CN117923950A - Ceramic matrix composite heat dissipation substrate and preparation method and application thereof - Google Patents
Ceramic matrix composite heat dissipation substrate and preparation method and application thereof Download PDFInfo
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- 239000000758 substrate Substances 0.000 title claims abstract description 72
- 239000011153 ceramic matrix composite Substances 0.000 title claims abstract description 58
- 230000017525 heat dissipation Effects 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title abstract description 21
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 122
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 72
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 72
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 58
- 239000010703 silicon Substances 0.000 claims abstract description 58
- JUZTWRXHHZRLED-UHFFFAOYSA-N [Si].[Cu].[Cu].[Cu].[Cu].[Cu] Chemical compound [Si].[Cu].[Cu].[Cu].[Cu].[Cu] JUZTWRXHHZRLED-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000002052 molecular layer Substances 0.000 claims abstract description 53
- 239000000919 ceramic Substances 0.000 claims abstract description 50
- 229910021360 copper silicide Inorganic materials 0.000 claims abstract description 31
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 30
- 239000004917 carbon fiber Substances 0.000 claims abstract description 30
- 239000004744 fabric Substances 0.000 claims abstract description 30
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000463 material Substances 0.000 claims abstract description 17
- 239000010410 layer Substances 0.000 claims description 149
- 238000000034 method Methods 0.000 claims description 35
- 238000000151 deposition Methods 0.000 claims description 25
- 239000000126 substance Substances 0.000 claims description 21
- 229910052751 metal Inorganic materials 0.000 claims description 20
- 239000002184 metal Substances 0.000 claims description 20
- 239000005543 nano-size silicon particle Substances 0.000 claims description 20
- 239000002356 single layer Substances 0.000 claims description 20
- 239000011159 matrix material Substances 0.000 claims description 16
- 238000002844 melting Methods 0.000 claims description 15
- 230000008018 melting Effects 0.000 claims description 15
- 239000002994 raw material Substances 0.000 claims description 14
- 238000001704 evaporation Methods 0.000 claims description 11
- 238000005229 chemical vapour deposition Methods 0.000 claims description 9
- 230000008595 infiltration Effects 0.000 claims description 9
- 238000001764 infiltration Methods 0.000 claims description 9
- 238000001771 vacuum deposition Methods 0.000 claims description 9
- 238000000576 coating method Methods 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 6
- 239000004065 semiconductor Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 4
- 239000002245 particle Substances 0.000 claims 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 28
- 239000001257 hydrogen Substances 0.000 description 28
- 229910052739 hydrogen Inorganic materials 0.000 description 28
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 23
- 229910052786 argon Inorganic materials 0.000 description 14
- 230000005587 bubbling Effects 0.000 description 14
- 230000008021 deposition Effects 0.000 description 14
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 11
- 229910052802 copper Inorganic materials 0.000 description 11
- 239000010949 copper Substances 0.000 description 11
- 238000010790 dilution Methods 0.000 description 9
- 239000012895 dilution Substances 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 229910002804 graphite Inorganic materials 0.000 description 7
- 239000010439 graphite Substances 0.000 description 7
- 230000009286 beneficial effect Effects 0.000 description 5
- 230000008020 evaporation Effects 0.000 description 5
- 150000002431 hydrogen Chemical class 0.000 description 5
- 238000007738 vacuum evaporation Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 238000005452 bending Methods 0.000 description 3
- 238000005219 brazing Methods 0.000 description 3
- 239000011229 interlayer Substances 0.000 description 3
- 238000007655 standard test method Methods 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- LTPBRCUWZOMYOC-UHFFFAOYSA-N Beryllium oxide Chemical compound O=[Be] LTPBRCUWZOMYOC-UHFFFAOYSA-N 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- FRWYFWZENXDZMU-UHFFFAOYSA-N 2-iodoquinoline Chemical compound C1=CC=CC2=NC(I)=CC=C21 FRWYFWZENXDZMU-UHFFFAOYSA-N 0.000 description 1
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
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Abstract
The invention discloses a ceramic matrix composite heat dissipation substrate, a preparation method and application thereof, and relates to the technical field of preparation of ceramic heat dissipation substrates. The heat dissipation substrate includes: a C f/SiC layer, a CVD-SiC layer, a silicon nano layer and a copper silicide layer; the CVD-SiC layer is coated on the outer surface of the C f/SiC layer, the silicon nano layer is coated on the upper surface of the CVD-SiC layer, and the copper silicide layer is coated on the upper surface of the silicon nano layer; the C f/SiC layer is a silicon carbide ceramic matrix composite material reinforced by carbon fiber cloth. The heat dissipation substrate of the ceramic matrix composite material prepared by the invention has the heat conductivity of more than 296W/(m.K), high fracture toughness and high flexural strength, and is suitable for being used on high-power modules. The invention solves the problem of low heat conductivity of the ceramic heat dissipation substrate in the prior art.
Description
Technical Field
The invention relates to the technical field of preparation of ceramic heat dissipation substrates, in particular to a ceramic matrix composite heat dissipation substrate, a preparation method and application thereof.
Background
Along with the rising industries of rail transit, electric vehicles, hybrid vehicles, high-voltage inverters, direct current power transmission, high-power LEDs, 5G communication and the like, the high-voltage and high-current power semiconductor devices are widely applied, and at the moment, the ceramic heat dissipation substrate with high heat conductivity, high insulativity and high heat conductivity plays an increasing role in the field of electronic technology.
The most basic structure of the ceramic heat dissipation substrate is composed of a ceramic layer and a copper layer, wherein the ceramic layer mainly comprises beryllium oxide (BeO), aluminum oxide (Al 2O3), aluminum nitride (AlN) and silicon nitride (Si 3N4) according to the material classification, and the BeO ceramic has higher heat conductivity but toxicity; the Al 2O3 ceramic substrate has low price and good thermal shock resistance, but has the problems of low heat conductivity and unmatched thermal expansion rate with silicon phase; the AlN and Si 3N4 ceramic heat dissipation substrate has good thermal expansion rate matching with silicon and high thermal conductivity. However, in order to adapt to higher power and withstand higher breakdown voltage, higher thermal conductivity, insulativity and thermal conductivity of the ceramic heat dissipation substrate are required, and the thermal expansion coefficient is matched with that of silicon, so that the above ceramic heat dissipation substrate material cannot completely meet the trend of the power device towards high power and high breakdown voltage. The ceramic heat dissipation substrate is generally prepared by forming and sintering ceramic powder to prepare a ceramic layer, and then coating the ceramic layer with a copper layer on one or both sides by a direct copper coating method (DBC) or an active metal brazing method (AMB). The purity, granularity, phase, oxygen content and forming process of the powder adopted by the ceramic layer forming are key factors influencing the physical and mechanical properties of the ceramic substrate, and have higher requirements on the material control and process technology integration capability. The direct copper coating method has low cost, but the wettability of the ceramic layer and the copper layer is poor, micro-pores are easy to generate between the ceramic layer and the copper layer, and the thermal conductivity is influenced; the active metal brazing method developed on the basis is to wet and react AgCu solder with active elements Ti and Zr at the interface of a ceramic layer and a copper layer to realize heterogeneous bonding of ceramic and metal, but the thermal conductivity of the active metal brazing method is still not ideal. Therefore, a new ceramic matrix composite heat dissipating substrate is urgently needed.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a ceramic matrix composite heat dissipation substrate, a preparation method and application thereof, so as to solve the problem of low heat conductivity of the ceramic heat dissipation substrate in the prior art.
The technical scheme for solving the technical problems is as follows: provided is a ceramic matrix composite heat dissipating substrate comprising: a C f/SiC layer, a CVD-SiC layer, a silicon nano layer and a copper silicide layer; the CVD-SiC layer is coated on the outer surface of the C f/SiC layer, the silicon nano layer is coated on the upper surface of the CVD-SiC layer, and the copper silicide layer is coated on the upper surface of the silicon nano layer; the C f/SiC layer is a silicon carbide ceramic matrix composite reinforced by carbon fiber cloth.
Based on the technical scheme, the invention can also be improved as follows:
further, the number of the carbon fiber cloth layers is a single layer.
The beneficial effects of adopting the further technical scheme are as follows: in order to improve the toughness of the heat dissipation substrate and the heat dissipation uniformity on the whole base surface, the carbon fiber cloth is selected to be a single layer, so that the influence on the heat conductivity caused by the fact that multiple layers of carbon fiber cloth are introduced into more air holes which cannot be compact in later stages is avoided.
Further, the thickness of the C f/SiC layer is 0.1-0.2mm.
Further, the thickness of the CVD-SiC layer on one side of the C f/SiC layer is 0.2 to 1mm.
The beneficial effects of adopting the further technical scheme are as follows: to further improve the high power resistance and bending strength of a heat dissipating substrate.
Further, the thickness of the silicon nano layer is 15-100nm.
The beneficial effects of adopting the further technical scheme are as follows: in order to enhance the bonding strength of the CVD-SiC layer and the copper silicide, the heat dissipation effect is better, a silicon nano transition layer is designed between the CVD-SiC layer and the copper silicide, and the thickness of the silicon nano transition layer is controlled to be 15-100nm.
Further, the thickness of the copper silicide layer is 0.2-0.4mm.
The invention also provides a preparation method of the ceramic matrix composite heat dissipation substrate, which sequentially comprises the following steps:
S1: depositing a silicon carbide ceramic matrix on the surface of the single-layer carbon fiber cloth by adopting a chemical vapor infiltration method to prepare a C f/SiC layer;
S2: coating and depositing a silicon carbide ceramic matrix on the outer surface of the C f/SiC layer prepared in the step S1 by adopting a chemical vapor deposition method to prepare a CVD-SiC layer;
s3: evaporating nano silicon on the upper surface of the CVD-SiC layer prepared in the step S2 by using nano silicon powder as a raw material by adopting a vacuum evaporation method to prepare a silicon nano layer;
S4: and (3) preparing a copper silicide layer on the upper surface of the silicon nano layer prepared in the step (S3) by using copper silicide powder as a raw material and adopting a vacuum metal melting method to prepare the ceramic matrix composite heat dissipation substrate.
Further, in steps S1 and S2, a C f/SiC layer and a CVD-SiC layer are sequentially formed in the same chemical vapor vacuum equipment by changing reaction parameters.
Further, in step S1, the gas flow parameter of the chemical vapor infiltration method is bubbling hydrogen: dilution of hydrogen: diluted argon= (0.2-0.4) L/min: (0.1-0.3) L/min: (0.2-0.4) L/min, furnace pressure of 100-200Pa and deposition temperature of 900-1000 ℃.
Further, in step S1, the gas flow parameter of the chemical vapor infiltration method is bubbling hydrogen: dilution of hydrogen: diluted argon = 0.3L/min:0.2L/min:0.3L/min, furnace pressure 150Pa, deposition temperature 950 ℃.
Further, in step S2, the gas flow parameters of the chemical vapor deposition method are bubbling hydrogen: dilution of hydrogen: diluted argon= (1-2) L/min: (1-1.5) L/min: (1-2) L/min, the furnace pressure is 450-550Pa, and the deposition temperature is 1350-1450 ℃.
Further, in step S2, the gas flow parameters of the chemical vapor deposition method are bubbling hydrogen: dilution of hydrogen: diluted argon = 1.5L/min:1.2L/min:1.5L/min, furnace pressure 500Pa, deposition temperature 1400 ℃.
In the step S3, the grain diameter of the nanometer silicon powder is 5-25nm.
In step S3, the vacuum evaporation method is carried out at a temperature of 1500-2000 ℃ and a furnace pressure of 100-150Pa.
Further, in step S3, the vacuum deposition method was carried out at a temperature of 1700℃and a furnace pressure of 120Pa.
Further, in step S4, the mesh number of the copper silicide powder is 750-850 mesh.
Further, in step S4, vacuum metal melting is performed at 830-850 ℃.
Further, in step S4, copper silicide powder with a thickness of 1-2mm is buried on the silicon nanolayer, and then placed in a graphite box with a cover, and vacuum metal melting is performed.
The beneficial effects of adopting the further technical scheme are as follows: in order to reduce the surface roughness of the heat dissipation substrate and accurately control the thickness of the copper silicide layer, the mesh number of the copper silicide powder is 750-850 meshes, the thickness of the embedded copper silicide powder is 1-2mm, and vacuum metal melting is carried out at 830-850 ℃.
The invention also provides application of the ceramic matrix composite heat dissipation substrate in the aspect of semiconductor device preparation.
The invention has the following beneficial effects:
1. The ceramic layer of the ceramic matrix composite heat dissipation substrate consists of a C f/SiC layer and a CVD-SiC layer, wherein a SiC matrix and a CVD-SiC material in the C f/SiC layer are beta-SiC, and the heat conductivity of the ceramic matrix and the CVD-SiC material is higher than that of ceramics such as silicon nitride, aluminum oxide and the like; in addition, the C f/SiC layer contains single-layer continuous carbon fiber cloth, so that the heat conduction is uniform, the heat dissipation efficiency can be further improved, the thermal stress caused by heat accumulation of the substrate can be absorbed, and the fracture toughness of the material is higher.
2. The copper layer of the ceramic matrix composite heat dissipation substrate is a copper silicide (Cu 5 Si) layer, the heat conductivity of the copper layer is not greatly different from that of copper, and the silicon nano layer is used as a transition layer, so that the interface between the copper silicide (Cu 5 Si) layer and the ceramic layer is wetted, and the bonding strength of the copper silicide (Cu 5 Si) layer and the ceramic layer is ensured.
3. The ceramic matrix composite material heat dissipation substrate has the advantages of thinner overall thickness, about 1-2mm, small heat accumulation and quick heat dissipation. In addition, the C f/SiC layer of 0.1-0.2mm and the CVD-SiC material of 0.2-1 mm on one side can ensure the flexural strength although the thickness is thinner.
4. The copper silicide (Cu 5 Si) layer adopts a vacuum metal melting process, so that the defect that the bonding interface of the ceramic layer and the copper layer has no air holes and the like is ensured, and the heat conduction performance is excellent.
5. The heat dissipation substrate of the ceramic matrix composite material prepared by the invention has the heat conductivity of more than 296W/(m.K), high fracture toughness and high flexural strength, and is suitable for being used on high-power modules.
Drawings
FIG. 1 is a schematic illustration of the preparation process of the present invention;
FIG. 2 shows the bonding strength of the heat dissipating substrates prepared in examples 1-5 and comparative example 1;
fig. 3 is a graph showing bending strength of the heat dissipating substrates prepared in examples 1 to 5 and comparative example 1;
FIG. 4 is the fracture toughness of the heat dissipating substrates prepared in examples 1-5 and comparative example 1;
Fig. 5 is thermal conductivity of the heat dissipating substrates prepared in examples 1-5 and comparative example 1.
In fig. 1, a carbon fiber cloth; 2. a C f/SiC layer; 3. a CVD-SiC layer; 4. a silicon nanolayer; 5. and a copper silicide layer.
Detailed Description
The principles and features of the present invention are described below with reference to the drawings, the examples are illustrated for the purpose of illustrating the invention and are not to be construed as limiting the scope of the invention. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1:
A ceramic matrix composite heat sink substrate comprising: a C f/SiC layer 2 with the thickness of 0.17mm, a CVD-SiC layer 3 with the thickness of 0.2mm on one side, a silicon nano layer 4 with the thickness of 15nm and a copper silicide layer 5 with the thickness of 0.2 mm; the CVD-SiC layer 3 is coated on the outer surface of the C f/SiC layer 2, the silicon nano layer 4 is coated on the upper surface of the CVD-SiC layer 3, and the copper silicide layer 5 is coated on the upper surface of the silicon nano layer 4; c f/SiC layer 2 is a silicon carbide ceramic matrix composite material reinforced by carbon fiber cloth 1.
The preparation method of the ceramic matrix composite heat dissipation substrate sequentially comprises the following steps (the schematic diagram of the preparation process is shown in figure 1):
S1: firstly, taking single-layer carbon fiber cloth 1, placing the single-layer carbon fiber cloth in a chemical vapor vacuum furnace in the direction perpendicular to the residual air flow direction, adopting a chemical vapor infiltration method (CVI) (the air flow parameter is bubbling hydrogen, diluted hydrogen is diluted argon=0.3L/min, 0.2L/min is 0.3L/min, the furnace pressure is 150Pa, and the deposition temperature is 950 ℃), and depositing a silicon carbide ceramic matrix on the surface of the single-layer carbon fiber cloth 1 to prepare a C f/SiC layer 2 (the thickness is 0.17 mm);
S2: continuously in the same chemical vapor vacuum furnace, changing the airflow parameters and the temperature parameters, namely, the airflow parameters are bubbling hydrogen: dilution of hydrogen: diluted argon = 1.5L/min:1.2L/min:1.5L/min, furnace pressure of 500Pa, deposition temperature of 1400 ℃, and coating and depositing a silicon carbide ceramic matrix on the outer surface of the C f/SiC layer 2 prepared in the step S1 by adopting a chemical vapor deposition method to prepare a CVD-SiC layer 3 (single-side thickness is 0.2 mm);
S3: after the preparation of the ceramic layer is finished, taking nano silicon powder with the grain diameter of 15nm as a raw material, placing the nano silicon powder in a vacuum evaporation furnace with the evaporation surface facing downwards, and evaporating nano silicon on the upper surface of the CVD-SiC layer 3 prepared in the step S2 by adopting a vacuum evaporation method (the temperature is 1700 ℃ and the furnace pressure is 120 Pa) to prepare a silicon nano layer 4 (the thickness is 15 nm);
S4: the 800-mesh copper silicide powder is used as a raw material, the thickness of the copper silicide powder buried on the silicon nano layer 4 is 1mm, then the silicon nano layer is placed in a graphite box with a cover, a copper silicide layer 5 (the thickness is 0.2 mm) is prepared on the upper surface of the silicon nano layer 4 prepared in the step S3 by adopting a vacuum metal melting method in a vacuum metal melting furnace at the temperature of 840 ℃, and the surface is polished after the silicon nano layer is discharged, so that the ceramic matrix composite heat dissipation substrate is prepared.
Example 2:
A ceramic matrix composite heat sink substrate comprising: a C f/SiC layer 2 with the thickness of 0.17mm, a CVD-SiC layer 3 with the thickness of 1mm on one side, a silicon nano layer 4 with the thickness of 100nm and a copper silicide layer 5 with the thickness of 0.4 mm; the CVD-SiC layer 3 is coated on the outer surface of the C f/SiC layer 2, the silicon nano layer 4 is coated on the upper surface of the CVD-SiC layer 3, and the copper silicide layer 5 is coated on the upper surface of the silicon nano layer 4; c f/SiC layer 2 is a silicon carbide ceramic matrix composite material reinforced by carbon fiber cloth 1.
The preparation method of the ceramic matrix composite heat dissipation substrate sequentially comprises the following steps:
s1: firstly, taking single-layer carbon fiber cloth 1, placing the single-layer carbon fiber cloth in a chemical vapor vacuum furnace in the direction perpendicular to the residual air flow direction, adopting a chemical vapor infiltration method (CVI) (the air flow parameter is bubbling hydrogen, diluted hydrogen is diluted argon=0.4L/min, 0.3L/min is 0.4L/min, the furnace pressure is 200Pa, and the deposition temperature is 1000 ℃), and depositing a silicon carbide ceramic matrix on the surface of the single-layer carbon fiber cloth 1 to prepare a C f/SiC layer 2 (the thickness is 0.17 mm);
S2: continuously in the same chemical vapor vacuum furnace, changing the airflow parameters and the temperature parameters, namely, the airflow parameters are bubbling hydrogen: dilution of hydrogen: diluted argon = 2L/min:1.5L/min:2L/min, the furnace pressure is 550Pa, the deposition temperature is 1450 ℃, a chemical vapor deposition method is adopted to coat and deposit a silicon carbide ceramic matrix on the outer surface of the C f/SiC layer 2 prepared in the step S1, and a CVD-SiC layer 3 (the thickness of one side is 1 mm) is prepared;
S3: after the preparation of the ceramic layer is finished, taking nano silicon powder with the grain diameter of 5nm as a raw material, placing the nano silicon powder in a vacuum evaporation furnace with the evaporation surface facing downwards, and evaporating nano silicon on the upper surface of the CVD-SiC layer 3 prepared in the step S2 by adopting a vacuum evaporation method (the temperature is 2000 ℃ and the furnace pressure is 150 Pa) to prepare a silicon nano layer 4 (the thickness is 100 nm);
S4: and (3) taking 750-mesh copper silicide powder as a raw material, embedding copper silicide powder with the thickness of 2mm on the silicon nano layer 4, then placing the silicon nano layer 4 in a graphite box with a cover, preparing a copper silicide layer 5 (with the thickness of 0.4 mm) on the upper surface of the silicon nano layer 4 prepared in the step (S3) by adopting a vacuum metal melting method in a vacuum metal melting furnace at the temperature of 830 ℃, and polishing the surface after discharging to obtain the ceramic matrix composite heat dissipation substrate.
Example 3:
A ceramic matrix composite heat sink substrate comprising: a C f/SiC layer 2 with the thickness of 0.1mm, a CVD-SiC layer 3 with the thickness of 0.3mm on one side, a silicon nano layer 4 with the thickness of 50nm and a copper silicide layer 5 with the thickness of 0.3 mm; the CVD-SiC layer 3 is coated on the outer surface of the C f/SiC layer 2, the silicon nano layer 4 is coated on the upper surface of the CVD-SiC layer 3, and the copper silicide layer 5 is coated on the upper surface of the silicon nano layer 4; c f/SiC layer 2 is a silicon carbide ceramic matrix composite material reinforced by carbon fiber cloth 1.
The preparation method of the ceramic matrix composite heat dissipation substrate sequentially comprises the following steps:
S1: firstly, taking single-layer carbon fiber cloth 1, placing the single-layer carbon fiber cloth in a chemical vapor vacuum furnace in the direction perpendicular to the residual air flow direction, adopting a chemical vapor infiltration method (CVI) (the air flow parameter is bubbling hydrogen, diluted hydrogen is diluted argon=0.2L/min, 0.1L/min is 0.2L/min, the furnace pressure is 100Pa, and the deposition temperature is 900 ℃), and depositing a silicon carbide ceramic matrix on the surface of the single-layer carbon fiber cloth 1 to prepare a C f/SiC layer 2 (the thickness is 0.1 mm);
s2: continuously in the same chemical vapor vacuum furnace, changing the airflow parameters and the temperature parameters, namely, the airflow parameters are bubbling hydrogen: dilution of hydrogen: diluted argon = 1L/min:1L/min:1L/min, furnace pressure 450Pa, deposition temperature 1350 ℃, and coating and depositing a silicon carbide ceramic matrix on the outer surface of the C f/SiC layer 2 prepared in the step S1 by adopting a chemical vapor deposition method to prepare a CVD-SiC layer 3 (the thickness of one side is 0.3 mm);
S3: after the preparation of the ceramic layer is finished, taking nano silicon powder with the grain diameter of 25nm as a raw material, placing the nano silicon powder in a vacuum evaporation furnace with the evaporation surface facing downwards, and evaporating nano silicon on the upper surface of the CVD-SiC layer 3 prepared in the step S2 by adopting a vacuum evaporation method (the temperature is 1500 ℃ and the furnace pressure is 100 Pa) to prepare a silicon nano layer 4 (the thickness is 50 nm);
S4: the 850-mesh copper silicide powder is used as a raw material, the thickness of the copper silicide powder buried on the silicon nano layer 4 is 1.5mm, then the silicon nano layer is placed in a graphite box with a cover, a copper silicide layer 5 (the thickness is 0.3 mm) is prepared on the upper surface of the silicon nano layer 4 prepared in the step S3 by adopting a vacuum metal melting method in a vacuum metal melting furnace at the temperature of 850 ℃, and the surface is polished after the copper silicide layer is discharged, so that the ceramic matrix composite heat dissipation substrate is prepared.
Example 4:
A ceramic matrix composite heat sink substrate comprising: a C f/SiC layer 2 with the thickness of 0.18mm, a CVD-SiC layer 3 with the thickness of 0.5mm on one side, a silicon nano layer 4 with the thickness of 60nm and a copper silicide layer 5 with the thickness of 0.35 mm; the CVD-SiC layer 3 is coated on the outer surface of the C f/SiC layer 2, the silicon nano layer 4 is coated on the upper surface of the CVD-SiC layer 3, and the copper silicide layer 5 is coated on the upper surface of the silicon nano layer 4; c f/SiC layer 2 is a silicon carbide ceramic matrix composite material reinforced by carbon fiber cloth 1.
The preparation method of the ceramic matrix composite heat dissipation substrate sequentially comprises the following steps:
S1: firstly, taking single-layer carbon fiber cloth 1, placing the single-layer carbon fiber cloth in a chemical vapor vacuum furnace in the direction perpendicular to the residual air flow direction, adopting a chemical vapor infiltration method (CVI) (the air flow parameter is bubbling hydrogen, diluted hydrogen is diluted argon=0.3L/min, 0.2L/min is 0.3L/min, the furnace pressure is 150Pa, and the deposition temperature is 950 ℃), and depositing a silicon carbide ceramic matrix on the surface of the single-layer carbon fiber cloth 1 to prepare a C f/SiC layer 2 (the thickness is 0.18 mm);
S2: continuously in the same chemical vapor vacuum furnace, changing the airflow parameters and the temperature parameters, namely, the airflow parameters are bubbling hydrogen: dilution of hydrogen: diluted argon = 1.5L/min:1.2L/min:1.5L/min, furnace pressure of 500Pa, deposition temperature of 1400 ℃, and coating and depositing a silicon carbide ceramic matrix on the outer surface of the C f/SiC layer 2 prepared in the step S1 by adopting a chemical vapor deposition method to prepare a CVD-SiC layer 3 (single-side thickness is 0.5 mm);
s3: after the preparation of the ceramic layer is finished, taking nano silicon powder with the grain diameter of 10nm as a raw material, placing the nano silicon powder in a vacuum evaporation furnace with the evaporation surface facing downwards, and evaporating nano silicon on the upper surface of the CVD-SiC layer 3 prepared in the step S2 by adopting a vacuum evaporation method (the temperature is 1700 ℃ and the furnace pressure is 120 Pa) to prepare a silicon nano layer 4 (the thickness is 60 nm);
S4: the 760 mesh copper silicide powder is used as raw material, the thickness of the copper silicide powder buried on the silicon nano layer 4 is 1.8mm, and then the copper silicide powder is placed in a graphite box with a cover, and the graphite box is placed in a vacuum metal melting furnace at 845 ℃. And (3) preparing a copper silicide layer 5 (with the thickness of 0.35 mm) on the upper surface of the silicon nano layer 4 prepared in the step (S3) by adopting a vacuum metal melting method, and polishing the surface after discharging to prepare the ceramic matrix composite heat dissipation substrate.
Example 5:
A ceramic matrix composite heat sink substrate comprising: a C f/SiC layer 2 with the thickness of 0.19mm, a CVD-SiC layer 3 with the thickness of 0.9mm on one side, a silicon nano layer 4 with the thickness of 90nm and a copper silicide layer 5 with the thickness of 0.39 mm; the CVD-SiC layer 3 is coated on the outer surface of the C f/SiC layer 2, the silicon nano layer 4 is coated on the upper surface of the CVD-SiC layer 3, and the copper silicide layer 5 is coated on the upper surface of the silicon nano layer 4; c f/SiC layer 2 is a silicon carbide ceramic matrix composite material reinforced by carbon fiber cloth 1.
The preparation method of the ceramic matrix composite heat dissipation substrate sequentially comprises the following steps:
S1: firstly, taking single-layer carbon fiber cloth 1, placing the single-layer carbon fiber cloth in a chemical vapor vacuum furnace in the direction perpendicular to the residual air flow direction, and adopting a chemical vapor infiltration method (CVI) (the air flow parameter is bubbling hydrogen, diluted hydrogen is diluted argon=0.35L/min, 0.25L/min is 0.35L/min, the furnace pressure is 155Pa, and the deposition temperature is 955 ℃), so as to deposit a silicon carbide ceramic matrix on the surface of the single-layer carbon fiber cloth 1, thereby preparing a C f/SiC layer 2 (the thickness is 0.19 mm);
s2: continuously in the same chemical vapor vacuum furnace, changing the airflow parameters and the temperature parameters, namely, the airflow parameters are bubbling hydrogen: dilution of hydrogen: diluted argon = 1.8L/min:1.3L/min:1.8L/min, the furnace pressure is 520Pa, the deposition temperature is 1430 ℃, and a chemical vapor deposition method is adopted to coat and deposit a silicon carbide ceramic matrix on the outer surface of the C f/SiC layer 2 prepared in the step S1, so that a CVD-SiC layer 3 (the thickness of one side is 0.9 mm) is prepared;
s3: after the preparation of the ceramic layer is finished, taking nano silicon powder with the grain diameter of 24nm as a raw material, placing the nano silicon powder in a vacuum evaporation furnace with the evaporation surface facing downwards, and adopting a vacuum evaporation method (the temperature is 1750 ℃ and the furnace pressure is 125 Pa) to evaporate nano silicon on the upper surface of the CVD-SiC layer 3 prepared in the step S2 so as to prepare a silicon nano layer 4 (the thickness is 90 nm);
S4: the 830-mesh copper silicide powder is used as a raw material, the silicon nano layer 4 is buried with the copper silicide powder with the thickness of 1.8mm, then the copper silicide powder is placed in a graphite box with a cover, a vacuum metal melting furnace is adopted to prepare a copper silicide layer 5 (with the thickness of 0.39 mm) on the upper surface of the silicon nano layer 4 prepared in the step S3 under the condition of 848 ℃ by adopting a vacuum metal melting method, and the surface is polished after the copper silicide layer is discharged, so that the ceramic matrix composite heat dissipation substrate is prepared.
Comparative example 1:
a ceramic matrix composite heat sink substrate, excluding the silicon nanolayer 4, was the same as in example 5.
Test examples
1. Binding strength detection
The ceramic matrix composite heat dissipating substrates prepared in examples 1 to 5 and comparative example 1 were tested for interlayer bonding strength according to ASTM-C633-01, STANDARD TEST Method for Adhesion or Cohesion Strength of THERMAL SPRAY Coatings, and the results are shown in FIG. 2.
As can be seen from FIG. 2, the average bonding strength of the ceramic matrix composite heat dissipation substrate prepared by the invention reaches 34.2MPa, and the interlayer bonding strength of the comparative sample is only 20MPa.
2. Flexural Strength
The ceramic matrix composite heat dissipating substrates prepared in examples 1 to 5 and comparative example 1 were tested for flexural strength according to ASTM-C1341-13S"tandard Test Method for Flexural Properties of Continuous Fiber-Reinforced Advanced Ceramic Composites1",, and the results are shown in fig. 3.
As can be seen from FIG. 3, the average bending strength of the ceramic matrix composite heat dissipation substrate prepared by the invention reaches 355.8MPa.
3. Fracture toughness
The ceramic matrix composite heat dissipating substrates prepared in examples 1-5 and comparative example 1 were tested for fracture toughness according to ASTM C1421-18"Standard Test Methods for Determination of Fracture Toughness of Advanced Ceramics at Ambient Temperature",.
As can be seen from FIG. 4, the fracture toughness of the ceramic matrix composite heat dissipation substrate prepared by the invention is more than or equal to 7 MPa.m 1/2.
4. Thermal conductivity
The ceramic matrix composite heat dissipating substrates prepared in examples 1-5 and comparative example 1 were tested for thermal conductivity according to ASTM E1461-13, "STANDARD TEST Method for Thermal Diffusivity by the Flash Method", the results of which are shown in FIG. 5.
As can be seen from FIG. 5, the average thermal conductivity of the ceramic matrix composite heat dissipation substrate prepared by the invention is 296W/(m.K), and the interlayer bonding strength of the comparative sample is only 160W/(m.K).
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (10)
1. A ceramic matrix composite heat sink substrate, the heat sink substrate comprising: a C f/SiC layer (2), a CVD-SiC layer (3), a silicon nano layer (4) and a copper silicide layer (5); the CVD-SiC layer (3) is coated on the outer surface of the C f/SiC layer (2), the silicon nano layer (4) is coated on the upper surface of the CVD-SiC layer (3), and the copper silicide layer (5) is coated on the upper surface of the silicon nano layer (4); the C f/SiC layer (2) is a silicon carbide ceramic matrix composite material reinforced by carbon fiber cloth (1).
2. The ceramic matrix composite heat sink substrate according to claim 1, wherein the thickness of the C f/SiC layer (2) is 0.1-0.2mm.
3. The ceramic matrix composite heat sink substrate according to claim 1, wherein the CVD-SiC layer (3) has a thickness of 0.2-1mm on one side of the C f/SiC layer (2).
4. The ceramic matrix composite heat sink substrate according to claim 1, wherein the thickness of the silicon nanolayer (4) is 15-100nm.
5. Ceramic matrix composite heat sink substrate according to claim 1, characterized in that the thickness of the copper silicide layer (5) is 0.2-0.4mm.
6. The method for preparing a ceramic matrix composite heat dissipating substrate according to any one of claims 1 to 5, comprising the steps of, in order:
s1: depositing a silicon carbide ceramic matrix on the surface of the single-layer carbon fiber cloth (1) by adopting a chemical vapor infiltration method to prepare a C f/SiC layer (2);
S2: coating and depositing a silicon carbide ceramic matrix on the outer surface of the C f/SiC layer (2) prepared in the step S1 by adopting a chemical vapor deposition method to prepare a CVD-SiC layer (3);
s3: evaporating nano silicon on the upper surface of the CVD-SiC layer (3) prepared in the step S2 by using nano silicon powder as a raw material by adopting a vacuum evaporation method to prepare a silicon nano layer (4);
S4: and (3) preparing a copper silicide layer (5) on the upper surface of the silicon nano layer (4) prepared in the step (S3) by using copper silicide powder as a raw material and adopting a vacuum metal melting method to prepare the ceramic matrix composite heat dissipation substrate.
7. The method for manufacturing a ceramic matrix composite heat sink substrate according to claim 5, wherein in steps S1 and S2, the C f/SiC layer (2) and the CVD-SiC layer (3) are sequentially formed by changing reaction parameters in the same chemical vapor vacuum apparatus.
8. The method for manufacturing a ceramic matrix composite heat dissipating substrate as set forth in claim 5, wherein in step S3, the nano silicon powder has a particle size of 5 to 25nm.
9. The method of manufacturing a ceramic matrix composite heat sink substrate according to claim 5, wherein in step S4, the mesh number of the copper silicide powder is 750-850 mesh.
10. Use of the ceramic matrix composite heat sink substrate of any one of claims 1-5 in the manufacture of semiconductor devices.
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