CN115196967A - Method for preparing nano powder modified silicon carbide composite ceramic by spark plasma sintering - Google Patents
Method for preparing nano powder modified silicon carbide composite ceramic by spark plasma sintering Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 64
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical class [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 239000011858 nanopowder Substances 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000002490 spark plasma sintering Methods 0.000 title claims abstract description 17
- 239000002131 composite material Substances 0.000 title claims description 19
- 238000005245 sintering Methods 0.000 claims abstract description 31
- 239000002994 raw material Substances 0.000 claims abstract description 25
- 229910052580 B4C Inorganic materials 0.000 claims abstract description 23
- 238000002156 mixing Methods 0.000 claims abstract description 22
- 238000000498 ball milling Methods 0.000 claims abstract description 21
- 238000005469 granulation Methods 0.000 claims abstract description 16
- 230000003179 granulation Effects 0.000 claims abstract description 16
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 16
- 239000007921 spray Substances 0.000 claims abstract description 16
- 238000004321 preservation Methods 0.000 claims abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 73
- 229910002804 graphite Inorganic materials 0.000 claims description 50
- 239000010439 graphite Substances 0.000 claims description 50
- 239000011268 mixed slurry Substances 0.000 claims description 25
- 239000000843 powder Substances 0.000 claims description 25
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 20
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims description 12
- 235000015895 biscuits Nutrition 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 8
- 239000011230 binding agent Substances 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000002270 dispersing agent Substances 0.000 claims description 7
- 238000003760 magnetic stirring Methods 0.000 claims description 7
- 238000003825 pressing Methods 0.000 claims description 7
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium group Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 229920000058 polyacrylate Polymers 0.000 claims description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 5
- 238000011068 loading method Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 4
- 229910010271 silicon carbide Inorganic materials 0.000 description 15
- 150000003376 silicon Chemical class 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 5
- 229910052581 Si3N4 Inorganic materials 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 238000005452 bending Methods 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000002159 nanocrystal Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention relates to a method for preparing nano powder modified silicon carbide complex phase ceramic by spark plasma sintering, belonging to the technical field of armor protection materials, comprising the following steps: s1, primary mixing of raw materials; s2, ball milling and mixing; s3, spray granulation; s4, prepressing and forming; s5, assembling and sintering; the nano powder modified silicon carbide complex phase ceramic prepared according to the method is nano powder modified silicon carbide-boron carbide complex phase ceramic or nano powder modified silicon carbide-graphene complex phase ceramic. The discharge plasma sintering technology adopted by the invention has the advantages of rapid preparation and simple process, can prepare the complex phase ceramic with fine, uniform and high toughness grains at lower temperature in a shorter time, and solves the problem of excessive growth of nano grains caused by overhigh sintering temperature and overlong heat preservation time in other sintering technologies.
Description
Technical Field
The invention belongs to the technical field of elastic-resistant ceramic materials, and particularly relates to a method for preparing nano powder modified silicon carbide complex phase ceramic by spark plasma sintering.
Background
With the rapid development of science and technology, especially the development of the fields of energy, automobile industry, armor protection and the like, the requirements on the performance of materials are more and more strict. Particularly, in the high temperature parts in the above fields, development of a novel structural material having light weight, high strength and high temperature resistance is urgently required. Silicon carbide (SiC) ceramics developed in recent years have good chemical stability and unique electrical properties due to their mechanical properties of high strength, high hardness, wear resistance, thermal properties of high temperature resistance, low thermal expansion coefficient, high thermal conductivity and shock resistance. The ceramic material has attracted wide interest and attention in the scientific and industrial fields, becomes an important high-temperature structural ceramic, and has very important application prospect.
Although silicon carbide has many advantages, its disadvantages are also quite apparent. Firstly, silicon carbide is a compound with strong covalent bond property, has high melting point and small self-diffusion coefficient, so that the diffusion rate is low during sintering, the sintering property is poor, the silicon carbide is difficult to form, and a densified structure is difficult to obtain even under the process conditions of high temperature and high pressure; secondly, the silicon carbide ceramic has a severe brittleness tendency at room temperature, and is one of the reasons for difficult processing and forming due to low fracture toughness, so that the application of the material in the engineering field is limited to a great extent. In order to solve the above problems, various preparation methods have been developed, and the traditional methods of hot-pressing sintering, hot isostatic pressing, etc. for preparing silicon carbide ceramics are difficult to ensure the size of crystal grains, and the requirement of densification can be met under the conditions of high temperature and high pressure. And the spark plasma sintering can obviously inhibit the coarsening of crystal grains due to the advantages of rapid temperature rise, short sintering time, low sintering temperature and the like, has great advantages for preparing high-density and fine-grain ceramics, and is a novel energy-saving and environment-friendly processing technology.
The sintering mode is changed, and methods such as adding a second phase or a sintering aid and the like are used for promoting the sintering of the silicon carbide and improving the mechanical property of the silicon carbide. Therefore, the silicon carbide-based complex phase ceramic prepared by selecting a proper sintering mode and an addition phase has important significance on the research work of the silicon carbide ceramic.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for preparing nano powder modified silicon carbide complex phase ceramic by spark plasma sintering, so as to solve the technical problem of nano crystal grain growth at higher sintering temperature.
The specific technical scheme for solving the technical problems is as follows:
the method for preparing the nano powder modified silicon carbide composite ceramic by spark plasma sintering is characterized by comprising the following steps of:
s1, primary mixing of raw materials: mixing raw materials of silicon carbide powder, nano boron carbide powder and carbon powder or raw materials of silicon carbide powder, multi-layer graphene and carbon powder with deionized water, and performing magnetic stirring and ultrasonic dispersion at room temperature to obtain uniform mixed slurry;
s2, ball milling and mixing: adding an organic binder and a dispersant into the mixed slurry, and performing ball-milling wet mixing on the mixed slurry in a ball-milling tank by using zirconia grinding balls to obtain wet mixed slurry;
s3, spray granulation: carrying out spray granulation on the wet mixed slurry, controlling the spray pressure to be 0.2-0.4 MPa, the inlet temperature to be 140-170 ℃ and the outlet temperature to be 60-110 ℃ to prepare granulated powder with the granularity of 90-240 mu m;
s4, pre-pressing and forming: prepressing the granulation powder by using a tablet press, keeping the pressure for 15-25 s to prepare a ceramic biscuit, wherein the loading pressure range is 15-20 MPa;
s5, assembling and sintering: and (2) putting the pressed ceramic biscuit into a graphite mold, wherein a layer of graphite paper is lined in the graphite mold, a graphite felt is wrapped outside the graphite mold, graphite pressure heads are placed on two sides of the graphite mold, after the graphite mold is assembled, the graphite mold is put into a discharge plasma sintering furnace, pressure is applied under the nitrogen atmosphere, the temperature is raised for sintering, and after heat preservation, the graphite mold is cooled along with the furnace, so that the nano powder modified silicon carbide composite ceramic is obtained.
Further, in the S1, the mass ratio of the deionized water to the raw materials is (1.5-2): 1, the time of the magnetic stirring and the ultrasonic dispersion is 15 to 25 minutes.
Further, in the S2, the organic binder is a polyvinyl alcohol solution, and the addition amount is 10wt% -15 wt%; the dispersant is ammonium polyacrylate, and the addition amount is 1-2 wt%.
Further, in the step S2, the ball milling time is 20-24 h, and the mass ratio of the zirconia grinding balls to the raw material components is (3-4): 1, the rotation speed of the ball mill is 700-800 r/min.
Further, in the S5, the applied pressure is 25-30 MPa, the temperature rising rate is increased to 1500-1600 ℃ at a speed of 100 +/-10 ℃/min, and then the temperature rising rate is increased to 1700-1900 ℃ at a speed of 40 +/-10 ℃/min; the heat preservation time is 10-20 minutes.
The purpose of the invention and the technical problem to be solved are also realized by adopting the following technical scheme.
According to the nano powder modified silicon carbide complex phase ceramic prepared by the method, the nano powder modified silicon carbide complex phase ceramic is nano powder modified silicon carbide-boron carbide complex phase ceramic;
the nano powder modified silicon carbide-boron carbide complex phase ceramic comprises the following raw material components in percentage by mass: 78-93% of silicon carbide powder, 5-20% of nano boron carbide powder and 2% of carbon powder.
Furthermore, the average particle size of the silicon carbide powder is 0.5-1.0 μm, and the average particle size of the nano boron carbide powder is 50-100 nm.
Furthermore, the purity of the silicon carbide powder is more than or equal to 98 percent, and the purity of the nano boron carbide powder is more than or equal to 99.9 percent.
The purpose of the invention and the technical problem to be solved can also be realized by adopting the following technical scheme.
According to the nano powder modified silicon carbide complex phase ceramic prepared by the method, the nano powder modified silicon carbide complex phase ceramic is nano powder modified silicon carbide-graphene complex phase ceramic;
the nano powder modified silicon carbide-graphene complex phase ceramic comprises the following components in percentage by mass: 96-97.85% of silicon carbide powder, 0.15-2% of multilayer graphene and 2% of carbon powder.
Further, the purity of the silicon carbide powder is more than or equal to 98%, and the average thickness of the multilayer graphene is 30-50 nm.
The invention has the following advantages:
the method adopts the spark plasma sintering technology, compared with other sintering technologies of silicon carbide complex phase ceramics, the method has the advantages of fast preparation, simple process, capability of preparing the complex phase ceramics with excellent performance at lower temperature in shorter time, overcoming the difficulty of realizing high temperature and high pressure in the process, solving the problem of excessive growth of nano crystal grains caused by overhigh sintering temperature and overlong heat preservation time in other sintering technologies, and finally preparing the silicon carbide ceramics with fine, uniform and high toughness crystal grains.
Detailed Description
The principles and features of this invention are described below in conjunction with examples, which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
Example 1:
the method for preparing the nano powder modified silicon carbide composite ceramic by spark plasma sintering comprises the following raw material components in percentage by mass: 88 percent of silicon carbide powder, 10 percent of nano boron carbide powder and 2 percent of carbon powder, wherein the grain diameter of the silicon carbide is 0.8 mu m, and the grain diameter of the nano boron carbide is 50nm.
The method comprises the following specific steps:
s1, primary mixing of raw materials: weighing 88g of raw material silicon carbide powder, 10g of nano boron carbide powder and 2g of carbon powder according to the mass percentage, mixing the raw material powder with 150g of deionized water, and performing magnetic stirring and ultrasonic dispersion for 20 minutes at room temperature to obtain mixed slurry;
s2, ball milling and mixing: adding 15wt% of organic binder polyvinyl alcohol solution and 2wt% of dispersant ammonium polyacrylate into the mixed slurry, carrying out ball milling for 20h, and carrying out wet mixing on the mixed slurry in a ball milling tank by using zirconia grinding balls, wherein the mass of the zirconia grinding balls is 300g, and the ball milling rotating speed is 700r/min, so as to obtain wet mixed slurry;
s3, spray granulation: carrying out spray granulation on the wet mixed slurry, wherein the spray pressure is 0.2MPa, the air inlet temperature is 140 ℃, the air outlet temperature is 90 ℃, and granulating powder with the particle size of 90 mu m is prepared;
s4, pre-pressing and forming: prepressing the granulation powder by using a tablet press, wherein the selected forming pressure is 16MPa, and the pressure maintaining time is 20s, so as to obtain a pressed ceramic biscuit;
s5, assembling and sintering: and (2) putting the pressed biscuit into a graphite mold, spraying silicon nitride on the surface of the graphite mold, coating a layer of graphite paper in the graphite mold, wrapping a graphite felt outside the graphite mold, placing graphite pressure heads on two sides of the graphite mold, putting the graphite mold into a discharge plasma sintering furnace after the graphite mold is assembled, applying pressure of 30MPa in the nitrogen atmosphere, rapidly increasing the temperature to 1600 ℃ at the heating rate of 100 ℃/min, then increasing the temperature to 1850 ℃ at the heating rate of 45 ℃/min, preserving the temperature for 15 minutes, and cooling along with the furnace to obtain the nano-powder modified silicon carbide-boron carbide composite ceramic.
The properties of the silicon carbide-boron carbide complex phase ceramic prepared in the embodiment are as follows: the relative density is 3.25g/cm 3 Bending strength of 510MPa, vickers hardness of 29GPa, and fracture toughness of 6.7 MPa.m 1/2 。
Example 2:
the method for preparing the nano powder modified silicon carbide complex phase ceramic by spark plasma sintering comprises the following raw material components in percentage by mass: 97% of silicon carbide powder, 1% of multilayer graphene and 2% of carbon powder; wherein the grain diameter of the silicon carbide is 0.68 μm, and the thickness of the graphene is 40nm.
The method comprises the following specific steps:
s1, primary mixing of raw materials: weighing 97g of raw material silicon carbide powder, 1g of multilayer graphene and 2g of carbon powder according to the mass percentage, mixing the raw material powder with 200g of deionized water, and performing magnetic stirring and ultrasonic dispersion for 25 minutes at room temperature to obtain mixed slurry;
s2, ball milling and mixing: adding 10wt% of organic binder polyvinyl alcohol solution and 1wt% of dispersant ammonium polyacrylate into the mixed slurry, carrying out ball milling for 24 hours, and carrying out wet mixing on the mixed slurry in a ball milling tank by using zirconia grinding balls, wherein the mass of the zirconia grinding balls is 400g, and the ball milling speed is 780r/min, so as to obtain wet mixed slurry;
s3, spray granulation: carrying out spray granulation on the wet mixed slurry, wherein the spray pressure is 0.3MPa, the air inlet temperature is 160 ℃, the air outlet temperature is 100 ℃, and granulating powder with the particle size of 100 mu m is prepared;
s4, pre-pressing and forming: prepressing the granulation powder by using a tablet press, wherein the selected forming pressure is 20MPa, and the pressure maintaining time is 15s, so as to obtain a pressed ceramic biscuit;
s5, assembling and sintering: and (2) putting the pressed biscuit into a graphite mold, spraying silicon nitride on the surface of the graphite mold, coating a layer of graphite paper in the graphite mold, wrapping a graphite felt outside the graphite mold, placing graphite pressure heads on two sides of the graphite mold, putting the graphite mold into a discharge plasma sintering furnace after the graphite mold is assembled, rapidly increasing the applied pressure to 1500 ℃ at the heating rate of 110 ℃/min under the nitrogen atmosphere, then increasing the temperature to 1800 ℃ at the heating rate of 40 ℃/min, preserving the heat for 20 minutes, and cooling along with the furnace to obtain the nano powder modified silicon carbide-graphene composite ceramic.
The properties of the silicon carbide-graphene complex phase ceramic prepared in the embodiment are as follows: the relative density is 2.95g/cm 3 The bending strength is 490MPa, the Vickers hardness is 28.5GPa, and the fracture toughness is 5.9 MPa.m 1/2 。
Example 3:
the method for preparing the nano powder modified silicon carbide complex phase ceramic by spark plasma sintering comprises the following raw material components in percentage by mass: 83 percent of silicon carbide powder, 15 percent of nano boron carbide powder and 2 percent of carbon powder, wherein the grain diameter of the silicon carbide is 0.55 mu m, and the grain diameter of the nano boron carbide is 60nm.
The method comprises the following specific steps:
s1, primary mixing of raw materials: weighing 83g of raw material silicon carbide powder, 15g of nano boron carbide powder and 2g of carbon powder according to the mass percentage, mixing the raw material powder with 150g of deionized water, and performing magnetic stirring and ultrasonic dispersion for 20 minutes at room temperature to obtain mixed slurry;
s2, ball milling and mixing: adding 12wt% of organic binder polyvinyl alcohol solution and 1.5wt% of dispersant ammonium polyacrylate into the mixed slurry, carrying out ball milling for 22h, and carrying out wet mixing on the mixed slurry in a ball milling tank by using zirconia grinding balls, wherein the mass of the zirconia grinding balls is 300g, and the ball milling speed is 720r/min, so as to obtain wet mixed slurry;
s3, spray granulation: carrying out spray granulation on the wet mixed slurry, wherein the spray pressure is 0.3MPa, the air inlet temperature is 170 ℃, the air outlet temperature is 110 ℃, and granulating powder with the particle size of 160 mu m is prepared;
s4, pre-pressing and forming: prepressing the granulation powder by using a tablet press, wherein the selected forming pressure is 18MPa, and the pressure maintaining time is 25s, so as to obtain a pressed ceramic biscuit;
s5, assembling and sintering: and (2) putting the pressed biscuit into a graphite mold, spraying silicon nitride on the surface of the graphite mold, coating a layer of graphite paper in the graphite mold, wrapping a graphite felt outside the graphite mold, placing graphite pressure heads on two sides of the graphite mold, putting the graphite mold into a discharge plasma sintering furnace after the graphite mold is assembled, applying pressure of 28MPa in the nitrogen atmosphere, rapidly increasing the temperature to 1550 ℃ at a heating rate of 90 ℃/min, then increasing the temperature to 1750 ℃ at a rate of 35 ℃/min, preserving the temperature for 15 minutes, and cooling the product along with the furnace to obtain the nano powder modified silicon carbide-boron carbide composite ceramic.
The properties of the silicon carbide-boron carbide complex phase ceramic prepared in the embodiment are as follows: the relative density was 2.78g/cm 3 The bending strength is 435MPa, the Vickers hardness is 26.5GPa, and the fracture toughness is 5.6 MPa.m 1/2 。
In conclusion, the method adopts the spark plasma sintering technology, the preparation is rapid, the process is simple, the complex phase ceramic with excellent performance can be prepared at lower temperature in shorter time, the difficulty of realizing high temperature and high pressure in the process is overcome, the problem that nano crystal grains grow excessively due to overhigh sintering temperature and overlong heat preservation time in other sintering technologies is solved, and finally the high-toughness silicon carbide ceramic with small and uniform size of 100-500 nm is prepared.
It is to be understood that the present invention has been described with reference to certain embodiments and that various changes in form and details may be made therein by those skilled in the art without departing from the spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from the essential scope thereof. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.
Claims (10)
1. The method for preparing the nano powder modified silicon carbide complex phase ceramic by spark plasma sintering is characterized by comprising the following steps of:
s1, primary mixing of raw materials: mixing raw materials of silicon carbide powder, nano boron carbide powder and carbon powder or raw materials of silicon carbide powder, multi-layer graphene and carbon powder with deionized water, and performing magnetic stirring and ultrasonic dispersion at room temperature to obtain uniform mixed slurry;
s2, ball milling and mixing: adding an organic binder and a dispersing agent into the mixed slurry, and performing ball-milling wet mixing on the mixed slurry in a ball-milling tank by using zirconia grinding balls to obtain wet mixed slurry;
s3, spray granulation: carrying out spray granulation on the wet mixed slurry, controlling the spray pressure to be 0.2-0.4 MPa, the inlet temperature to be 140-170 ℃ and the outlet temperature to be 60-110 ℃, and preparing powder with the particle size of 90-240 mu m;
s4, pre-pressing and forming: prepressing the granulation powder by using a tablet press, keeping the pressure for 15-25 s to prepare a ceramic biscuit, wherein the loading pressure range is 15-20 MPa;
s5, assembling and sintering: and (2) putting the pressed ceramic biscuit into a graphite mold, wherein a layer of graphite paper is lined in the graphite mold, a graphite felt is wrapped outside the graphite mold, graphite pressure heads are placed on two sides of the graphite mold, after the graphite mold is assembled, the graphite mold is put into a discharge plasma sintering furnace, pressure is applied under the nitrogen atmosphere, the temperature is raised for sintering, and after heat preservation, the graphite mold is cooled along with the furnace, so that the nano powder modified silicon carbide composite ceramic is obtained.
2. The method for preparing the nano-powder modified silicon carbide complex phase ceramic by spark plasma sintering according to claim 1, wherein in S1, the mass ratio of the deionized water to the raw materials is (1.5-2): 1, the time of the magnetic stirring and the ultrasonic dispersion is 15 to 25 minutes.
3. The method for preparing nano powder modified silicon carbide composite ceramic by spark plasma sintering as claimed in claim 1, wherein in the step S2, the organic binder is polyvinyl alcohol solution, and the addition amount is 10wt% to 15wt%; the dispersant is ammonium polyacrylate, and the addition amount is 1-2 wt%.
4. The method for preparing the nano-powder modified silicon carbide complex phase ceramic by spark plasma sintering as claimed in claim 1, wherein in the step S2, the ball milling time is 20-24 hours, and the mass ratio of the zirconia grinding ball to the raw material components is (3-4): 1, the rotation speed of the ball mill is 700-800 r/min.
5. The method for preparing the nano-powder modified silicon carbide complex phase ceramic by spark plasma sintering as claimed in claim 1, wherein in S5, the applied pressure is 25-30 MPa, the temperature rise rate is increased to 1500-1600 ℃ at 100 ± 10 ℃/min, and then the temperature rise rate is increased to 1700-1900 ℃ at 40 ± 10 ℃/min; the heat preservation time is 10-20 minutes.
6. The nano powder modified silicon carbide composite ceramic prepared by the method according to any one of claims 1 to 5, wherein the nano powder modified silicon carbide composite ceramic is a nano powder modified silicon carbide-boron carbide composite ceramic;
the nano powder modified silicon carbide-boron carbide complex phase ceramic comprises the following raw material components in percentage by mass: 78-93% of silicon carbide powder, 5-20% of nano boron carbide powder and 2% of carbon powder.
7. The nano-powder modified silicon carbide composite ceramic of claim 6, wherein the average particle size of the silicon carbide powder is 0.5-1.0 μm, and the average particle size of the nano-boron carbide powder is 50-100 nm.
8. The nano-powder modified silicon carbide composite ceramic as claimed in claim 6, wherein the purity of the silicon carbide powder is not less than 98%, and the purity of the nano-boron carbide powder is not less than 99.9%.
9. The nano-powder modified silicon carbide composite ceramic prepared by the method of any one of claims 1 to 5, wherein the nano-powder modified silicon carbide composite ceramic is a nano-powder modified silicon carbide-graphene composite ceramic;
the nano powder modified silicon carbide-graphene complex phase ceramic comprises the following components in percentage by mass: 96-97.85% of silicon carbide powder, 0.15-2% of multilayer graphene and 2% of carbon powder.
10. The nano-powder modified silicon carbide composite ceramic of claim 9, wherein the purity of the silicon carbide powder is not less than 98%, and the average thickness of the multilayer graphene is 30-50 nm.
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Application publication date: 20221018 |