CN117964365A - Composite-configuration high-heat-conductivity diamond SiC composite material and preparation method thereof - Google Patents
Composite-configuration high-heat-conductivity diamond SiC composite material and preparation method thereof Download PDFInfo
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- CN117964365A CN117964365A CN202410194218.9A CN202410194218A CN117964365A CN 117964365 A CN117964365 A CN 117964365A CN 202410194218 A CN202410194218 A CN 202410194218A CN 117964365 A CN117964365 A CN 117964365A
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- 239000002131 composite material Substances 0.000 title claims abstract description 68
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 57
- 239000010432 diamond Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000843 powder Substances 0.000 claims description 74
- 238000010438 heat treatment Methods 0.000 claims description 33
- 239000002243 precursor Substances 0.000 claims description 25
- 239000002113 nanodiamond Substances 0.000 claims description 20
- 238000000498 ball milling Methods 0.000 claims description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 15
- 230000004913 activation Effects 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 14
- 239000006229 carbon black Substances 0.000 claims description 12
- 229910021389 graphene Inorganic materials 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- 229910052582 BN Inorganic materials 0.000 claims description 7
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 7
- VVTSZOCINPYFDP-UHFFFAOYSA-N [O].[Ar] Chemical compound [O].[Ar] VVTSZOCINPYFDP-UHFFFAOYSA-N 0.000 claims description 7
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- 238000000465 moulding Methods 0.000 claims description 7
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 7
- 229910052903 pyrophyllite Inorganic materials 0.000 claims description 7
- 230000000630 rising effect Effects 0.000 claims description 7
- 239000011780 sodium chloride Substances 0.000 claims description 7
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 5
- 238000011068 loading method Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 2
- 238000004100 electronic packaging Methods 0.000 description 4
- 239000005022 packaging material Substances 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000001808 coupling effect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention discloses a composite-configuration high-heat-conductivity diamond SiC composite material and a preparation method thereof.
Description
Technical Field
The invention relates to the technical field of electronic packaging material preparation, in particular to a composite-configuration high-heat-conductivity diamond SiC composite material and a preparation method thereof.
Background
The electronic packaging material is an important component of the integrated circuit and is used for protecting important electronic components from external damage. With the continuous improvement of electronic computing capability, the unit heat of an integrated circuit is obviously increased, and if the electronic packaging material cannot timely discharge the heat, the service efficiency and the service life of electronic components are seriously affected. Diamond has excellent heat conductivity and chemical corrosion resistance, is a common electronic packaging material, but is difficult to manufacture into a compact block due to the strong covalent bond composition. The addition of a binder phase can solve the above problems, however, the difference in thermal expansion coefficient and the difference in physicochemical properties between diamond and binder phase makes the diamond composite material lower in strength and shorter in lifetime.
The crystal structure of SiC is similar to that of diamond, and the thermal conductivity of SiC is also good, so that the SiC is an important diamond composite material binder, but different components make the SiC and the diamond composite material difficult to form a good interface structure, and the thermal conductivity and the service life of the diamond/SiC composite material are affected.
Disclosure of Invention
The invention discloses a composite-configuration high-heat-conductivity diamond SiC composite material and a preparation method thereof, and aims to solve the technical problem that the same components in the background technology make the two difficult to form a good interface structure, and influence the heat conductivity and the service life of the diamond/SiC composite material.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the preparation method of the composite configuration high heat conduction diamond SiC composite material comprises the following steps:
Step one: firstly, carrying out activation heat treatment on nano diamond powder and nano SiC powder, and then mixing and ball milling with graphene and carbon black powder to obtain a diamond/SiC composite material precursor;
step two: and loading the precursor into a high-pressure assembly, forming at high temperature and high pressure in a hexahedral press, and finally performing discharge plasma rapid heat treatment to finally obtain the composite-configuration high-heat-conductivity diamond/SiC composite material.
In a preferred scheme, in the first step, the activation heat treatment atmosphere of the nano diamond powder and the nano SiC powder is 96-98: 2-4 volume ratio argon-oxygen mixture gas, the temperature is 620-670 ℃, the time is 65-82 seconds, and the temperature rising/reducing rate is 18-26 ℃/min; weighing powder and nano diamond powder according to mass percent: nano SiC powder: graphene powder: carbon black powder=73 to 79.1:20.5 to 26:0.2 to 0.5:0.2 to 0.5, a roller ball mill is adopted for mixing ball milling, the ball-material ratio is 14 to 18:1, the rotating speed of the ball mill is 82 to 89 r/min, and the ball milling time is 1.5 to 2.5 hours.
In a preferred scheme, in the second step, the high-voltage component consists of zirconium dioxide, a sodium chloride heat-insulating layer and a hexagonal boron nitride and pyrophyllite pressure transmission layer, and the height-diameter ratio of the cavity of the component is 1.15-1.2: 1, cold press molding is carried out under 48-56 MPa before the precursor powder is filled into a high-voltage component, so that the density of a green body is 45-50%, and then the green body is wrapped with hafnium foil or tantalum foil; the high-temperature high-pressure process temperature is 1450-1550 ℃ and the pressure is 6-8 GPa; the rapid heat treatment temperature of the discharge plasma is 980-1040 ℃, the pressure is 12-15 MPa, the time is 40-65 seconds, and the temperature rising rate is 340-420 ℃/min.
In a preferred scheme, the prepared diamond/SiC composite material has a composite structure and excellent heat conduction performance, the relative density is more than or equal to 96.3%, the hardness is more than or equal to 18GPa, and the heat conductivity is more than or equal to 540W/mK.
From the above, the preparation method of the composite configuration high heat conduction diamond SiC composite material comprises the following steps: step one: firstly, carrying out activation heat treatment on nano diamond powder and nano SiC powder, and then mixing and ball milling with graphene and carbon black powder to obtain a diamond/SiC composite material precursor; step two: and loading the precursor into a high-pressure assembly, forming at high temperature and high pressure in a hexahedral press, and finally performing discharge plasma rapid heat treatment to finally obtain the composite-configuration high-heat-conductivity diamond/SiC composite material. The composite configuration high heat conduction diamond SiC composite material and the preparation method thereof provided by the invention have the following technical effects:
1: the preparation method comprises the steps of carrying out activation heat treatment on nano diamond powder and nano SiC powder, mixing and ball milling with graphene and carbon black powder to obtain a powder precursor, loading the precursor into a high-pressure assembly, forming at high temperature and high pressure in a hexahedral top press, and finally carrying out rapid heat treatment on discharge plasma; the activation heat treatment of the nano powder etches the surface of the nano powder through a micro-oxygen atmosphere, damages a surface regular tetrahedral structural layer, increases powder surface dangling bonds, improves surface activity, and provides necessary conditions for stabilizing an interface structure and promoting sintering densification; the main purpose of adding a small amount of graphene and carbon black powder is to facilitate the formation of various carbon structures such as cubes, hexagons and twin crystals in the subsequent high-temperature and high-pressure process by introducing high-energy structural carbon components, so that the diamond/SiC composite material forms a multi-structure composite structure, coordinate the interface structure of diamond and SiC, improve the blocking capability of the interface to microcrack expansion under the action of external force, and promote the composite material to have high thermal conductivity and excellent mechanical properties; the rapid heat treatment of the discharge plasma eliminates the residual stress of the high-pressure sample tissue by utilizing the coupling effect of the magnetic field, the electric field and the force field of the discharge plasma sintering, and further improves the performance of the diamond/SiC composite material.
2: The diamond/SiC composite material prepared by the invention has a composite structure and excellent heat conduction performance, the relative density is more than or equal to 96.3%, the hardness is more than or equal to 18GPa, and the heat conductivity is more than or equal to 540W/mK.
3: In the preparation process of the composite-configuration high-heat-conductivity diamond/SiC composite material, the invention adopts powder surface covalent bond activation, multi-structure carbon doping, high-temperature high-pressure configuration design and rapid heat treatment series means to form the multi-phase diamond/SiC composite material, regulates and controls interface tissues of the multi-phase diamond/SiC composite material, and researches the relationship between an activation heat treatment process, component proportion, ball milling process parameters, high-temperature high-pressure process parameters, discharge plasma rapid heat treatment process and performance of the diamond/SiC composite material. In order to obtain the diamond/SiC composite material with high heat conductivity and long service life, the optimal activation heat treatment process, component proportion, ball milling process parameters, high-temperature high-pressure process parameters and discharge plasma rapid heat treatment process are selected. The preparation method has the advantages of high control precision of microstructure structure, high process stability, high repeatability and the like, and can realize the efficient preparation of the diamond/SiC composite material.
Drawings
Fig. 1 is a comparative example of an embodiment of a composite-structured high-thermal-conductivity diamond SiC composite material and a method for preparing the same according to the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments.
Referring to fig. 1, a preparation method of a composite-configuration high-heat-conductivity diamond SiC composite material specifically includes the following steps:
step one: 96-98: 2-4 volume ratio argon-oxygen mixed atmosphere, the temperature is 620-670 ℃, the time is 65-82 seconds, the nano diamond powder and the nano SiC powder are subjected to activation heat treatment under the condition of 18-26 ℃/min of temperature rise/fall rate, and the powder is weighed according to the mass percentage, the nano diamond powder: nano SiC powder: graphene powder: carbon black powder=73 to 79.1:20.5 to 26:0.2 to 0.5: mixing and ball milling with a roller ball mill at a ball-material ratio of 14-18:1 and a ball mill rotation speed of 82-89 r/min for 1.5-2.5 hours to obtain a diamond/SiC composite material precursor;
Step two: the precursor is filled into a high-voltage component, the high-voltage component consists of a zirconium dioxide and sodium chloride heat-insulating layer and a hexagonal boron nitride and pyrophyllite pressure-transmitting layer, and the height-diameter ratio of a component cavity is 1.15-1.2: 1, cold press molding precursor powder under 48-56 MPa to obtain a green compact with density of 45-50%, wrapping a blank body with hafnium foil or tantalum foil, forming at 1450-1550 ℃ in a hexahedral press under high temperature and high pressure of 6-8 GPa, and performing discharge plasma rapid heat treatment at 980-1040 ℃ under 12-15 MPa for 40-65 seconds and at a heating rate of 340-420 ℃/min to obtain the composite high-heat-conductivity diamond/SiC composite material.
Example 1
The preparation method of the composite configuration high heat conduction diamond SiC composite material specifically comprises the following steps:
Step one: at 96:4, carrying out activation heat treatment on nano diamond powder and nano SiC powder under the condition of argon-oxygen mixed atmosphere with the volume ratio, the temperature of 620 ℃ and the time of 65 seconds and the heating/cooling rate of 18 ℃/min, and weighing the powder according to the mass percentage, wherein the temperature of the nano diamond powder is equal to the temperature of the nano diamond powder: nano SiC powder: graphene powder: carbon black powder = 73:26:0.5:0.5, mixing and ball milling by adopting a roller ball mill, wherein the ball-material ratio is 18:1, the rotating speed of the ball mill is 82 r/min, and the ball milling time is 1.5 hours, so that the precursor of the diamond/SiC composite material is obtained;
Step two: the precursor is filled into a high-voltage component, the high-voltage component is composed of a zirconium dioxide and sodium chloride heat-insulating layer and a hexagonal boron nitride and pyrophyllite pressure-transmitting layer, and the height-diameter ratio of a component cavity is 1.15:1, cold press molding precursor powder under 48MPa to obtain a green compact with the density of 45%, wrapping a hafnium foil or a tantalum foil on the green compact, forming at 1450 ℃ and 6GPa in a hexahedral press at high temperature and high pressure, and performing discharge plasma rapid heat treatment at 980 ℃ and 12MPa for 40 seconds at the temperature and the pressure and at the heating and cooling rate of 340 ℃/min to obtain the composite-configuration high-heat-conductivity diamond/SiC composite material.
Example 2
The preparation method of the composite configuration high heat conduction diamond SiC composite material specifically comprises the following steps:
Step one: at 98:2, carrying out activation heat treatment on nano diamond powder and nano SiC powder under the condition of an argon-oxygen mixed atmosphere with the volume ratio, the temperature of 670 ℃ and the time of 82 seconds and the heating/cooling rate of 18 ℃ per minute, and weighing the powder according to the mass percentage, wherein the nano diamond powder is as follows: nano SiC powder: graphene powder: carbon black powder = 75:24:0.5:0.5, mixing and ball milling by adopting a roller ball mill, wherein the ball-material ratio is 15:1, the rotating speed of the ball mill is 84 r/min, and the ball milling time is 2 hours, so that the diamond/SiC composite material precursor is obtained;
Step two: the precursor is filled into a high-voltage component, the high-voltage component is composed of a zirconium dioxide and sodium chloride heat-insulating layer and a hexagonal boron nitride and pyrophyllite pressure-transmitting layer, and the height-diameter ratio of a component cavity is 1.2:1, cold press molding precursor powder under 56MPa to obtain a green compact with the density of 50%, wrapping a hafnium foil or a tantalum foil on the green compact, forming at 1460 ℃ in a hexahedral press at 7GPa under high temperature and high pressure, and performing discharge plasma rapid heat treatment at 1040 ℃ and 13MPa for 45 seconds at a temperature rising rate of 360 ℃/min to obtain the composite-configuration high-heat-conductivity diamond/SiC composite material.
Example 3
The preparation method of the composite configuration high heat conduction diamond SiC composite material specifically comprises the following steps:
Step one: at 97:3, carrying out activation heat treatment on nano diamond powder and nano SiC powder under the condition of an argon-oxygen mixed atmosphere with the volume ratio, the temperature of 650 ℃ and the time of 69 seconds, and the temperature rise/fall rate of 23 ℃ per minute, wherein the powder is weighed according to the mass percentage, and the nano diamond powder is prepared by the following steps: nano SiC powder: graphene powder: carbon black powder=79.1: 20.5:0.2:0.2, mixing and ball milling by adopting a roller ball mill, wherein the ball-material ratio is 16:1, the rotating speed of the ball mill is 88 r/min, and the ball milling time is 2.5 hours, so that the precursor of the diamond/SiC composite material is obtained;
Step two: the precursor is filled into a high-voltage component, the high-voltage component is composed of a zirconium dioxide and sodium chloride heat-insulating layer and a hexagonal boron nitride and pyrophyllite pressure-transmitting layer, and the height-diameter ratio of a component cavity is 1.2:1, cold press molding the precursor powder under 55MPa to obtain a green compact with the density of 47%, wrapping a hafnium foil or a tantalum foil on the green compact, forming the green compact in a hexahedral press at 1520 ℃ and under 7GPa pressure at high temperature and high pressure, and performing discharge plasma rapid heat treatment at 1040 ℃ and under 15MPa for 55 seconds at a temperature and pressure of 15MPa at a temperature rising rate of 420 ℃/min to obtain the composite-configuration high-heat-conductivity diamond/SiC composite material.
Example 4
The preparation method of the composite configuration high heat conduction diamond SiC composite material specifically comprises the following steps:
step one: at 98:2, carrying out activation heat treatment on nano diamond powder and nano SiC powder under the conditions of an argon-oxygen mixed atmosphere with the volume ratio, the temperature of 660 ℃ and the time of 68 seconds and the rising/falling speed of 22 ℃/min, and weighing the powder according to the mass percentage, wherein the temperature of the nano diamond powder is equal to the temperature of the nano diamond powder: nano SiC powder: graphene powder: carbon black powder=76: 23.4:0.3:0.3, mixing and ball milling by adopting a roller ball mill, wherein the ball-material ratio is 15:1, the rotating speed of the ball mill is 85 r/min, and the ball milling time is 2 hours, so that the diamond/SiC composite material precursor is obtained;
Step two: the precursor is filled into a high-voltage component, the high-voltage component is composed of a zirconium dioxide and sodium chloride heat-insulating layer and a hexagonal boron nitride and pyrophyllite pressure-transmitting layer, and the height-diameter ratio of a component cavity is 1.2:1, cold press molding precursor powder under 52MPa to obtain a green compact with a density of 47%, wrapping a hafnium foil or a tantalum foil on the green compact, forming at 1480 ℃ and 8GPa in a hexahedral press at high temperature and high pressure, and performing discharge plasma rapid heat treatment at 980 ℃ and 15MPa for 40 seconds at a temperature of up-down temperature rate of 420 ℃/min to obtain the composite-configuration high-heat-conductivity diamond/SiC composite material.
Examples 1-4 the performance parameters of the composite configuration high thermal conductivity diamond/SiC composite materials are shown in figure 1.
As can be seen from the drawing, the diamond/SiC composite material prepared by the invention has a composite structure and excellent heat conduction performance, the relative density is more than or equal to 96.3%, the hardness is more than or equal to 18GPa, and the heat conductivity is more than or equal to 540W/mK.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (4)
1. The preparation method of the composite-configuration high-heat-conductivity diamond SiC composite material is characterized by comprising the following steps of:
Step one: firstly, carrying out activation heat treatment on nano diamond powder and nano SiC powder, and then mixing and ball milling with graphene and carbon black powder to obtain a diamond/SiC composite material precursor;
step two: and loading the precursor into a high-pressure assembly, forming at high temperature and high pressure in a hexahedral press, and finally performing discharge plasma rapid heat treatment to finally obtain the composite-configuration high-heat-conductivity diamond/SiC composite material.
2. The method for preparing the composite-structured high-heat-conductivity diamond SiC composite material according to claim 1, wherein in the first step, the activation heat treatment atmosphere of the nano diamond powder and the nano SiC powder is 96-98: 2-4 volume ratio argon-oxygen mixture gas, the temperature is 620-670 ℃, the time is 65-82 seconds, and the temperature rising/reducing rate is 18-26 ℃/min; weighing powder and nano diamond powder according to mass percent: nano SiC powder: graphene powder: carbon black powder=73 to 79.1:20.5 to 26:0.2 to 0.5:0.2 to 0.5, a roller ball mill is adopted for mixing ball milling, the ball-material ratio is 14 to 18:1, the rotating speed of the ball mill is 82 to 89 r/min, and the ball milling time is 1.5 to 2.5 hours.
3. The method for preparing the composite-configuration high-heat-conductivity diamond SiC composite material according to claim 1, wherein in the second step, the high-voltage component consists of zirconium dioxide, a sodium chloride heat-insulating layer, a hexagonal boron nitride and pyrophyllite pressure-transmitting layer, and the height-diameter ratio of the component cavity is 1.15-1.2: 1, cold press molding is carried out under 48-56 MPa before the precursor powder is put into a high-pressure component, so that the density of a green body is 45-50%, then the green body is wrapped with hafnium foil or tantalum foil, the high-temperature high-pressure process temperature is 1450-1550 ℃, and the pressure is 6-8 GPa; the rapid heat treatment temperature of the discharge plasma is 980-1040 ℃, the pressure is 12-15 MPa, the time is 40-65 seconds, and the temperature rising rate is 340-420 ℃/min.
4. The composite-structured high-heat-conductivity diamond SiC composite material is used for the preparation method of the composite-structured high-heat-conductivity diamond SiC composite material according to any one of claims 1-3, and is characterized in that the prepared diamond/SiC composite material has a composite structure and excellent heat conductivity, the relative density is more than or equal to 96.3%, the hardness is more than or equal to 18GPa, and the heat conductivity is more than or equal to 540W/mK.
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