CN106892663B - Lamellar nitride ceramic particles and preparation method thereof - Google Patents
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- 239000002245 particle Substances 0.000 title claims abstract description 89
- 239000000919 ceramic Substances 0.000 title claims abstract description 47
- 150000004767 nitrides Chemical class 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 18
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 14
- 230000007797 corrosion Effects 0.000 claims abstract description 10
- 238000005260 corrosion Methods 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 239000002159 nanocrystal Substances 0.000 claims abstract description 6
- 238000004519 manufacturing process Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000004321 preservation Methods 0.000 claims abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 16
- 239000010410 layer Substances 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000010439 graphite Substances 0.000 claims description 8
- 229910002804 graphite Inorganic materials 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 5
- 239000011241 protective layer Substances 0.000 claims description 5
- 238000005121 nitriding Methods 0.000 claims description 4
- 229910052720 vanadium Inorganic materials 0.000 claims description 4
- 238000003475 lamination Methods 0.000 claims description 3
- 229910052723 transition metal Inorganic materials 0.000 claims description 3
- 229910019637 Nb2AlC Inorganic materials 0.000 claims description 2
- 229910052758 niobium Inorganic materials 0.000 claims description 2
- 150000003624 transition metals Chemical group 0.000 claims description 2
- 241000446313 Lamella Species 0.000 claims 2
- 239000011159 matrix material Substances 0.000 abstract description 4
- 238000005728 strengthening Methods 0.000 abstract description 2
- SKKMWRVAJNPLFY-UHFFFAOYSA-N azanylidynevanadium Chemical compound [V]#N SKKMWRVAJNPLFY-UHFFFAOYSA-N 0.000 description 19
- CFJRGWXELQQLSA-UHFFFAOYSA-N azanylidyneniobium Chemical compound [Nb]#N CFJRGWXELQQLSA-UHFFFAOYSA-N 0.000 description 14
- 239000002243 precursor Substances 0.000 description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- INZDTEICWPZYJM-UHFFFAOYSA-N 1-(chloromethyl)-4-[4-(chloromethyl)phenyl]benzene Chemical compound C1=CC(CCl)=CC=C1C1=CC=C(CCl)C=C1 INZDTEICWPZYJM-UHFFFAOYSA-N 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- UNASZPQZIFZUSI-UHFFFAOYSA-N methylidyneniobium Chemical compound [Nb]#C UNASZPQZIFZUSI-UHFFFAOYSA-N 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000000441 X-ray spectroscopy Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- -1 transition metal nitride Chemical class 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/58007—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on refractory metal nitrides
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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- C—CHEMISTRY; METALLURGY
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3817—Carbides
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3817—Carbides
- C04B2235/3839—Refractory metal carbides
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/46—Gases other than oxygen used as reactant, e.g. nitrogen used to make a nitride phase
Abstract
The invention discloses a lamellar nitride ceramic particle and a preparation method thereof, wherein the nitrideThe ceramic particles are composed of multiple layers of nano crystal grains and have a laminated structure; the preparation process comprises the following steps: (1) mixing XnPutting the Al-C phase powder material into hydrofluoric acid with the mass concentration of 47% for corrosion, and corroding for 20-40 hours at the temperature of 40-60 ℃ to obtain lamellar carbide particles; (2) washing the carbide particles obtained in the step (1) until the PH value of a washing solution reaches 7, and then drying; (3) putting the carbide particles obtained in the step (2) into flowing nitrogen, carrying out heat preservation treatment for 1-4 hours at the temperature of 900-1300 ℃, and cooling to obtain a target product; the nitride ceramic particles prepared by the invention have a lamellar structure, can introduce a matrix material into lamellar gaps, play a role in strengthening, fitting and improving the performance, and have the advantages of simple preparation process and low production cost.
Description
Technical Field
The invention relates to nitride ceramic particles and a preparation method thereof, in particular to nitride ceramic particles with a lamellar structure and a preparation method thereof, wherein the nitride ceramic particles are composed of nanocrystals.
Background
Transition group metal nitride ceramics have good thermal stability, high hardness, high modulus and good electrical processability and are widely available in industry; for example, vanadium nitride is used as an additive of the cubic boron nitride die, and niobium nitride is used as a hard alloy additive, so that the service life of the tool can be greatly prolonged; in addition, the nitride electrode can be used as an electrode material of a super capacitor, and has very good chemical stability; the commercial nitride particles are usually irregular solid particles, and are dispersed in a matrix in a mixing mode in use to play a role in reinforcing and toughening, but the effect is poor.
Disclosure of Invention
The invention discloses nitride ceramic particles with a lamellar structure and composed of nanocrystals and a preparation method thereof.
The technical scheme adopted by the invention is as follows: the nitride ceramic particles are composed of multiple layers of nano crystal grains and have a laminated structure, the number of the layers of the laminated structure is 10-100, lamellar gaps are formed among the layers, and the layers are partially adhered to form the nitride ceramic particles. Each sheet layer of the lamination is a sheet-shaped nitride ceramic crystal grain, and the thickness of the sheet layer of the sheet-shaped nitride ceramic crystal grain is 10-100 nm.
Further, the nitride ceramic is a transition metal nitride ceramic, specifically, one of niobium nitride and vanadium nitride.
A preparation method of lamellar nitride ceramic particles comprises the following steps:
(1) mixing XnPutting the Al-C phase powder material into hydrofluoric acid with the mass concentration of 47% for corrosion, and corroding for 20-40 hours at the temperature of 40-60 ℃ to obtain lamellar carbide particles;
(2) washing the carbide particles obtained in the step (1) until the PH value of a washing solution reaches 7, and then drying;
(3) and (3) putting the carbide particles obtained in the step (2) into flowing nitrogen, carrying out heat preservation treatment for 1-4 hours at the temperature of 900-1300 ℃, and cooling to obtain the target product.
Further, in the step (1), X is a transition metal, and n is 2.
Further, in the step (1), X is Nb or V, namely Nb2AlC or V2AlC is a raw material for preparing niobium nitride or vanadium nitride ceramic particles with a lamellar structure.
Further, in the step (2), the drying is carried out at 20-60 ℃ for 24 hours.
Further, a protective layer is arranged on the surface of the carbide particles in the process from the step (2) to the step (3), and the protective layer can prevent the material from being polluted in the process of transferring.
Further, the protective layer comprises graphite paper arranged on the surfaces of the carbide particles and graphite powder arranged on the graphite paper; the graphite structure is stable and is not easy to react.
Further, the temperature rise rate of the nitriding treatment in the step (3) is 1-30 ℃/min, and X isnthe-Al-C phase ceramic has good thermal conductivity, and can uniformly transfer heat under the condition of the limit heating rate of 30 ℃/min, thereby being suitable for industrial production and greatly saving time and energy.
Furthermore, an oil bath is adopted for heating in the corrosion process in the step (1), so that the temperature can be stable and the heating is more uniform by adopting the oil bath for heating.
The invention has the beneficial effects that:
(1) the nitride ceramic particles have a lamellar structure, and a matrix material can be introduced into lamellar gaps, so that the effect of strengthening, fitting and improving the performance is achieved;
(2) the nitride ceramic particle sheet layer is composed of nanocrystalline, and can be used for preparing a nano composite material with excellent performance as an electrode;
(3) the preparation process of the invention does not need special process means, and has simple process, convenient preparation and convenient industrialized production.
Drawings
FIG. 1 is a scanning electron micrograph of a flaky vanadium carbide precursor in example 1.
FIG. 2 is a scanning electron micrograph of the plate-like niobium carbide precursor of example 3.
FIG. 3 is a scanning electron micrograph of the flaky vanadium nitride particles in example 1.
FIG. 4 is a scanning electron micrograph of the niobium nitride flake particles of example 3.
In fig. 5, curve a is the X-ray diffraction pattern of the vanadium nitride particles in example 1, and curve b is the X-ray diffraction pattern of the niobium nitride particles in example 3.
Detailed Description
The invention is further described with reference to the following figures and specific embodiments.
Example 1
Lamellar vanadium nitride particles were prepared according to the following procedure
(1) 2gV is mixed2Putting the AlC powder material into 50ml of hydrofluoric acid with the mass concentration of 47% for corrosion, and corroding the AlC powder material in an oil bath at the temperature of 60 ℃ for 20 hours to obtain lamellar carbide particles;
(2) washing the carbide particles obtained in the step (1) by using deionized water until the pH value of a washing solution reaches 7, and then drying the carbide particles for 24 hours in a vacuum drying oven at the temperature of 60 ℃;
(3) putting the carbide particles obtained in the step (2) into an alumina crucible, covering graphite paper on the surfaces of the particles, and covering a layer of graphite powder; the crucible was placed in a furnace and treated in flowing high purity nitrogen (99.9%) for 1 hour; preserving heat for 1 hour at 1300 ℃, and obtaining a target product after furnace cooling, wherein the heating rate is 1 ℃/min.
The thickness of the obtained lamellar vanadium nitride ceramic particles is 20 nanometers; FIG. 1 is a scanning electron microscope image of the flaky vanadium carbide ceramic particle precursor obtained in step (2), and it can be seen from the image that the typical lamellar structure of the precursor provides a very good template for subsequent heat treatment, so as to ensure that the nitride with the same lamellar structure is prepared; FIG. 3 is a drawing of the obtained lamellar vanadium nitride ceramic particles, which can be seen to have a unique lamination structure, each lamellar being composed of nanocrystalline vanadium nitride particles; table 1 shows the elemental composition of the ceramic particles obtained by X-ray spectroscopy, and it was found that there are nitrogen, oxygen and carbon elements, as well as a small amount of aluminum and a small amount of fluorine in the vanadium nitride particles, probably due to the small amount of alumina formed during the treatment and the resulting nitride doped with a small amount of carbon to form a vanadium carbonitride compound; all diffraction peaks are sharp as shown in curve a in fig. 5, indicating that the crystallinity of the crystal grains is very good and the prepared lamellar vanadium nitride ceramic particles have few defects.
TABLE 1X-ray energy spectrum element content analysis table of vanadium nitride particles
Example 2
Lamellar vanadium nitride particles were prepared according to the following procedure
(1) Mixing 5gV2Placing the AlC powder material into 100ml of hydrofluoric acid with the mass concentration of 47% for corrosion, and corroding in an oil bath at the temperature of 40 ℃ for 20 hours to obtain lamellar carbide particles;
(2) washing the carbide particles obtained in the step (1) by using deionized water until the pH value of a washing solution reaches 7, and then drying the carbide particles for 24 hours in a vacuum drying oven at the temperature of 20 ℃;
(3) putting the carbide particles obtained in the step (2) into an alumina crucible, covering graphite paper on the surfaces of the particles, and covering a layer of graphite powder; the crucible was placed in a furnace and treated in flowing high purity nitrogen (99.9%) for 4 hours; preserving heat for 1 hour at 900 ℃, and obtaining a target product after furnace cooling, wherein the heating rate is 30 ℃/min.
The obtained lamellar vanadium nitride ceramic particles have the lamellar thickness of 14.8 nanometers.
Example 3
The lamellar niobium nitride particles were prepared as follows
(1) 5gNb2Putting the AlC powder material into 200ml of hydrofluoric acid with the mass concentration of 47% for corrosion, and corroding in an oil bath at the temperature of 50 ℃ for 30 hours to obtain lamellar carbide particles;
(2) washing the carbide particles obtained in the step (1) with deionized water until the pH value of a washing solution reaches 7, and then drying the carbide particles in a vacuum drying oven at 40 ℃ for 24 hours;
(3) putting the carbide particles obtained in the step (2) into an alumina crucible, covering graphite paper on the surfaces of the particles, and covering a layer of graphite powder; the crucible was placed in a furnace and treated in flowing high purity nitrogen (99.9%) for 3 hours; and (3) preserving heat for 3 hours at 1100 ℃, and cooling along with the furnace to obtain a target product, wherein the heating rate is 20 ℃/min.
The thickness of the obtained lamellar niobium nitride ceramic particles is 100 nanometers.
FIG. 2 is a scanning electron microscope image of the flaky niobium carbide ceramic particle precursor obtained in step (2), from which it can be seen that the typical lamellar structure of the precursor provides a very good template for subsequent heat treatment, which can ensure that the nitride with the same lamellar structure is prepared; FIG. 4 shows the obtained lamellar niobium nitride ceramic particles, which are seen to have a unique laminated structure, each lamellar being composed of nanocrystalline vanadium nitride particles; table 1 shows the elemental composition of the ceramic particles obtained by X-ray spectroscopy, and it was found that the presence of nitrogen, oxygen and carbon elements, as well as a small amount of aluminum and a small amount of fluorine elements in the niobium nitride particles, probably due to the small amount of alumina formed during the treatment and the resulting nitrides doped with a small amount of carbon, form vanadium carbonitride compounds; all diffraction peaks are sharp as shown in the curve b in fig. 5, indicating that the crystallinity of the crystal grains is very good and the defects of the prepared lamellar niobium nitride ceramic particles are few.
TABLE 2X-ray energy spectrum element content analysis table of niobium nitride particles
Example 4
Lamellar vanadium nitride particles were prepared according to the following procedure
(1) 2gNb2Placing the AlC powder material into 30ml of hydrofluoric acid with the mass concentration of 47% for corrosion, and corroding in an oil bath for 40 hours at the temperature of 40 ℃ to obtain lamellar carbide particles;
(2) washing the carbide particles obtained in the step (1) by using deionized water until the pH value of a washing solution reaches 7, and then drying the carbide particles for 24 hours in a vacuum drying oven at the temperature of 20 ℃;
(3) putting the carbide particles obtained in the step (2) into an alumina crucible, covering graphite paper on the surfaces of the particles, and covering a layer of graphite powder; the crucible was placed in a furnace and treated in flowing high purity nitrogen (99.9%) for 2 hours; preserving heat for 2 hours at 1000 ℃, and obtaining a target product after furnace cooling, wherein the heating rate is 10 ℃/min.
The thickness of the obtained lamellar niobium nitride ceramic particles is 88.4 nanometers.
The lamellar vanadium nitride and niobium nitride ceramic particles prepared by the method have unique structures and are obviously different from the commercial solid ceramic particles at present; for example: (j. alloys compad., 464,75-80(2008)) using a precursor nitridation process to produce vanadium nitride nanoparticles having a grain size of about 50 nm as an aggregated nanoparticle collection; (j. alloys compact, 389,296-8(2005)) using a hydrothermal method to synthesize ceramic particles with a size of 10-20 nm as agglomerates of nanoparticles; the method takes the laminar vanadium carbide and niobium carbide ceramic particles prepared by corrosion as precursors, and after the precursors are treated by a simple high-temperature nitriding process, the laminar ceramic particles composed of nitride nanocrystals are obtained by in-situ nitriding; the prepared lamellar vanadium nitride and niobium nitride ceramic particles have special microstructures, can be used as matrix reinforcing phases and electrode materials of super capacitors, and have the advantages of simple structural process and low production cost.
Claims (4)
1. A preparation method of lamellar nitride ceramic particles is characterized by comprising the following steps:
(1) mixing XnPutting the Al-C phase powder material into hydrofluoric acid with the mass concentration of 47% for corrosion, and corroding for 20-40 hours at the temperature of 40-60 ℃ to obtain lamellar carbide particles;
(2) washing the carbide particles obtained in the step (1) until the pH value of a washing solution reaches 7, and then drying;
(3) putting the carbide particles obtained in the step (2) into flowing nitrogen, carrying out heat preservation treatment for 1-4 hours at the temperature of 900-1300 ℃, and cooling to obtain a target product;
arranging a protective layer on the surface of the carbide particles in the process from the step (2) to the step (3); the protective layer comprises graphite paper arranged on the surface of the carbide particles and graphite powder arranged on the graphite paper;
the nitride ceramic particles are composed of multiple layers of nano crystal grains and have a laminated structure, the number of the layers of the laminated structure is 10-100, lamellar gaps are formed among the layers, and the layers are partially adhered to form the nitride ceramic particles; each lamella of the lamination consists of nitride ceramic polycrystalline particles, and the lamella thickness of the lamellar nitride ceramic crystal grains is 10-100 nm;
in the step (1), X is a transition metal, and n is 2; in the step (1), X is one of Nb or V, namely Nb2AlC or V2AlC。
2. The method for preparing lamellar nitride ceramic particles according to claim 1, characterized in that in step (2) drying is carried out at 20-60 ℃ for 24 hours.
3. The method for producing platelet-shaped nitride ceramic particles according to claim 1, characterized in that: the temperature rise rate of the nitriding treatment in the step (3) is 1-30 ℃/min.
4. The method for producing platelet-shaped nitride ceramic particles according to claim 1, characterized in that: and (2) adopting oil bath heating in the corrosion process in the step (1).
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