CN112321310B - Preparation method of nanoparticle toughened high-toughness SiC product - Google Patents
Preparation method of nanoparticle toughened high-toughness SiC product Download PDFInfo
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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
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Abstract
A preparation method of a nanoparticle toughened high-toughness SiC product relates to a preparation method of a high-toughness SiC product. The invention mainly solves the problems that in the existing process of toughening silicon carbide ceramics by silicon carbide nano-particles, the nano-particles are easy to agglomerate and combine and can not achieve uniform dispersion. The preparation method comprises the following steps: firstly, pretreating powder; dispersing the micro-rice flour; thirdly, primary granulation; fourthly, nano-wrapping; fifthly, secondary granulation; sixthly, pressing the biscuit; and seventhly, sintering the workpiece. The method is used for preparing the high-toughness SiC product toughened by the nano particles.
Description
Technical Field
The invention relates to a preparation method of a high-toughness SiC product.
Background
As a typical covalent bond compound, 78% of valence bond energy in silicon carbide belongs to a covalent state, 22% belongs to an ionic state, and the structural characteristics determine that the silicon carbide has the characteristics of high strength, high hardness, stable chemical properties and the like, but the silicon carbide also has the defects of lack of plastic deformation capability and high brittleness, and further application of the silicon carbide is limited to a certain extent. The silicon carbide ceramic is reinforced and toughened, so that the application potential of the silicon carbide ceramic can be further developed, and a new application scene of the silicon carbide ceramic is developed.
By introducing the silicon carbide nanoparticles in the preparation process of the silicon carbide ceramic, the nanoparticles are dispersed in the silicon carbide ceramic matrix, so that the strength and toughness of the silicon carbide ceramic can be effectively improved. The dispersion of the silicon carbide particles in the ceramic matrix will lead to two existing forms of nanoparticles: firstly, distributing the grain boundary in a matrix; secondly, the crystal particles are distributed in the crystal of the matrix. When the nano particles are distributed in the grain boundary of the matrix, a secondary interface and microcracks are generated in the matrix grains, so that the growth of the matrix grains is effectively inhibited, and the abnormal growth of the grains is reduced. In addition, the nano particles will make the cracks in the fracture process generate secondary deflection, and the fracture energy is consumed. Thereby achieving the purpose of enhancing the fracture toughness of the SiC ceramic.
Nano-toughening focuses on uniformly dispersing nanoparticles in a ceramic matrix. However, the nano powder has the characteristics of small particle size, large specific surface area, insufficient coordination of atoms on the surface of particles, high specific surface energy and the like, so that the nano powder has high surface activity. In order to reduce the total energy of the system, the nano particles are easy to combine with each other through agglomeration, when the material is dispersed, the agglomeration among the nano particles is broken through by adopting a proper dispersion method, and uniform and stable dispersion slurry is obtained, which is a difficulty in preparing the nano toughened ceramic.
Disclosure of Invention
The invention provides a preparation method of a high-toughness SiC product toughened by nano-particles, aiming at solving the problems that in the existing process of toughening silicon carbide ceramics by the silicon carbide nano-particles, the nano-particles are easy to agglomerate and combine and can not be uniformly dispersed.
A preparation method of a nanoparticle toughened high-toughness SiC product comprises the following steps:
firstly, pretreating powder:
respectively placing the silicon carbide micro-powder, the silicon carbide nano-powder and the sintering aid in an oven for constant-temperature drying to obtain pretreated silicon carbide micro-powder, pretreated silicon carbide nano-powder and pretreated sintering aid;
the grain diameter of the silicon carbide micro-powder is 0.3-10 mu m; the grain diameter of the silicon carbide nano powder is 1 nm-200 nm;
dispersing the micro-rice flour:
adding the pretreated silicon carbide micro-powder and the pretreated sintering aid into deionized water containing the aid, and uniformly dispersing to obtain micro-powder slurry;
the mass ratio of the pretreated silicon carbide micro-powder to the pretreated sintering aid is 1 (0.001-0.05); the mass ratio of the pretreated silicon carbide micro-powder to the auxiliary agent is 1 (0.05-0.25); the mass ratio of the pretreated silicon carbide micro-powder to the deionized water is 1 (0.8-1.3);
thirdly, primary granulation:
under the conditions that the stirring speed of the slurry is 10-50 rpm, the temperature of an air inlet of spray drying is 150-250 ℃, the air outlet temperature is 65-100 ℃ and the rotating speed of an atomizing disc is 3000-20000 rpm, the micro-rice flour slurry is subjected to spray drying to obtain primary granulated powder;
fourthly, nano-packaging:
adding the primary granulation powder into an organic solvent containing a silane coupling agent, uniformly dispersing, then adding the pretreated silicon carbide nano powder, and continuously dispersing to obtain nano-coated silicon carbide slurry;
the mass ratio of the primary granulation powder to the silane coupling agent is 1 (0.001-0.02); the mass ratio of the primary granulated powder to the organic solvent is 1 (0.8-1.2); the mass ratio of the primary granulated powder to the pretreated silicon carbide nano powder is 1 (0.01-0.25);
fifthly, secondary granulation:
spray-drying the nano-coated silicon carbide slurry under the conditions that the stirring speed of the slurry is 10-50 rpm, the temperature of an air inlet of spray-drying is 150-250 ℃, the air outlet temperature is 65-100 ℃ and the rotating speed of an atomizing disc is 3000-20000 rpm to obtain secondary granulation powder;
sixthly, biscuit pressing:
placing the secondary granulation powder in a hydraulic press mold, pressurizing to 50-200 MPa, and keeping constant pressure for 3-30 s to obtain a biscuit;
seventhly, sintering of the workpiece:
and (3) placing the biscuit in a high-temperature sintering furnace, and sintering for 1-2 h at the sintering temperature of 1900-2300 ℃ to obtain the nano-particle toughened high-toughness SiC product.
The invention has the beneficial effects that:
1. according to the invention, a secondary granulation process is adopted, silane coupling agent is used for carrying out surface modification on primary granulated powder, silicon carbide nano powder is adsorbed on the surface of the primary granulated powder, silicon carbide granulated powder with uniformly wrapped nano particles is obtained through secondary granulation, and a macroscopic uniform nano toughened SiC part is obtained in the subsequent biscuit pressing and part sintering processes, so that the problems that nano particles are easy to agglomerate and combine and cannot be uniformly dispersed in the existing silicon carbide nano particle toughened silicon carbide ceramic process are solved, the operation equipment is simple, and the process flow is not complex.
2. The silicon carbide nano powder is added, so that the surface energy is higher, the sintering driving force during biscuit sintering is improved, the densification of a sintered body can be promoted, and the density can reach more than 97%;
4. the invention generates a secondary interface and microcracks in matrix grains through the nano toughening effect, inhibits the grains from growing, reduces the grain size, and ensures that the average grain size of the silicon carbide is only 1-4 mu m;
5. the nano particles of the invention can lead the cracks which continue and develop forward in the fracture process to generate secondary deflection, consume fracture energy, play a role in toughening, and have the bending strength of more than 550MPa and the fracture toughness of 4.5 MPa.m1/2Above, the elastic modulus can reach above 420 GPa.
The invention relates to a preparation method of a nanoparticle toughened high-toughness SiC product.
Drawings
FIG. 1 is a scanning electron microscope image of a primary granulated powder prepared in the third step of the example, at a magnification of 100 times;
FIG. 2 is a SEM image of the secondary granulated powder prepared in step V of the example at 2500 times magnification;
FIG. 3 is a scanning electron microscope image of a cross-section of a green body prepared at step six of the example, at 200 times magnification;
fig. 4 is a scanning electron microscope picture of the nanoparticle toughened high toughness SiC article prepared in example one after grain boundary corrosion, with a magnification of 2850 times.
Detailed Description
The first embodiment is as follows: the embodiment of the invention relates to a preparation method of a nanoparticle toughened high-toughness SiC product, which comprises the following steps:
firstly, pretreating powder:
respectively placing the silicon carbide micro-powder, the silicon carbide nano-powder and the sintering aid in an oven for constant-temperature drying to obtain pretreated silicon carbide micro-powder, pretreated silicon carbide nano-powder and pretreated sintering aid;
the grain diameter of the silicon carbide micro-powder is 0.3-10 mu m; the grain diameter of the silicon carbide nano powder is 1 nm-200 nm;
dispersing the micro-rice flour:
adding the pretreated silicon carbide micro-powder and the pretreated sintering aid into deionized water containing the aid, and uniformly dispersing to obtain micro-powder slurry;
the mass ratio of the pretreated silicon carbide micro-powder to the pretreated sintering aid is 1 (0.001-0.05); the mass ratio of the pretreated silicon carbide micro-powder to the auxiliary agent is 1 (0.05-0.25); the mass ratio of the pretreated silicon carbide micro-powder to the deionized water is 1 (0.8-1.3);
thirdly, primary granulation:
under the conditions that the stirring speed of the slurry is 10-50 rpm, the temperature of an air inlet of spray drying is 150-250 ℃, the air outlet temperature is 65-100 ℃ and the rotating speed of an atomizing disc is 3000-20000 rpm, the micro-rice flour slurry is subjected to spray drying to obtain primary granulated powder;
fourthly, nano-packaging:
adding the primary granulation powder into an organic solvent containing a silane coupling agent, uniformly dispersing, then adding the pretreated silicon carbide nano powder, and continuously dispersing to obtain nano-coated silicon carbide slurry;
the mass ratio of the primary granulation powder to the silane coupling agent is 1 (0.001-0.02); the mass ratio of the primary granulated powder to the organic solvent is 1 (0.8-1.2); the mass ratio of the primary granulated powder to the pretreated silicon carbide nano powder is 1 (0.01-0.25);
fifthly, secondary granulation:
spray-drying the nano-coated silicon carbide slurry under the conditions that the stirring speed of the slurry is 10-50 rpm, the temperature of an air inlet of spray-drying is 150-250 ℃, the air outlet temperature is 65-100 ℃ and the rotating speed of an atomizing disc is 3000-20000 rpm to obtain secondary granulation powder;
sixthly, biscuit pressing:
placing the secondary granulation powder in a hydraulic press mold, pressurizing to 50-200 MPa, and keeping constant pressure for 3-30 s to obtain a biscuit;
seventhly, sintering of the workpiece:
and (3) placing the biscuit in a high-temperature sintering furnace, and sintering for 1-2 h at the sintering temperature of 1900-2300 ℃ to obtain the nano-particle toughened high-toughness SiC product.
And in the first step, constant-temperature drying is carried out to remove the water adsorbed on the surface of the powder.
The beneficial effects of the embodiment are as follows:
1. the embodiment adopts a secondary granulation process, uses a silane coupling agent to perform surface modification on primary granulated powder, adsorbs silicon carbide nano powder on the surface of the primary granulated powder, obtains the silicon carbide granulated powder uniformly wrapped by nano particles through secondary granulation, and obtains a macroscopic uniform nano toughened SiC part in the subsequent biscuit pressing and part sintering processes, thereby solving the problems that in the existing silicon carbide nano particle toughened silicon carbide ceramic process, the nano particles are easy to agglomerate and combine and can not be uniformly dispersed, the operation equipment is simple, and the process flow is not complex.
2. The silicon carbide nano powder is added in the embodiment, so that the surface energy is higher, the sintering driving force during biscuit sintering is improved, the densification of a sintered body can be promoted, and the density can reach more than 97%;
4. in the embodiment, a secondary interface and microcracks are generated in matrix grains through the nano toughening effect, the growth of the grains is inhibited, the grain size is reduced, and the average grain size of the silicon carbide is only 1-4 mu m;
5. the nano particles of the embodiment can lead the cracks which continue and develop forwards in the fracture process to generate secondary deflection, consume fracture energy, play a role in toughening, and have the bending strength of more than 550MPa and the fracture toughness of 4.5 MPa.m1/2Above, the elastic modulus can reach above 420 GPa.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the sintering aid in the step one is one or a mixture of more of carbon, boron and boron carbide; the constant-temperature drying temperature in the step one is 60-120 ℃, and the drying time is 2-24 h. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the auxiliary agent in the second step is one or a mixture of more of tetramethyl ammonium hydroxide, polyvinylpyrrolidone, sodium hydroxymethyl cellulose, polyethylene glycol, phenolic resin, polyvinyl butyral, n-octanol, polyvinyl alcohol and polyacrylamide. The other is the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: the mass ratio of the pretreated silicon carbide micro-powder to the pretreated sintering aid in the step two is 1 (0.005-0.05); the mass ratio of the pretreated silicon carbide micro-powder to the auxiliary agent in the step two is 1 (0.08-0.2); the mass ratio of the pretreated silicon carbide micro-powder to the deionized water in the step two is 1 (1-1.3). The others are the same as the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the silane coupling agent in the fourth step is one or a mixture of more of KH-550, KH-560, KH-570, KH-792, DL-602 and A-151; the organic solvent in the fourth step is one or a mixture of methanol, ethanol, acetone and toluene. The rest is the same as the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: the mass ratio of the primary granulated powder to the silane coupling agent in the fourth step is 1 (0.001-0.01); the mass ratio of the primary granulated powder to the organic solvent in the fourth step is 1 (0.9-1.2); the mass ratio of the primary granulated powder to the pretreated silicon carbide nano powder in the fourth step is 1 (0.05-0.25). The rest is the same as the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: the dispersion in the second step and the fourth step is ball milling dispersion, ultrasonic dispersion or stirring dispersion; the ball milling dispersion is to ball mill for 6 to 24 hours by using zirconia balls, alumina balls, silicon carbide balls or boron carbide balls as a ball milling medium under the conditions that the rotating speed of the ball mill is 10 to 100rpm and the ball-to-material ratio is (2 to 10):1, wherein the ball diameter of the ball milling medium is 1 to 20 mm; the ultrasonic dispersion is to use a rod type ultrasonic machine to carry out ultrasonic treatment for 10min to 120min under the condition that the frequency of the ultrasonic dispersion is between 28 and 40 kHz; the stirring dispersion is to stir for 8 to 24 hours by a blade type stirrer under the condition that the rotating speed of the stirrer is between 10 and 100 rpm. The others are the same as the first to sixth embodiments.
The specific implementation mode is eight: the present embodiment differs from one of the first to seventh embodiments in that: in the third step, the micro-rice flour slurry is spray-dried under the conditions that the slurry stirring speed is 15-40 rpm, the temperature of an air inlet of the spray-drying is 170-240 ℃, the air outlet temperature is 75-100 ℃ and the rotating speed of an atomizing disc is 8000-20000 rpm to obtain primary granulated powder; and step five, under the conditions that the stirring speed of the slurry is 15-30 rpm, the temperature of an air inlet of spray drying is 150-240 ℃, the air outlet temperature is 75-100 ℃ and the rotating speed of an atomizing disc is 3000-15000 rpm, the nano-coated silicon carbide slurry is subjected to spray drying to obtain secondary granulation powder. The rest is the same as the first to seventh embodiments.
The specific implementation method nine: the present embodiment differs from the first to eighth embodiments in that: and step six, placing the secondary granulated powder in a hydraulic press mold, pressurizing to 100-200 MPa, and keeping constant pressure for 10-20 s to obtain a biscuit. The other points are the same as those in the first to eighth embodiments.
The detailed implementation mode is ten: the present embodiment differs from one of the first to ninth embodiments in that: and step seven, sintering for 1-2 h at the sintering temperature of 2000-2200 ℃. The other points are the same as those in the first to ninth embodiments.
The following examples were used to demonstrate the beneficial effects of the present invention:
the first embodiment is as follows:
a preparation method of a nanoparticle toughened high-toughness SiC product comprises the following steps:
firstly, pretreating powder:
respectively placing the silicon carbide micro-powder, the silicon carbide nano-powder and the sintering aid in an oven for constant-temperature drying to obtain pretreated silicon carbide micro-powder, pretreated silicon carbide nano-powder and pretreated sintering aid;
dispersing the micro-rice flour:
adding the pretreated silicon carbide micro-powder and the pretreated sintering aid into deionized water containing the aid, and carrying out ball milling for 8 hours under the conditions that the rotating speed of a ball mill is 50rpm and the ball-to-material ratio is 5:1 to obtain micro-powder slurry;
thirdly, primary granulation:
spray drying the micron powder slurry under the conditions that the slurry stirring speed is 15rpm, the temperature of an air inlet of spray drying is 240 ℃, the temperature of air outlet is 75 ℃ and the rotating speed of an atomizing disc is 15000rpm to obtain primary granulated powder;
fourthly, nano-packaging:
adding the primary granulation powder into an organic solvent containing a silane coupling agent, carrying out ball milling for 8 hours under the conditions that the rotating speed of a ball mill is 50rpm and the ball-to-material ratio is 5:1, then adding the pretreated silicon carbide nano powder, and carrying out ball milling for 6 hours under the conditions that the rotating speed of the ball mill is 50rpm and the ball-to-material ratio is 5:1 to obtain nano-coated silicon carbide slurry;
fifthly, secondary granulation:
spray drying the nano-coated silicon carbide slurry under the conditions that the stirring speed of the slurry is 20rpm, the temperature of an air inlet of spray drying is 240 ℃, the temperature of air outlet is 75 ℃ and the rotating speed of an atomizing disc is 15000rpm to obtain secondary granulation powder;
sixthly, biscuit pressing:
placing the secondary granulation powder in a four-column hydraulic press mold, pressurizing to 200MPa, and keeping constant pressure for 15s to obtain a biscuit;
seventhly, sintering of the workpiece:
and (3) placing the biscuit in a high-temperature sintering furnace, and sintering for 1h at the sintering temperature of 2100 ℃ to obtain the nano-particle toughened high-toughness SiC product.
The sintering aid in the step one is boron carbide powder; d of the silicon carbide micro-rice flour in the step one501 μm; d of the silicon carbide nanopowder described in step one50130 nm; the constant-temperature drying temperature in the step one is 80 ℃, and the drying time is 16 h.
The auxiliary agent in the second step is a mixture of tetramethylammonium hydroxide and phenolic resin mixed according to the mass ratio of 2: 5.
The mass ratio of the pretreated silicon carbide micro-powder to the pretreated sintering aid in the step two is 1: 0.005; the mass ratio of the pretreated silicon carbide micro-powder to the auxiliary agent in the step two is 1: 0.14; the mass ratio of the pretreated silicon carbide micro-powder to the deionized water in the step two is 1: 1.
The silane coupling agent in the fourth step is KH-550; the organic solvent in the fourth step is ethanol.
The mass ratio of the primary granulated powder to the silane coupling agent in the fourth step is 1: 0.003; the mass ratio of the primary granulated powder to the organic solvent in the fourth step is 1: 0.9; the mass ratio of the primary granulated powder to the pretreated silicon carbide nano powder in the fourth step is 1: 0.05.
And in the ball milling in the second step and the fourth step, silicon carbide balls are used as ball milling media, and the ball diameter of the ball milling media is about 5 mm.
Fig. 1 is a scanning electron microscope image of the primary granulated powder prepared in the third step of the example, at a magnification of 100 times. As can be seen from the figure, the prepared primary granulated powder has regular shape, is a regular sphere, has a certain particle size ratio with the particle size distributed between 10 and 100 mu m, is beneficial to the subsequent biscuit pressing, and can fill gaps between large particles due to the existence of small particles.
Fig. 2 is a scanning electron microscope image of the secondary granulated powder prepared in one fifth step of the example, at a magnification of 2500 times. As can be seen from the figure, the prepared secondary granulated powder has regular, uniform and smooth appearance, and a layer of silicon carbide nano powder is coated outside the granulated powder micron particles, which shows that the secondary granulation process successfully introduces the silicon carbide nano powder on the surface of the granulated powder. And the silicon carbide nano powder is uniformly coated on the outer surface of the granulation powder micron particles, and agglomeration and combination do not occur, so that the technical effect of uniform dispersion of the nano powder can be achieved in the subsequent preparation process.
FIG. 3 is a scanning electron microscope image of a cross-section of a green body prepared in step six of the example, at 200 times magnification. It can be seen from the figure that after the granulated powder prepared by the secondary granulation process is pressed by using a hydraulic press, the granules of the granulated powder are completely crushed, the nano powder coated outside the granulated powder is successfully filled into the gaps among the granules of the granulated powder, and the obtained biscuit is compact and has few pores.
Fig. 4 is a scanning electron microscope picture of the nanoparticle toughened high toughness SiC article prepared in example one after grain boundary corrosion, with a magnification of 2850 times. The grain size of the silicon carbide was measured by the scribing method, and the average grain size of the silicon carbide after sintering was 2.7 μm.
The density of the nanoparticle toughened, high toughness SiC articles prepared in example one was calculated by archimedes drainage and the results showed that the density of the resulting sintered bodies was 3.17g/cm3The density reaches 98.5 percent.
Therefore, the silicon carbide nano powder is introduced in the secondary granulation, the density of the sintered body is successfully improved, and the grain size of the sintered body is refined.
The bending strength of the sample of the nanoparticle toughened high-toughness SiC product prepared in the first embodiment is detected by a three-point bending method, the size of the sample is 3mm multiplied by 4mm multiplied by 30mm, the span is 20mm, the loading rate is 0.5mm/min, and the fracture toughness is detected by an indentation method. The results show that the sample prepared in example one has a flexural strength of 573MPa and a fracture toughness of 4.7MPa · m1/2The elastic modulus was 440 GPa.
Claims (1)
1. A preparation method of a nanoparticle toughened high-toughness SiC product is characterized by comprising the following steps:
firstly, pretreating powder:
respectively placing the silicon carbide micro-powder, the silicon carbide nano-powder and the sintering aid in an oven for constant-temperature drying to obtain pretreated silicon carbide micro-powder, pretreated silicon carbide nano-powder and pretreated sintering aid;
dispersing the micro-rice flour:
adding the pretreated silicon carbide micro-powder and the pretreated sintering aid into deionized water containing the aid, and carrying out ball milling for 8 hours under the conditions that the rotating speed of a ball mill is 50rpm and the ball-to-material ratio is 5:1 to obtain micro-powder slurry;
thirdly, primary granulation:
spray drying the micron powder slurry under the conditions that the slurry stirring speed is 15rpm, the temperature of an air inlet of spray drying is 240 ℃, the temperature of air outlet is 75 ℃ and the rotating speed of an atomizing disc is 15000rpm to obtain primary granulated powder;
fourthly, nano-packaging:
adding the primary granulation powder into an organic solvent containing a silane coupling agent, carrying out ball milling for 8 hours under the conditions that the rotating speed of a ball mill is 50rpm and the ball-to-material ratio is 5:1, then adding the pretreated silicon carbide nano powder, and carrying out ball milling for 6 hours under the conditions that the rotating speed of the ball mill is 50rpm and the ball-to-material ratio is 5:1 to obtain nano-coated silicon carbide slurry;
fifthly, secondary granulation:
spray drying the nano-coated silicon carbide slurry under the conditions that the stirring speed of the slurry is 20rpm, the temperature of an air inlet of spray drying is 240 ℃, the temperature of air outlet is 75 ℃ and the rotating speed of an atomizing disc is 15000rpm to obtain secondary granulation powder;
sixthly, biscuit pressing:
placing the secondary granulation powder in a four-column hydraulic press mold, pressurizing to 200MPa, and keeping constant pressure for 15s to obtain a biscuit;
seventhly, sintering of the workpiece:
placing the biscuit in a high-temperature sintering furnace, and sintering for 1h at the sintering temperature of 2100 ℃ to obtain a nano-particle toughened high-toughness SiC product;
the sintering aid in the step one is boron carbide powder; d of the silicon carbide micro-rice flour in the step one501 μm; d of the silicon carbide nanopowder described in step one50130 nm; the constant-temperature drying temperature in the step one is 80 ℃, and the drying time is 16 h;
the auxiliary agent in the second step is a mixture of tetramethylammonium hydroxide and phenolic resin mixed according to the mass ratio of 2: 5;
the mass ratio of the pretreated silicon carbide micro-powder to the pretreated sintering aid in the step two is 1: 0.005; the mass ratio of the pretreated silicon carbide micro-powder to the auxiliary agent in the step two is 1: 0.14; the mass ratio of the pretreated silicon carbide micro-powder to the deionized water in the step two is 1: 1;
the silane coupling agent in the fourth step is KH-550; the organic solvent in the step four is ethanol;
the mass ratio of the primary granulated powder to the silane coupling agent in the fourth step is 1: 0.003; the mass ratio of the primary granulated powder to the organic solvent in the fourth step is 1: 0.9; the mass ratio of the primary granulated powder to the pretreated silicon carbide nano powder in the fourth step is 1 (0.01-0.25);
and in the ball milling in the second step and the fourth step, silicon carbide balls are used as ball milling media, and the ball diameter of the ball milling media is about 5 mm.
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| CN107459357A (en) * | 2017-09-06 | 2017-12-12 | 西安博尔新材料有限责任公司 | Silicon carbide composite powder body and its preparation method and application |
| CN110054497A (en) * | 2019-05-24 | 2019-07-26 | 哈尔滨工业大学 | A kind of preparation method of the nanometer toughening silicon carbide complex phase ceramic of densification |
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