CN113735583A - Novel diamond/silicon carbide composite ceramic and preparation method thereof - Google Patents
Novel diamond/silicon carbide composite ceramic and preparation method thereof Download PDFInfo
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- CN113735583A CN113735583A CN202111252935.5A CN202111252935A CN113735583A CN 113735583 A CN113735583 A CN 113735583A CN 202111252935 A CN202111252935 A CN 202111252935A CN 113735583 A CN113735583 A CN 113735583A
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- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 96
- 239000010432 diamond Substances 0.000 title claims abstract description 96
- 239000002131 composite material Substances 0.000 title claims abstract description 77
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 64
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 239000000919 ceramic Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title abstract description 16
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000000843 powder Substances 0.000 claims abstract description 42
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 42
- 238000005475 siliconizing Methods 0.000 claims abstract description 29
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000005011 phenolic resin Substances 0.000 claims abstract description 17
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 17
- 238000005238 degreasing Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000000465 moulding Methods 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000007710 freezing Methods 0.000 claims abstract description 5
- 230000008014 freezing Effects 0.000 claims abstract description 5
- 230000008569 process Effects 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims description 12
- 238000005245 sintering Methods 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000007791 liquid phase Substances 0.000 claims description 6
- 239000012071 phase Substances 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 19
- 230000000694 effects Effects 0.000 abstract description 5
- 238000005469 granulation Methods 0.000 abstract description 4
- 230000003179 granulation Effects 0.000 abstract description 4
- 239000007921 spray Substances 0.000 abstract description 3
- 239000002002 slurry Substances 0.000 abstract 1
- 229910052799 carbon Inorganic materials 0.000 description 8
- 229910002804 graphite Inorganic materials 0.000 description 7
- 239000010439 graphite Substances 0.000 description 7
- 238000011065 in-situ storage Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000010304 firing Methods 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 238000011161 development Methods 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000004913 activation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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Abstract
The invention discloses a novel diamond/silicon carbide composite ceramic and a preparation method thereof, and relates to the technical field of composite ceramics. The novel diamond/silicon carbide composite ceramic comprises the following raw materials in percentage by volume: 30-55% of diamond powder, 20-35% of silicon powder and 15-25% of phenolic resin, wherein the novel diamond/silicon carbide composite ceramic is prepared by preparing slurry without adding graphite powder, and performing freezing spray granulation, hot press molding, degreasing and siliconizing reaction. The composite ceramic prepared by the raw material formula and the preparation method disclosed by the invention has good compactness and excellent performances in the aspects of hardness, elastic modulus and thermal conductivity, and the preparation method saves the siliconizing time in the siliconizing process, thereby saving energy and achieving the effect of saving cost.
Description
Technical Field
The invention belongs to the technical field of composite ceramics, and particularly relates to novel diamond/silicon carbide composite ceramics and a preparation method thereof.
Background
The diamond-silicon carbide composite material not only has higher thermal conductivity and adjustable thermal expansion coefficient, but also has the characteristics of lower density, high hardness, good physical and chemical stability and the like, so the diamond/silicon carbide composite material is used in many aspects at present. In particular, the diamond/silicon carbide composite material has wide application in high heat conduction, and due to the continuous development of electronic technology, the integration degree of electronic components and semiconductors is higher and higher, the heat generation amount of the components is also higher and higher, and the components cannot work in an environment with overhigh temperature, so that the heat dissipation problem becomes a great importance in the development of the electronic information industry, and the diamond/silicon carbide composite material has good heat conduction performance, so the diamond/silicon carbide composite material becomes a leading material for solving the heat dissipation problem of the components.
At present, the diamond/silicon carbide composite ceramic is mainly prepared by using diamond, graphite, phenolic resin and silicon powder as main raw materials, but the requirement on the particle size of the graphite is harsh, if the particle size of the graphite particles is large, the siliconizing time can be greatly prolonged during siliconizing so as to achieve the effect of complete reaction of the graphite and silicon, otherwise, the graphite particles only can generate silicon carbide on the surface layer, and are still graphite in the interior, so that the ultrahigh heat conductivity coefficient of the composite ceramic is seriously influenced.
Disclosure of Invention
Based on the above, the invention provides a novel diamond/silicon carbide composite ceramic and a preparation method thereof, and graphite powder is not added in the preparation method, so that the siliconizing time is saved in the siliconizing process, the energy is further saved, and the effect of saving the cost is achieved.
In order to achieve the above purpose, the invention provides the following technical scheme:
the novel diamond/silicon carbide composite ceramic comprises the following raw materials in percentage by volume:
30-55% of diamond powder;
20-35% of silicon powder;
15-25% of phenolic resin.
Preferably, the diamond powder comprises monocrystalline diamond powder and polycrystalline diamond powder, and the granularity of the diamond powder is 80-120 mu m.
Preferably, the purity of the silicon powder is more than or equal to 95 percent, and the particle size of the silicon powder is 30-50 mu m.
Preferably, the purity of the silicon powder is most preferably equal to or more than 99.99%.
The invention provides a preparation method of novel diamond/silicon carbide composite ceramic, which comprises the following steps:
uniformly mixing diamond powder, silicon powder and phenolic resin with absolute ethyl alcohol to prepare liquid with viscosity of 2000-;
secondly, placing the composite powder prepared in the first step into a mould, and carrying out hot press molding at the temperature of 130 ℃ and 150 ℃ to prepare a blank;
carrying out degreasing treatment on the green body prepared in the step II at the temperature of 1000-1100 ℃ to prepare a porous prefabricated body;
fourthly, siliconizing and sintering the porous prefabricated body prepared in the third step in a vacuum high-temperature furnace at 1450-1600 ℃ to prepare the novel diamond/silicon carbide composite ceramic.
Preferably, in the step (I), the pressure during the freezing, spraying and granulating is 15-45 MPa; the particle size of the composite powder is 130-150 mu m.
Preferably, in the step two, the hot-press forming pressure is 30-70MPa, and the pressure maintaining time is 10-20 min.
Preferably, in the third step, the heating rate of degreasing is 1-3 ℃/min; the degreasing time is 90-120 min.
Preferably, in the step (iv), during the siliconizing sintering, the heat preservation time is 30min at the temperature of 1450 ℃, the heating rate is 3 ℃/min to 5 ℃/min at the temperature of 1450-; the vacuum degree in the siliconizing process is 0.1-320 pa.
Preferably, in the step (iv), the siliconizing means includes liquid phase siliconizing and gas phase siliconizing; the dosage of the added silicon powder in the liquid-phase siliconizing is 2.0-2.5 times of the weight of the porous preform; the dosage of the added silicon powder in the gas-phase siliconizing is 2.8-3.2 times of the weight of the porous preform.
The invention has the following beneficial effects:
(1) the novel diamond/silicon carbide composite material prepared by the invention adopts graphite powder without addition, so that the silicon powder and the diamond powder are more effectively wrapped by the phenolic resin in the granulation process, the contact area of the silicon powder and the diamond powder is further increased, the carbon source directly generated on the surfaces of the degreased residual carbon and the diamond has higher reaction activation energy, the silicon powder in contact with the carbon powder is more easily reacted in situ to generate silicon carbide, the possibility of greatly reducing the related physical properties of the material due to incomplete reaction of carbon particles is avoided, the siliconizing time is saved on the other hand, the energy is saved, and the effect of saving the cost is achieved.
(2) The novel diamond-silicon carbide composite material prepared by the invention adopts the diamond powder with larger grain diameter, micro-graphitization can be generated on the surface of the diamond powder at high temperature, and the generated graphite layer provides a new carbon source to react with silicon to generate silicon carbide, so that the density of the material is increased.
(3) The invention adopts the freezing spray granulation method to prepare uniform and single powder particle size, and can also recover the solvent absolute ethyl alcohol to achieve the effect of recycling, thereby saving the cost.
Drawings
In order to illustrate the embodiments of the invention more clearly, the drawings that are needed in the description of the embodiments will be briefly described below, it being apparent that the drawings in the following description are only some embodiments of the invention, and that other drawings may be derived from those drawings by a person skilled in the art without inventive effort.
FIG. 1 is an SEM photograph of a porous preform in example 3 of the present invention (FIG. a is a photograph of a porous preform, and FIG. b is a photograph of a diamond/silicon carbide composite ceramic);
FIG. 2 is an SEM photograph of a porous preform in example 4 of the present invention (FIG. c is a photograph of the porous preform, and FIG. d is a photograph of a diamond/silicon carbide composite ceramic);
FIG. 3 is an SEM photograph of a porous preform in example 5 of the present invention (FIG. (e) is a photograph of the porous preform, and FIG. (f) is a photograph of a diamond/silicon carbide composite ceramic);
FIG. 4 is an SEM photograph of a porous preform in example 6 of the present invention (FIG. (g) is a photograph of the porous preform, and FIG. (h) is a photograph of a diamond/silicon carbide composite ceramic).
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention in conjunction with the examples, but it will be understood that the description is intended to illustrate the features and advantages of the invention further and is not intended to limit the invention to the claims.
All of the starting materials of the present invention, without particular limitation as to their source, may be purchased commercially or prepared according to conventional methods well known to those skilled in the art.
The test methods described in the following examples of the present invention are all carried out in a conventional manner unless otherwise specified.
The following detailed description will be made with reference to specific embodiments and accompanying drawings to provide a novel diamond/silicon carbide composite ceramic and a method for preparing the same, and the scope of the invention is not limited by the following embodiments.
Example 1
The novel diamond/silicon carbide composite ceramic comprises the following raw materials in percentage by volume:
30-55% of diamond powder;
20-35% of silicon powder;
15-25% of phenolic resin.
Wherein the diamond powder comprises monocrystalline diamond powder and polycrystalline diamond powder, and the granularity of the diamond powder is 80-120 μm; the purity of the silicon powder is more than or equal to 95 percent, the granularity of the silicon powder is 30-50 mu m, and the most preferable purity of the silicon powder is more than or equal to 99.99 percent.
Example 2
A preparation method of novel diamond/silicon carbide composite ceramic comprises the following steps:
firstly, 30-55% of diamond powder, 20-35% of silicon powder and 15-25% of phenolic resin are uniformly mixed by absolute ethyl alcohol according to volume percentage to prepare liquid with viscosity of 2000-5000mPa.s and good dispersibility, and the liquid is subjected to pressure type freezing spray granulation to prepare the composite powder.
Secondly, placing the composite powder prepared in the step one in a mould, and carrying out hot press molding at the temperature of 130-150 ℃ to prepare a blank.
And thirdly, carrying out degreasing treatment on the blank prepared in the second step at the temperature of 1000-1100 ℃ to prepare the porous prefabricated body.
Fourthly, siliconizing and sintering the porous prefabricated body prepared in the third step in a vacuum high-temperature furnace at 1450-1600 ℃ to prepare the novel diamond/silicon carbide composite ceramic.
Example 3
A preparation method of novel diamond/silicon carbide composite ceramic comprises the following steps:
50 percent of diamond powder, 25 percent of silicon powder and 25 percent of phenolic resin are uniformly mixed by absolute ethyl alcohol according to volume percentage to prepare liquid with the viscosity of 2000-5000mPa.s and good dispersibility, and the liquid is frozen, sprayed and granulated when the pressure is 15MPa to prepare the composite powder.
Secondly, placing the composite powder prepared in the first step into a mould, and performing hot press molding at the temperature of 150 ℃, the pressure of 30MP and the pressure maintaining time of 10min to prepare a blank.
And thirdly, degreasing the blank prepared in the second step, wherein the heating rate is 1 ℃/min, and when the maximum temperature reaches 1000 ℃, the temperature is kept for 120min, so that the porous preform is prepared.
Fourthly, placing a small amount of silicon powder at the bottom of a firing tool, placing the porous preform prepared in the third step, paving silicon powder on the porous preform, covering the added silicon powder by using a cover made of the same material as the firing tool, and performing liquid-phase siliconizing sintering in a vacuum high-temperature furnace, wherein the using amount of the added silicon powder is 2 times of the weight of the porous preform, and the vacuum degree of the cover is controlled to be 0.1-320pa, so that the diamond/silicon carbide composite ceramic is prepared; wherein the temperature rise rate is 10 ℃/min from room temperature to 1450 ℃, the temperature is kept for 30min at 1450 ℃, the temperature rise rate is 3 ℃/min at 1450-1600 ℃ and the temperature is kept for 45min at 1600 ℃.
SEM photographs of the porous preform and the diamond/silicon carbide composite ceramic prepared in example 3 are shown in FIG. 1. FIG. (a) is a photograph of a porous preform from which it can be seen that residual carbon after phenolic resin degreasing is relatively uniformly dispersed in the mass and encapsulates the diamond; and (b) is an SEM picture of a fracture surface of the diamond/silicon carbide composite ceramic, wherein the fracture mode of the diamond is shown as transgranular fracture, and the matrix silicon carbide is proved to be in-situ growth of the diamond. The composite material finally obtained is the diamond/silicon carbide composite ceramic meeting the performance requirements.
Example 4
A preparation method of novel diamond/silicon carbide composite ceramic comprises the following steps:
55 percent of diamond powder, 20 percent of silicon powder and 25 percent of phenolic resin are uniformly mixed by absolute ethyl alcohol according to volume percentage to prepare liquid with the viscosity of 2000-5000mPa.s and good dispersibility, and the liquid is frozen, sprayed and granulated when the pressure is 25MPa to prepare the composite powder.
Secondly, placing the composite powder prepared in the first step into a mould, and performing hot press molding at the temperature of 130 ℃, the pressure of 45MP and the pressure maintaining time of 20min to prepare a blank.
And thirdly, degreasing the blank prepared in the second step, wherein the heating rate is 2 ℃/min, and the temperature is kept for 110min when the highest temperature reaches 1050 ℃, so that the porous preform is prepared.
Placing a small amount of silicon powder at the bottom of a firing tool, placing the porous preform prepared in the step (c), paving silicon powder on the porous preform, covering the added silicon powder by using a cover made of the same material as the firing tool, and performing gas-phase siliconizing sintering in a vacuum high-temperature furnace, wherein the using amount of the added silicon powder is 2.5 times of the weight of the porous preform, and the vacuum degree of the furnace is controlled to be 0.1-320pa, so that the diamond/silicon carbide composite ceramic is prepared; wherein, the temperature rise rate is 10 ℃/min from room temperature to 1450 ℃, the temperature is kept for 30min at 1450 ℃, the temperature rise rate is 4 ℃/min at 1450-1600 ℃ and the temperature is kept for 50min at 1600 ℃.
Among them, SEM photographs of the porous preform and the diamond/silicon carbide composite ceramic prepared in example 4 are shown in fig. 2. FIG. (c) is a photograph of a porous preform from which it can be seen that residual carbon after phenolic resin degreasing is relatively uniformly dispersed in the mass and encapsulates the diamond; and (d) is an SEM photograph of a fracture surface of the diamond/silicon carbide composite ceramic, wherein the fracture mode of the diamond can be seen as transgranular fracture, and the matrix silicon carbide is proved to be in-situ growth of the diamond.
Example 5
A preparation method of novel diamond/silicon carbide composite ceramic comprises the following steps:
55 percent of diamond powder, 25 percent of silicon powder and 20 percent of phenolic resin are uniformly mixed by absolute ethyl alcohol according to volume percentage to prepare liquid with the viscosity of 2000-5000mPa.s and good dispersibility, and the liquid is frozen, sprayed and granulated when the pressure is 35MPa to prepare the composite powder.
Secondly, placing the composite powder prepared in the first step into a mould, and performing hot press molding at the temperature of 130 ℃, the pressure of 60MP and the pressure maintaining time of 20min to prepare a blank.
And thirdly, degreasing the blank prepared in the second step, wherein the heating rate is 3 ℃/min, and when the highest temperature reaches 1100 ℃, the temperature is kept for 90min to prepare the porous preform.
Putting a small amount of silicon powder into a sintering tool, putting the porous prefabricated body prepared in the step (III) above the silicon powder within the height range of 0-3mm, wherein the amount of the added silicon powder is 2.8 times of the weight of the porous prefabricated body, performing liquid phase siliconizing sintering in a vacuum high-temperature furnace, and controlling the vacuum degree to be 0.1-320pa to prepare the diamond/silicon carbide composite ceramic; wherein, the temperature rise rate is 10 ℃/min from room temperature to 1450 ℃, the temperature is kept for 30min at 1450 ℃, the temperature rise rate is 5 ℃/min at 1450-1600 ℃ and the temperature is kept for 60min at 1600 ℃.
Among them, SEM photographs of the porous preform and the diamond/silicon carbide composite ceramic prepared in example 5 are shown in fig. 3. FIG. (e) is a photograph of a porous preform from which it can be seen that the residual carbon after the phenolic resin has been degreased is relatively uniformly dispersed in the mass and encapsulates the diamond; and (f) is an SEM picture of a fracture surface of the diamond/silicon carbide composite ceramic, wherein the fracture mode of the diamond can be seen as transgranular fracture, and the matrix silicon carbide is proved to be in-situ growth of the diamond.
Example 6
A preparation method of novel diamond/silicon carbide composite ceramic comprises the following steps:
50 percent of diamond powder, 30 percent of silicon powder and 20 percent of phenolic resin are uniformly mixed by absolute ethyl alcohol according to volume percentage to prepare liquid with the viscosity of 2000-5000mPa.s and good dispersibility, and the liquid is frozen, sprayed and granulated when the pressure is 45MPa to prepare the composite powder.
Secondly, placing the composite powder prepared in the first step into a mould, and performing hot press molding at the temperature of 130 ℃, the pressure of 70MP and the pressure maintaining time of 20min to prepare a blank.
And thirdly, degreasing the blank prepared in the second step, wherein the heating rate is 2 ℃/min, and when the highest temperature reaches 1100 ℃, the temperature is kept for 100min to prepare the porous preform.
Putting a small amount of silicon powder into a sintering tool, putting the porous prefabricated body prepared in the step (III) above the silicon powder within the height range of 0-3mm, wherein the amount of the added silicon powder is 3.2 times of the weight of the porous prefabricated body, and carrying out gas-phase siliconizing sintering in a vacuum high-temperature furnace, wherein the vacuum degree is controlled to be 0.1-320pa, so as to prepare the diamond/silicon carbide composite ceramic; wherein, the temperature rise rate is 10 ℃/min from room temperature to 1450 ℃, the temperature is kept for 30min at 1450 ℃, the temperature rise rate is 3 ℃/min at 1450-1600 ℃ and the temperature is kept for 50min at 1600 ℃.
Among them, SEM photographs of the porous preform and the diamond/silicon carbide composite ceramic prepared in example 6 are shown in fig. 4. FIG. g is a photograph of a porous preform from which it can be seen that residual carbon after phenolic resin degreasing is relatively uniformly dispersed in the mass and encapsulates the diamond; the graph (h) is an SEM photograph of a fracture surface of the diamond/silicon carbide composite ceramic, wherein the fracture mode of the diamond can be seen as transgranular fracture, and the matrix silicon carbide is proved to be in-situ growth of the diamond.
The novel diamond/silicon carbide composite ceramics obtained in examples 3, 4, 5 and 6 were subjected to the relevant performance tests, and the test results are shown in the following table.
Tests show that the diamond/silicon carbide composite ceramic material prepared by the raw material formula and the preparation method disclosed by the invention has good compactness and excellent performances in the aspects of hardness, elastic modulus and thermal conductivity.
The preparation method of the novel diamond/silicon carbide composite ceramic provided by the invention is described in detail above. The principles and embodiments of the present invention are explained herein using specific examples, which are presented only to assist in understanding the method and its core concepts. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
Claims (10)
1. A novel diamond/silicon carbide composite ceramic is characterized in that: the composite material consists of the following raw materials in percentage by volume:
30-55% of diamond powder;
20-35% of silicon powder;
15-25% of phenolic resin.
2. The novel diamond/silicon carbide composite ceramic according to claim 1, wherein: the diamond powder comprises monocrystalline diamond powder and polycrystalline diamond powder; the granularity of the diamond powder is 80-120 mu m.
3. The novel diamond/silicon carbide composite ceramic according to claim 1, wherein: the purity of the silicon powder is more than or equal to 95 percent; the granularity of the silicon powder is 10-50 μm.
4. A novel diamond/silicon carbide composite ceramic according to claim 3, wherein: the purity of the silicon powder is most preferably more than or equal to 99.99%.
5. The novel diamond/silicon carbide composite ceramic according to claim 1, characterized in that it is prepared by the following method:
uniformly mixing diamond powder, silicon powder and phenolic resin with absolute ethyl alcohol to prepare liquid with viscosity of 2000-;
secondly, placing the composite powder prepared in the first step into a mould, and carrying out hot press molding at the temperature of 130 ℃ and 150 ℃ to prepare a blank;
carrying out degreasing treatment on the green body prepared in the step II at the temperature of 1000-1100 ℃ to prepare a porous prefabricated body;
fourthly, siliconizing and sintering the porous prefabricated body prepared in the third step in a vacuum high-temperature furnace at 1450-1600 ℃ to prepare the novel diamond/silicon carbide composite ceramic.
6. The novel diamond/silicon carbide composite ceramic according to claim 5, wherein: in the step I, the pressure during freezing, spraying and granulating is 15-45 MPa; the particle size of the composite powder is 130-150 mu m.
7. The novel diamond/silicon carbide composite ceramic according to claim 5, wherein: in the second step, the hot-press molding pressure is 30-70MPa, and the pressure maintaining time is 10-20 min.
8. The novel diamond/silicon carbide composite ceramic according to claim 5, wherein: in the third step, the heating rate of degreasing is 1-3 ℃/min; the degreasing time is 90-120 min.
9. The novel diamond/silicon carbide composite ceramic according to claim 5, wherein: in the fourth step, during the siliconizing sintering, the heat preservation time is 30min at the temperature of 1450 ℃, the heating rate is 3 ℃/min-5 ℃/min at the temperature of 1450-1600 ℃, and the heat preservation time is 45-60min at the temperature of 1600 ℃; the vacuum degree in the siliconizing sintering process is 0.1-320 pa.
10. The novel diamond/silicon carbide composite ceramic according to claim 5, wherein: in the fourth step, the siliconizing mode comprises liquid phase siliconizing and gas phase siliconizing; the dosage of the added silicon powder in the liquid-phase siliconizing is 2.0-2.5 times of the weight of the porous preform; the dosage of the added silicon powder in the gas-phase siliconizing is 2.8-3.2 times of the weight of the porous preform.
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