjusted according to needs); specifically, the method comprises the following steps:
removing impurities by mixed acid: mixing the material with concentrated sulfuric acid (mass fraction 95%) and concentrated nitric acid (mass fraction 70%) in a glass reaction kettle, heating and stirring, reacting at 200 ℃ and 250 ℃ for 3-5h, cooling, and washing to be neutral;
during treatment, cubic boron nitride micro powder materials: mixed acid =1 g: 0.7-3 ml;
in the mixed acid, the volume ratio of concentrated nitric acid to concentrated sulfuric acid is 1: 5-9;
alkali mixing and impurity removal: uniformly mixing sodium hydroxide, potassium hydroxide and cubic boron nitride micro powder materials, reacting for 2-4 hours at 300-400 ℃, cooling after the reaction is finished (cooling to a certain temperature and adding water to accelerate cooling), and washing to be neutral;
during treatment, the mass ratio of sodium hydroxide: potassium hydroxide: cubic boron nitride material =3:2: 1-3;
secondary acid treatment: mixing cubic boron nitride micro powder material and aqua regia in a glass reaction kettle, heating and stirring, reacting at the temperature of 200 ℃ and 250 ℃ for 1-3h, cooling, and washing to be neutral;
when processed, cubic boron nitride material: aqua regia =1 g: 0.8-2.5 ml;
(III) sorting, detecting and packaging
And (3) according to the particle size, sorting the materials subjected to impurity removal treatment by using an automatic sorting machine, detecting the particle size (for example, detecting by using an S3500 series laser particle size analyzer), further drying the cubic boron nitride micro-powder materials qualified in detection, and packaging.
In actual production, the finest grain size of cubic boron nitride grains produced by a cubic press can reach 400 meshes (38 μm), but in practice, the direct preparation of finer grain size cubic boron nitride grains by the cubic press not only has the problem of high technical difficulty, but also has the defects of low typical yield and high cost. On the other hand, the actual high precision machining grinding tool preparation requires cubic boron nitride particles of 35 μm or less in diameter, and even finer to 1-10 μm. Therefore, further processing of the cubic boron nitride particles into ultra-fine cubic boron nitride micropowder is clearly necessary for high precision machining of the abrasive tools.
Based on factors such as cost and processing difficulty, the cubic boron nitride powder with the size of 40-80 meshes prepared by preliminary synthesis of a cubic press is selected as a raw material, and superfine cubic boron nitride micro powder is obtained through a plurality of series of processing treatments, so that a certain foundation is laid for the preparation of high-precision grinding tools.
In general, the cubic boron nitride micro powder obtained by the processing method of the cubic boron nitride micro powder has the product characteristics of high purity, concentrated granularity and regular crystal form, can better overcome the defects of high production cost, low yield, long time consumption and the like when the cubic boron nitride micro powder is prepared by directly using a cubic press, and has better technical significance for processing and manufacturing related high-precision grinding tools.
Drawings
FIG. 1 is a graph showing the particle size of the material before shaping in example 1;
FIG. 2 is a graph showing the particle size after shaping in example 1.
Detailed Description
The present application is further illustrated by the following examples.
Example 1
The specific process of the processing method of cubic boron nitride micro powder provided in this example is summarized as follows.
(I) air flow crushing
Taking cubic boron nitride of 40-80 meshes synthesized and prepared by a cubic press as a raw material, wherein the target granularity is 30-40 mu m, and adopting an airflow crushing mode;
when the materials are classified after the airflow is broken, the three-stage classification method can be designed according to the following reference: primary D50 of 25-35 μm, secondary D50 of 6-16 μm, and tertiary D50 of 1-4 μm, wherein the D50 value represents the median of particle size detection of materials;
when the airflow is crushed, the AB30 type airflow crusher which is heavily worked by Dalier in Shandong is adopted for relevant operation; the first-grade material is a target material, the design is carried out based on the target granularity output rate (the first-grade target material accounts for 70% of the total output material, and the first-grade material D50 is controlled to be 30-33 mu m), and the corresponding airflow crushing process parameters are as follows: controlling the shaping crushing pressure to be 0.4MPa and controlling the internal negative pressure to be 0.05 MPa; and when the crushed materials are classified, the primary classification frequency is 7.0, the secondary classification frequency is 25, and the frequency of an induced draft fan is 35.
(II) reshaping and impurity removal
Selecting the first-grade material in the step (I) for further shaping treatment;
the principle of the airflow shaping process is as follows: the drying air flow blows the materials in the cavity through the Laval nozzle, and the particle shapes of the materials are closer to a quasi-circular shape through mutual rotation, collision and friction among the materials;
the parameters of the gas flow shaping process are as follows: shaping pressure is 0.4Mpa, grading wheel frequency is 25, induced draft fan frequency is 40, and shaping time is 50 min.
The topography of the material before and after reshaping is shown in fig. 1 and fig. 2. It can be seen visually that the shaping treatment can effectively adjust the morphology of the material. Further detection results show that the D50 value of the shaped cubic boron nitride particles is 30.3-32.5, the circularity can reach 0.910, and the particle size and morphology are better improved.
Further removing impurities from the shaped cubic boron nitride micro powder material; the impurity removal treatment is to sequentially carry out mixed acid impurity removal, mixed alkali impurity removal and secondary acid treatment on the materials; specifically, the method comprises the following steps:
removing impurities by mixed acid: mixing a cubic boron nitride material with concentrated sulfuric acid (mass fraction 95%) and concentrated nitric acid (mass fraction 70%) in a glass reaction kettle, heating and stirring, reacting at 200 ℃ for 4 hours, cooling, and washing to be neutral;
during treatment, cubic boron nitride micro powder materials: mixed acid =1 g: 0.8 ml;
in the mixed acid, the volume ratio of concentrated nitric acid to concentrated sulfuric acid is 1: 6;
alkali mixing and impurity removal: uniformly mixing sodium hydroxide and potassium hydroxide with the cubic boron nitride micro powder material subjected to impurity removal by the mixed acid, reacting for 3 hours at 350 ℃, cooling (cooling to a certain temperature, adding water to accelerate cooling) after the reaction is finished, and washing to be neutral;
during treatment, the weight ratio of sodium hydroxide: potassium hydroxide: cubic boron nitride micro powder material =3:2: 3;
secondary acid treatment: mixing the cubic boron nitride material subjected to the impurity removal treatment with aqua regia in a glass reaction kettle, heating and stirring, reacting at 200 ℃ for 2 hours, cooling, and washing to be neutral;
during treatment, cubic boron nitride micro powder materials: aqua regia =1 g: 1 ml;
(III) sorting, detecting and packaging
And (3) according to the particle size, sorting the materials subjected to impurity removal treatment, detecting the particle size (by adopting an S3500 series laser particle size analyzer), further drying the cubic boron nitride micro-powder materials qualified in detection, and packaging.
Example 2
The operation related to this embodiment is substantially the same as that of embodiment 1, and only a part of the process parameters are adjusted as follows:
in the step (I), the particle size of 8-12 μm is taken as a target particle size: the crushing pressure is controlled to be 0.7MPa, and the internal negative pressure is controlled to be 0.04 MPa; primary stage frequency 16, secondary stage frequency 28 and induced draft fan frequency 32.
The obtained jet milling material is further divided into a first-level material, a second-level material and a third-level material according to the thickness degree of the particle size; the secondary material is a target material and accounts for about 60 percent of the total output material, and the secondary material D50 is controlled to be 9-10 mu m, wherein the value D50 represents the median of particle size detection of the material.
In the step (II), the second-level material in the step (I) is selected for further shaping treatment;
the parameters of the gas flow shaping process are as follows: shaping pressure is 0.4Mpa, grading wheel frequency is 22, induced draft fan frequency is 40, and shaping time is 70 min;
after the shaping is finished, the detection result shows that the D50 value is 9.0-9.7, the circularity of the shaped cubic boron nitride particles can reach 0.90, and the particle size and the morphology meet the requirements.
Further removing impurities from the materials; specifically, the method comprises the following steps:
removing impurities by mixed acid: mixing a cubic boron nitride material with concentrated sulfuric acid (mass fraction 95%) and concentrated nitric acid (mass fraction 70%) in a glass reaction kettle, heating and stirring, reacting at 200 ℃ for 5 hours, cooling, and washing to be neutral;
during treatment, cubic boron nitride micro powder materials: mixed acid =1 g: 1.5 ml;
in the mixed acid, the volume ratio of concentrated nitric acid to concentrated sulfuric acid is 1: 8;
alkali mixing and impurity removal: mixing sodium hydroxide and potassium hydroxide with the mixed acid, removing impurities, uniformly mixing, reacting at 350 ℃ for 4 hours, cooling after the reaction is finished (cooling to a certain temperature, adding water to accelerate cooling), and washing to be neutral;
during treatment, the weight ratio of sodium hydroxide: potassium hydroxide: cubic boron nitride micropowder material =3:2: 2;
secondary acid treatment: mixing the cubic boron nitride material subjected to the impurity removal treatment with aqua regia in a glass reaction kettle, heating and stirring, reacting at 200 ℃ for 3 hours, cooling, and washing to be neutral;
during treatment, cubic boron nitride micro powder materials: aqua regia =1 g: 1.5 ml;
(III) sorting, detecting and packaging
And (3) sorting the materials subjected to impurity removal treatment according to the particle size, detecting the particle size (by adopting an S3500 series laser particle size analyzer), further drying the cubic boron nitride micro-powder materials qualified in detection, and packaging.
Example 3
The operation related to this embodiment is substantially the same as that of embodiment 1, and only a part of the process parameters are adjusted as follows:
in the step (one), the granularity taking 1-2 μm as a target is as follows: the crushing pressure is controlled to be 0.7MPa, and the internal negative pressure is controlled to be 0.04 MPa; primary grading frequency 20, secondary grading frequency 30 and induced draft fan frequency 32.
The obtained jet milling material is further divided into a first-level material, a second-level material and a third-level material according to the thickness degree of the particle size; the third-level material is a target material and accounts for about 50% of the total output material, and the second-level material D50 is controlled to be about 1.5 mu m, wherein the D50 value represents the median of particle size detection of the material.
In the step (II), the second-level material in the step (I) is selected for further shaping treatment;
the parameters of the gas flow shaping process are as follows: shaping pressure is 0.4Mpa, grading wheel frequency is 20, induced draft fan frequency is 40, and shaping time is 90 min;
after the shaping is finished, the detection result shows that the D50 value is 1.50-1.57, the circularity of the shaped cubic boron nitride micro powder particles can reach 0.90, and the particle size and the morphology meet the requirements.
Further removing impurities from the materials; specifically, the method comprises the following steps:
removing impurities by mixed acid: mixing a cubic boron nitride material with concentrated sulfuric acid (mass fraction 95%) and concentrated nitric acid (mass fraction 70%) in a glass reaction kettle, heating and stirring, reacting at 200 ℃ for 5 hours, cooling, and washing to be neutral;
during treatment, cubic boron nitride micro powder materials: mixed acid =1 g: 2 ml;
in the mixed acid, the volume ratio of concentrated nitric acid to concentrated sulfuric acid is 1: 9;
alkali mixing and impurity removal: uniformly mixing sodium hydroxide and potassium hydroxide with the mixed acid and the materials after impurity removal, reacting for 5 hours at 350 ℃, cooling (cooling to a certain temperature, adding water to accelerate cooling) after the reaction is finished, and washing to be neutral;
during treatment, the weight ratio of sodium hydroxide: potassium hydroxide: cubic boron nitride micro powder material =3:2: 1;
secondary acid treatment: mixing the cubic boron nitride material subjected to the impurity removal treatment with aqua regia in a glass reaction kettle, heating and stirring, reacting at 200 ℃ for 3 hours, cooling, and washing to be neutral;
during treatment, cubic boron nitride micro powder materials: aqua regia =1 g: 2 ml;
(III) sorting, detecting and packaging
And (3) sorting the materials subjected to impurity removal treatment according to the particle size, detecting the particle size (for example, by adopting an S3500 series laser particle size analyzer), further drying the cubic boron nitride micro-powder materials qualified in detection, and packaging.
Claims (6)
1. A processing method of cubic boron nitride micro powder is characterized by comprising the following steps:
(I) air flow crushing
Crushing a cubic boron nitride raw material with 40-80 meshes by adopting an airflow crushing mode, and further grading the obtained airflow crushed material according to the thickness degree of the particle size, thereby facilitating subsequent processing treatment;
(II) reshaping and impurity removal
Shaping the airflow crushed material in the step (I) to enable the particle shape of the airflow crushed material to be closer to a circle;
the parameters of the gas flow shaping process are as follows: shaping under 0.2-0.6Mpa for 30-70 min;
further removing impurities from the shaped cubic boron nitride material; the impurity removal treatment is to carry out mixed acid impurity removal, mixed alkali impurity removal and secondary acid treatment on the material;
(III) sorting, detecting and packaging
And (4) according to the particle size, further sorting the cubic boron nitride material subjected to impurity removal treatment in the step (III), further detecting the particle size, further drying the qualified cubic boron nitride material, and packaging.
2. The method for processing and treating cubic boron nitride micropowder of claim 1, wherein in the step (one), the process parameters of the air current crushing are as follows: the crushing pressure is controlled at 0.4-0.7MPa, and the internal negative pressure is controlled at 0.02-0.07 MPa.
3. The method for processing cubic boron nitride micropowder of claim 1, wherein in the step (one), when classifying the material after the air current crushing, the three-stage classification method is designed as follows: primary D50, 25-35 μm, secondary D50, 6-16 μm, and tertiary D50, 1-4 μm, wherein the D50 value represents the median of particle size detection of materials.
4. The processing method of cubic boron nitride micropowder of claim 1, wherein in the step (two), the mixed acid impurity removal is: mixing the materials with concentrated sulfuric acid and concentrated nitric acid in a glass reaction kettle, heating and stirring, reacting at the temperature of 200-250 ℃ for 3-5h, cooling, and washing to be neutral;
during treatment, micro powder materials: mixed acid =1 g: 0.7-3 ml;
in the mixed acid, the volume ratio of concentrated nitric acid to concentrated sulfuric acid is 1: 5-9.
5. The processing method of cubic boron nitride micropowder of claim 1, wherein in the step (two), the alkali-mixing impurity removal is: uniformly mixing sodium hydroxide, potassium hydroxide and a cubic boron nitride material, reacting for 2-4 hours at 300-400 ℃, cooling after the reaction is finished, and washing to be neutral;
during treatment, the mass ratio of sodium hydroxide: potassium hydroxide: cubic boron nitride feed =3:2: 1-3.
6. The method for processing cubic boron nitride micropowder according to claim 1, wherein in the step (ii), the secondary acid treatment is: mixing cubic boron nitride material and aqua regia in a glass reaction kettle, heating and stirring, reacting at the temperature of 200 ℃ and 250 ℃ for 1-3h, cooling, and washing to be neutral;
when processed, cubic boron nitride material: aqua regia =1 g: 0.8-2.5 ml.
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| CN115106178A (en) * | 2022-06-24 | 2022-09-27 | 河南省豫星碳材有限公司 | Diamond micro-powder crystal form control method |
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| CN101891481A (en) * | 2010-07-12 | 2010-11-24 | 郑州中南杰特超硬材料有限公司 | Method for producing polycrystal cubic boron nitride abrasive materials |
| CN107805489A (en) * | 2017-10-12 | 2018-03-16 | 信阳市德隆超硬材料有限公司 | A kind of micro/nano level cubic boron nitride abrasive materials and preparation method thereof |
| CN112138835A (en) * | 2020-09-02 | 2020-12-29 | 郑州中南杰特超硬材料有限公司 | Shaping method of cubic boron nitride and application thereof |
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2021
- 2021-11-03 CN CN202111293170.XA patent/CN113956848A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891481A (en) * | 2010-07-12 | 2010-11-24 | 郑州中南杰特超硬材料有限公司 | Method for producing polycrystal cubic boron nitride abrasive materials |
| CN107805489A (en) * | 2017-10-12 | 2018-03-16 | 信阳市德隆超硬材料有限公司 | A kind of micro/nano level cubic boron nitride abrasive materials and preparation method thereof |
| CN112138835A (en) * | 2020-09-02 | 2020-12-29 | 郑州中南杰特超硬材料有限公司 | Shaping method of cubic boron nitride and application thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115106178A (en) * | 2022-06-24 | 2022-09-27 | 河南省豫星碳材有限公司 | Diamond micro-powder crystal form control method |
| CN115106178B (en) * | 2022-06-24 | 2024-01-16 | 河南省豫星碳材有限公司 | Crystal form control method of diamond micro powder |
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