CN111484330A - Diamond-enhanced silicon carbide substrate, preparation method thereof and electronic product - Google Patents
Diamond-enhanced silicon carbide substrate, preparation method thereof and electronic product Download PDFInfo
- Publication number
- CN111484330A CN111484330A CN202010284460.7A CN202010284460A CN111484330A CN 111484330 A CN111484330 A CN 111484330A CN 202010284460 A CN202010284460 A CN 202010284460A CN 111484330 A CN111484330 A CN 111484330A
- Authority
- CN
- China
- Prior art keywords
- diamond
- silicon carbide
- carbide substrate
- casting
- casting blank
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000758 substrate Substances 0.000 title claims abstract description 104
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 86
- 239000010432 diamond Substances 0.000 title claims abstract description 84
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 83
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000005266 casting Methods 0.000 claims abstract description 140
- 238000010345 tape casting Methods 0.000 claims abstract description 67
- 239000002002 slurry Substances 0.000 claims abstract description 57
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 49
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 49
- 239000010439 graphite Substances 0.000 claims abstract description 49
- 238000000498 ball milling Methods 0.000 claims abstract description 46
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 31
- 239000002270 dispersing agent Substances 0.000 claims abstract description 25
- 239000002904 solvent Substances 0.000 claims abstract description 25
- 239000011230 binding agent Substances 0.000 claims abstract description 23
- 239000004014 plasticizer Substances 0.000 claims abstract description 23
- 238000001171 gas-phase infiltration Methods 0.000 claims abstract description 16
- 238000001764 infiltration Methods 0.000 claims description 44
- 230000008595 infiltration Effects 0.000 claims description 44
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 34
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 30
- 238000005238 degreasing Methods 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 22
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 21
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 15
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 9
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 claims description 9
- 239000004359 castor oil Substances 0.000 claims description 6
- 235000019438 castor oil Nutrition 0.000 claims description 6
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- UBOXGVDOUJQMTN-UHFFFAOYSA-N trichloroethylene Natural products ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000012808 vapor phase Substances 0.000 claims 1
- 238000000465 moulding Methods 0.000 abstract description 7
- 238000001035 drying Methods 0.000 description 45
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 24
- 238000004321 preservation Methods 0.000 description 19
- 229910052710 silicon Inorganic materials 0.000 description 13
- 239000010703 silicon Substances 0.000 description 13
- 229910052786 argon Inorganic materials 0.000 description 12
- 239000000463 material Substances 0.000 description 11
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 11
- 238000005245 sintering Methods 0.000 description 11
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 10
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical group CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 10
- 238000005520 cutting process Methods 0.000 description 10
- 238000001914 filtration Methods 0.000 description 9
- -1 polytetrafluoroethylene Polymers 0.000 description 9
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 9
- 239000004810 polytetrafluoroethylene Substances 0.000 description 9
- 239000000047 product Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 7
- 238000004100 electronic packaging Methods 0.000 description 7
- 239000007788 liquid Substances 0.000 description 6
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- 238000004806 packaging method and process Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 239000005055 methyl trichlorosilane Substances 0.000 description 3
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 description 3
- 238000004377 microelectronic Methods 0.000 description 3
- 239000012466 permeate Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 2
- 229920006362 Teflon® Polymers 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- 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
- 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
- C04B35/52—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 carbon, e.g. graphite
- C04B35/528—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 carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components
- C04B35/532—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 carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components containing a carbonisable binder
-
- C—CHEMISTRY; METALLURGY
- 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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- 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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
- C04B35/65—Reaction sintering of free metal- or free silicon-containing compositions
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/12—Mountings, e.g. non-detachable insulating substrates
- H01L23/14—Mountings, e.g. non-detachable insulating substrates characterised by the material or its electrical properties
- H01L23/15—Ceramic or glass substrates
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
- H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
- H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
- H01L23/3731—Ceramic materials or glass
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
- H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
- H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
- H01L23/3732—Diamonds
-
- C—CHEMISTRY; METALLURGY
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
- C04B2235/425—Graphite
-
- C—CHEMISTRY; METALLURGY
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
- C04B2235/427—Diamond
-
- C—CHEMISTRY; METALLURGY
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/428—Silicon
-
- C—CHEMISTRY; METALLURGY
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/614—Gas infiltration of green bodies or pre-forms
-
- C—CHEMISTRY; METALLURGY
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
-
- C—CHEMISTRY; METALLURGY
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6565—Cooling rate
-
- C—CHEMISTRY; METALLURGY
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
Abstract
The invention relates to a diamond-enhanced silicon carbide substrate, a preparation method thereof and an electronic product. The preparation method of the diamond-enhanced silicon carbide substrate comprises the following steps: carrying out wet ball milling on diamond, graphite, a dispersing agent, a binder, a plasticizer and a solvent to obtain casting slurry; carrying out tape casting molding on the tape casting slurry to obtain a tape casting blank, wherein the thickness of the tape casting blank is 0.3-0.55 mm; and carrying out gas-phase infiltration on the casting blank and the silicon powder to obtain the diamond-enhanced silicon carbide substrate. The preparation method of the diamond-enhanced silicon carbide substrate can ensure that the prepared diamond-enhanced silicon carbide substrate has controllable size, high density and good thermal conductivity.
Description
Technical Field
The invention relates to the field of ceramic materials, in particular to a diamond-reinforced silicon carbide substrate, a preparation method thereof and an electronic product.
Background
The comprehensive performance of the high-thermal-conductivity electronic packaging substrate material is a key factor for restricting the integration of the microelectronic industry. In recent years, with the development of miniaturization, high power and high integration in the microelectronic industry, higher requirements are put on the performance of packaging substrate materials. Diamond/silicon carbide has been widely studied as a third generation electronic packaging material because of its excellent properties such as high thermal conductivity, high hardness, and low thermal expansion coefficient. At present, methods such as Hot Isostatic Pressing (HIP), high-temperature high-pressure sintering (HIHP) and the like are mostly adopted for preparing the diamond/silicon carbide composite material, but the method is difficult to prepare large-size products with thin thickness, and the prepared material has low density and cannot meet the requirements of high-thermal-conductivity packaging substrate materials for microelectronic heat dissipation.
Disclosure of Invention
Therefore, it is necessary to provide a method for preparing a diamond-enhanced silicon carbide substrate, so that the prepared diamond-enhanced silicon carbide substrate has controllable size and high density, aiming at the problems of limited size and low density of the traditional diamond/silicon carbide substrate.
Further, it is necessary to provide a diamond-reinforced silicon carbide substrate and an electronic product.
A preparation method of a diamond-enhanced silicon carbide substrate comprises the following steps:
carrying out wet ball milling on diamond, graphite, a dispersing agent, a binder, a plasticizer and a solvent to obtain casting slurry;
carrying out tape casting on the tape casting slurry to obtain a tape casting blank, wherein the thickness of the tape casting blank is 0.3-0.55 mm; and
and carrying out gas-phase infiltration on the casting blank and the silicon powder to obtain the diamond-enhanced silicon carbide substrate.
In one embodiment, in the step of performing gas-phase infiltration on the casting blank and the silicon powder, the infiltration temperature is 1450-1650 ℃, and the infiltration time is 1-5 h.
In one embodiment, the mass ratio of the diamond to the graphite is 100: 10-100: 24.
in one embodiment, the dispersant is selected from one of triethyl phosphate and castor oil.
In one embodiment, the solvent is one of isopropanol/toluene, ethanol/methyl ethyl ketone, ethanol/ethyl acetate, trichloroethylene/methyl ethyl ketone, and ethanol/water.
In one embodiment, the step of wet ball milling the diamond, the graphite, the dispersant, the binder, the plasticizer and the solvent is as follows: firstly, performing ball milling dispersion on the diamond, the graphite and the dispersing agent in the solvent for 5-7 h, then adding the binder and the plasticizer, and continuing ball milling for 5-7 h to obtain the casting slurry.
In one embodiment, before the step of casting the casting slurry, the step of casting further comprises: and carrying out defoaming treatment on the casting slurry.
In one embodiment, in the step of defoaming the casting slurry, the vacuum degree is-100 KPa to-87.5 KPa, and the defoaming time is 30min to 50 min.
In one embodiment, before the step of gas-phase infiltration of the casting blank and the silicon powder, the method further comprises: and carrying out degreasing treatment on the casting blank.
In one embodiment, the step of degreasing the casting blank comprises: degreasing the casting blank at 300-900 ℃ for 1-3 h, cooling to 100 ℃ at the speed of less than 5 ℃/min, and cooling along with the furnace.
The diamond-reinforced silicon carbide substrate prepared by the preparation method of the diamond-reinforced silicon carbide substrate is provided.
An electronic product, wherein a packaging substrate of the electronic product is the diamond-enhanced silicon carbide substrate.
According to the preparation method of the diamond-reinforced silicon carbide substrate, wet ball milling is carried out on diamond, graphite and the like to obtain casting slurry, then casting forming is carried out to obtain casting blanks with the thickness of 0.3-0.55 mm and controllable sizes, the requirement of the industry on the thickness of the heat dissipation substrate is met, finally silicon vapor permeates into the casting blanks through silicon vapor infiltration, the silicon vapor permeating into the casting blanks and graphite contained in the casting blanks are subjected to silicon-carbon reaction to generate silicon carbide, and the casting blanks are densified to obtain the dense diamond-reinforced silicon carbide substrate. The preparation method not only overcomes the limitation of the traditional forming mode by the size of a grinding tool, but also solves the problem of low density of the material.
Drawings
Fig. 1 is a process flow diagram of one embodiment of a method of making a diamond enhanced silicon carbide substrate;
fig. 2 is a scanning electron microscope image of fractures of the diamond-reinforced silicon carbide substrate prepared in example 1.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following description taken in conjunction with the accompanying drawings. The detailed description sets forth the preferred embodiments of the invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Referring to fig. 1, a method for manufacturing a diamond enhanced silicon carbide substrate according to an embodiment includes the steps of:
step S110: and carrying out wet ball milling on the diamond, the graphite, the dispersing agent, the binder, the plasticizer and the solvent to obtain casting slurry.
Wherein the dispersant is selected from one of triethyl phosphate and castor oil. The dispersant can uniformly disperse each raw material in the solvent.
The binder is polyvinyl butyral (PVB). The binder is capable of binding the raw materials together.
The plasticizer is dioctyl phthalate. The addition of the binder and plasticizer to the raw materials can increase the strength of the casting blank and improve the toughness and ductility of the casting blank to facilitate separation from the substrate material.
The solvent is one of isopropanol/toluene, ethanol/ethyl acetate, ethanol/methyl ethyl ketone, trichloroethylene/methyl ethyl ketone and ethanol/water. It is to be noted that, in this context, "/" indicates a mixture, such as isopropanol/toluene indicates a mixture of isopropanol and toluene. The uniformly dispersed and stable casting slurry can be obtained by mixing the diamond and the graphite with the dispersing agent, the binder, the plasticizer and the solvent, and the subsequent casting molding is facilitated.
In one embodiment, the mass ratio of diamond to graphite is 100: 10-100: 24. the mass ratio of the diamond to the dispersing agent, the plasticizer and the binder is 100:6.6:13: 13.
Further, step S110 is: firstly, performing ball milling dispersion on diamond, graphite and a dispersing agent in a solvent for 5-7 h, then adding a binder and a plasticizer, and continuing ball milling for 5-7 h to obtain casting slurry. The raw materials can be fully and uniformly mixed by adopting a step-by-step ball milling and mixing mode.
In one embodiment, the viscosity of the casting paste is 8000mPaS to 8340 mPaS. The function of controlling the viscosity of the slurry is to facilitate the subsequent tape casting process, and the viscosity of the slurry is related to the thickness of the casting blank in the tape casting process. In the present embodiment, the viscosity of the casting slurry can be set in accordance with the viscosity requirement of the slurry for the usual casting.
Step S120: and (4) defoaming the casting slurry.
Specifically, the defoaming treatment is performed under vacuum conditions. In one embodiment, the vacuum degree is-100 KPa to-87.5 KPa. The defoaming time is 30-50 min. Through defoaming treatment, bubbles in the casting slurry are discharged, the existence of large pores in a subsequent casting blank is avoided, the viscosity of the casting slurry is controlled within a certain range, and the casting slurry is beneficial to subsequent casting forming.
Step S130: and carrying out tape casting on the tape casting slurry to obtain a tape casting blank, wherein the thickness of the tape casting blank is 0.3-0.55 mm.
In one embodiment, in casting the casting slurry, the blade height is 1mm to 3 mm. The casting speed was 0.02 m/min. And in the step of carrying out tape casting molding on the tape casting slurry, partition type drying is adopted. In one embodiment, the temperature of the first drying zone is 40 ℃, the temperature of the second drying zone is 55 ℃, and the temperature of the third drying zone is 70 ℃. It is understood that, in other embodiments, the temperatures of the first drying zone, the second drying zone and the third drying zone are not limited to the above values, and the temperatures may be adjusted according to actual conditions. The adoption of the zone drying mode can slowly remove the solvent, avoid the conditions of cracking and the like caused by too fast volatilization of the solvent, and obtain a uniform casting blank through drying.
The casting molding mode has the advantages of stable process, high repeatability of the performance of the molded blank, high consistency of the size, uniform performance of the blank and the like. And the size of the substrate can be controlled by the tape casting forming mode, and the problem that the size of a die is limited in the traditional cold press forming process is solved.
The casting blank with the thickness of 0.3 mm-0.55 mm is prepared by a casting forming mode, and the requirement (0.38 mm-0.5 mm) of the thickness of a common heat conducting substrate in the industry can be met.
Further, after the step S130, before the step S140, a step of cutting the casting blank is further included so that the size of the casting blank satisfies the requirement.
Step S140: and degreasing the casting blank.
Specifically, in step S140, the temperature of the degreasing treatment is 300-900 ℃, and the heat preservation time is 1-3 h. The degreasing treatment is performed in a protective atmosphere. The protective atmosphere is argon or nitrogen. Further, in one embodiment, the step of subjecting the casting blank to degreasing treatment is: degreasing the casting blank at 300-900 ℃ for 1-3 h under the protective atmosphere, then cooling to 100 ℃ at the speed of less than 5 ℃/min, and then cooling along with the furnace. Since the casting base contains organic agents such as a dispersant, a binder, and a plasticizer, the organic agents are melted, decomposed, and volatilized at the time of subsequent sintering, and the substrate is deformed, cracked, and the like, thereby affecting the quality of the substrate. Therefore, the casting blank needs to be degreased before sintering. Similarly, after the degreasing treatment is finished, the temperature is lowered at a relatively slow speed to prevent the casting blank from being deformed to affect the quality of the substrate.
Step S150: and carrying out gas-phase infiltration on the casting blank and the silicon powder to obtain the diamond-enhanced silicon carbide substrate.
Wherein, the purity of the silicon powder used in the step S150 is greater than 95%. The silicon powder has high purity, and the influence of impurities on the performance of the prepared diamond enhanced silicon carbide substrate can be avoided as much as possible.
And in the process of carrying out gas-phase infiltration on the casting blank and the silicon powder, the infiltration temperature is 1450-1650 ℃, and the infiltration time is 1-5 h. Furthermore, the infiltration temperature is 1575-1600 ℃. In one embodiment, the infiltration pressure is less than 30 Pa. And applying pressure in the infiltration process, so that the reaction of the silicon powder and the graphite is carried out in the direction of producing silicon carbide on one hand, and the compactness of the prepared substrate is further improved on the other hand. In the gas-phase infiltration process, silicon powder is melted and evaporated into silicon vapor, and the silicon vapor diffuses into the casting blank and fully reacts with graphite to generate silicon carbide, so that the obtained diamond enhanced silicon carbide substrate is densified. Compared with the CVI (chemical vapor infiltration) process, the density of the prepared diamond silicon carbide substrate can be further improved by adopting the silicon vapor infiltration.
Specifically, step S150 is performed in a vacuum infiltration furnace. In one embodiment, step S150 is: and (3) placing the casting blank into a graphite box filled with silicon powder, separating the casting blank from the silicon powder, and then placing the graphite box into a vacuum infiltration furnace for gas-phase infiltration.
The diamond-reinforced silicon carbide substrate with the density of more than 96 percent and even up to 99 percent can be prepared through the steps S110 to S150, and the diamonds are uniformly distributed in the substrate and well combined with the substrate.
In the traditional technology, the diamond silicon carbide composite material is prepared by permeating gas phase silicon into a diamond and graphite mixed prefabricated body and carrying out silicon-carbon reaction under the condition of 1600 ℃ non-pressure argon protection, the prepared material has extremely high density, and the thermal conductivity and the thermal expansion coefficient are respectively higher than 500W/(m × k) and lower than 5 × 10 at the temperature of below 500 DEG C-6and/K, shows excellent thermophysical properties. However, due to the limitation of the grinding tool, it is impossible to prepare a large-sized thin substrate material having a thickness of 0.38mm to 0.50 mm.
A substrate material with the thickness of 3mm is prepared through multiple casting and CVI, the thermal conductivity of the substrate material reaches 241W/(m × k), and the thermophysical performance of the substrate material is far greater than that of the currently applied Al2O3A substrate. However, the composite material prepared by the CVI method has density gradient, so that the density is reduced, and the further improvement of the thermal conductivity is limited.
The preparation method of the diamond-reinforced silicon carbide substrate at least has the following advantages:
(1) according to the preparation method of the diamond-enhanced silicon carbide substrate, wet ball milling is carried out on diamond, graphite and the like to obtain casting slurry, then casting forming is carried out to obtain a casting blank with controllable size and uniform and porous property, finally silicon vapor permeates into the casting blank through silicon vapor infiltration, the silicon vapor permeating into the casting blank and graphite contained in the casting blank are subjected to silicon-carbon reaction to generate silicon carbide, and the casting blank is densified to obtain the compact diamond-enhanced silicon carbide substrate. The preparation method not only overcomes the limitation of the size of a cold press molding grinding tool, but also solves the problem of low density of the composite material in the CVI process.
(2) The diamond-enhanced silicon carbide substrate prepared by the preparation method of the diamond-enhanced silicon carbide substrate has the characteristics of controllable size, low density, high strength and high thermal conductivity, is expected to become an ideal electronic packaging substrate, and has important significance for promoting the development of ceramic-based electronic packaging substrates.
(3) The preparation method of the diamond-reinforced silicon carbide substrate has the advantages of simple preparation process and short production period, and is suitable for large-scale production.
A diamond-reinforced silicon carbide substrate according to an embodiment is produced by the method for producing a diamond-reinforced silicon carbide substrate. The thickness of the diamond enhanced silicon carbide substrate is 0.3 mm-0.55 mm, and the density is more than 96%. The diamond-enhanced silicon carbide substrate has the characteristics of controllable size, low density, high strength and high thermal conductivity, is expected to become an ideal electronic packaging substrate, and has important significance for promoting the development of ceramic-based electronic packaging substrates.
In an electronic product according to an embodiment, the package substrate of the electronic product is the diamond-reinforced silicon carbide substrate according to the embodiment. The diamond-enhanced silicon carbide substrate has the advantages of controllable size, small thickness, high density, high thermal conductivity and the like, and meets the requirements of high-thermal-conductivity electronic packaging substrates, so that the diamond-enhanced silicon carbide substrate can be used as the packaging substrate of electronic products.
The following are specific examples:
example 1
The preparation process of the diamond-reinforced silicon carbide substrate of the embodiment is specifically as follows:
(1) adding diamond, graphite, a dispersing agent (triethyl phosphate) and a solvent (ethanol and ethyl acetate azeotropic liquid) into a polytetrafluoroethylene ball milling tank according to the proportion of 50g, 5g, 3.3g and 21.7g, carrying out ball milling for 6 hours, adding 6.5g of a binding agent (PVB) and 6.5g of a plasticizer (dioctyl phthalate) into the ball milling tank, and continuing ball milling for 6 hours to obtain casting slurry with the viscosity of about 8000 mPaS.
(2) And (2) carrying out vacuum defoaming on the casting slurry prepared in the step (1) for 30min under a negative pressure environment of-87.5 KPa, and then filtering.
(3) And (3) carrying out tape casting on the tape casting slurry treated in the step (2) by using a tape casting machine, controlling the height of a scraper to be 1.3mm, controlling the tape casting speed to be 0.02m/min, and setting the temperatures of the first drying zone, the second drying zone and the third drying zone to be 40 ℃, 55 ℃ and 70 ℃ respectively to obtain a tape casting blank with the thickness of 0.47 mm. And cutting the casting blank after drying.
(4) And (3) degreasing the casting blank in an argon environment, wherein the degreasing temperature is set to be 500 ℃, and the heat preservation time is 120 min. After the heat preservation is finished, the temperature is reduced to 100 ℃ at the speed of 2 ℃/min, and then the furnace is cooled.
(5) And (3) placing the degreased casting blank into a graphite box containing silicon powder, separating the casting blank from the silicon powder by using a graphite rod, and then placing the whole casting blank into a high-vacuum sintering furnace for vacuum gas phase infiltration. The infiltration temperature is 1575 ℃, the infiltration pressure is 2Pa, and the infiltration time is 3 h. The obtained density is about 3.1g/cm after furnace cooling3And the density is more than 96 percent.
The thermal conductivity of the diamond-enhanced silicon carbide substrate prepared in this example was about 140W/(m × k) and the coefficient of thermal expansion was 2.1 × 10-6/K。
The fracture morphology of the diamond-enhanced silicon carbide substrate prepared in example 1 was observed with a scanning electron microscope to obtain fig. 2. As can be seen from fig. 2, the prepared diamond-enhanced silicon carbide substrate has extremely high density, and no obvious gap is seen. The diamond has complete appearance and no graphitization phenomenon.
Example 2
The preparation process of the diamond-reinforced silicon carbide substrate of the embodiment is specifically as follows:
(1) adding diamond, graphite, a dispersing agent (triethyl phosphate) and a solvent (ethanol and ethyl acetate azeotropic liquid) into a polytetrafluoroethylene ball milling tank according to the proportion of 50g, 10g, 3.3g and 21.7g, carrying out ball milling for 6 hours, adding 6.5g of a binding agent (PVB) and 6.5g of a plasticizer (dioctyl phthalate) into the ball milling tank, and continuing ball milling for 6 hours to obtain casting slurry with the viscosity of about 8210 mPAS.
(2) And (2) carrying out vacuum defoaming on the casting slurry prepared in the step (1) for 30min under a negative pressure environment of-87.5 KPa, and then filtering.
(3) And (3) carrying out tape casting on the tape casting slurry treated in the step (2) by using a tape casting machine, controlling the height of a scraper to be 1.3mm, controlling the tape casting speed to be 0.02m/min, and setting the temperatures of the first drying zone, the second drying zone and the third drying zone to be 40 ℃, 55 ℃ and 70 ℃ respectively to obtain a tape casting blank with the thickness of 0.51 mm. And cutting the casting blank after drying.
(4) And (3) degreasing the casting blank in an argon environment, wherein the degreasing temperature is set to be 500 ℃, and the heat preservation time is 120 min. After the heat preservation is finished, the temperature is reduced to 100 ℃ at the speed of 2 ℃/min, and then the furnace is cooled.
(5) And (3) placing the degreased casting blank into a graphite box containing silicon powder, separating the casting blank from the silicon powder by using a graphite rod, and then placing the whole casting blank into a high-vacuum sintering furnace for vacuum gas phase infiltration. The infiltration temperature is 1575 ℃, the infiltration pressure is 2Pa, and the infiltration time is 3 h. The obtained density is about 3.12g/cm after furnace cooling3And the density is more than 96.7 percent.
The thermal conductivity of the diamond-enhanced silicon carbide substrate prepared in this example was about 153W/(m × k) and the coefficient of thermal expansion was 1.8 × 10-6/K。
Example 3
The preparation process of the diamond-reinforced silicon carbide substrate of the embodiment is specifically as follows:
(1) adding diamond, graphite, a dispersing agent (triethyl phosphate) and a solvent (ethanol and ethyl acetate azeotropic liquid) into a polytetrafluoroethylene ball milling tank according to the proportion of 50g, 5g, 3.3g and 21.7g, carrying out ball milling for 6 hours, adding 6.5g of a binding agent (PVB) and 6.5g of a plasticizer (dioctyl phthalate) into the ball milling tank, and continuing ball milling for 6 hours to obtain casting slurry with the viscosity of about 8000 mPaS.
(2) And (2) carrying out vacuum defoaming on the casting slurry prepared in the step (1) for 30min under a negative pressure environment of-87.5 KPa, and then filtering.
(3) And (3) carrying out tape casting on the tape casting slurry treated in the step (2) by using a tape casting machine, controlling the height of a scraper to be 1.3mm, controlling the tape casting speed to be 0.02m/min, and setting the temperatures of the first drying zone, the second drying zone and the third drying zone to be 40 ℃, 55 ℃ and 70 ℃ respectively to obtain a tape casting blank with the thickness of 0.47 mm. And cutting the casting blank after drying.
(4) And (3) degreasing the casting blank in an argon environment, wherein the degreasing temperature is set to be 500 ℃, and the heat preservation time is 120 min. After the heat preservation is finished, the temperature is reduced to 100 ℃ at the speed of 2 ℃/min, and then the furnace is cooled.
(5) Placing the degreased multi-flow casting blank in a graphite box containing silicon powder, and using a graphite rod to make the multi-flow casting blank flowSeparating the rolled blank from the silicon powder, and then putting the whole body in a high vacuum sintering furnace for vacuum gas phase permeation. The infiltration temperature is 1600 ℃, the infiltration pressure is 2Pa, and the infiltration time is 3 h. The obtained density is about 3.23g/cm after furnace cooling3And the density is more than 98 percent.
The thermal conductivity of the diamond-enhanced silicon carbide substrate prepared in this example was about 148W/(m × k) and the coefficient of thermal expansion was 1.9 × 10-6/K。
Example 4
The preparation process of the diamond-reinforced silicon carbide substrate of the embodiment is specifically as follows:
(1) adding diamond, graphite, a dispersing agent (triethyl phosphate) and a solvent (ethanol and ethyl acetate azeotropic liquid) into a polytetrafluoroethylene ball milling tank according to the proportion of 50g, 10g, 3.3g and 21.7g, carrying out ball milling for 6 hours, adding 6.5g of a binding agent (PVB) and 6.5g of a plasticizer (dioctyl phthalate) into the ball milling tank, and continuing ball milling for 6 hours to obtain casting slurry with the viscosity of about 8210 mPAS.
(2) And (2) carrying out vacuum defoaming on the casting slurry prepared in the step (1) for 30min under a negative pressure environment of-87.5 KPa, and then filtering.
(3) And (3) carrying out tape casting on the tape casting slurry treated in the step (2) by using a tape casting machine, controlling the height of a scraper to be 1.3mm, controlling the tape casting speed to be 0.02m/min, and setting the temperatures of the first drying zone, the second drying zone and the third drying zone to be 40 ℃, 55 ℃ and 70 ℃ respectively to obtain a tape casting blank with the thickness of 0.51 mm. And cutting the casting blank after drying.
(4) And (3) degreasing the casting blank in an argon environment, wherein the degreasing temperature is set to be 500 ℃, and the heat preservation time is 120 min. After the heat preservation is finished, the temperature is reduced to 100 ℃ at the speed of 2 ℃/min, and then the furnace is cooled.
(5) And (3) placing the degreased casting blank into a graphite box containing silicon powder, separating the casting blank from the silicon powder by using a graphite rod, and then placing the whole casting blank into a high-vacuum sintering furnace for vacuum gas phase infiltration. The infiltration temperature is 1600 ℃, the infiltration pressure is 2Pa, and the infiltration time is 3 h. The obtained density is about 3.13g/cm after furnace cooling3And the density is more than 99 percent.
The thermal conductivity of the diamond-enhanced silicon carbide substrate prepared in this example was about 151W/(m × k) and the coefficient of thermal expansion was 1.7 × 10-6/K。
Example 5
The preparation process of the diamond-reinforced silicon carbide substrate of the embodiment is specifically as follows:
(1) adding diamond, graphite, a dispersant (castor oil) and a solvent (ethanol and ethyl acetate azeotrope) into a polytetrafluoroethylene ball milling tank according to the proportion of 50g, 12g, 3.3g and 21.7g, carrying out ball milling for 6 hours, adding 6.5g of a binder (PVB) and 6.5g of a plasticizer (dioctyl phthalate) into the polytetrafluoroethylene ball milling tank, and continuing ball milling for 6 hours to obtain casting slurry with the viscosity of about 8340 mPas.
(2) And (2) carrying out vacuum defoaming on the casting slurry prepared in the step (1) for 30min under a negative pressure environment of-87.5 KPa, and then filtering.
(3) And (3) carrying out tape casting on the tape casting slurry treated in the step (2) by using a tape casting machine, controlling the height of a scraper to be 1.3mm, controlling the tape casting speed to be 0.02m/min, and setting the temperatures of the first drying zone, the second drying zone and the third drying zone to be 40 ℃, 55 ℃ and 70 ℃ respectively to obtain a tape casting blank with the thickness of 0.53 mm. And cutting the casting blank after drying.
(4) And (3) degreasing the casting blank in an argon environment, wherein the degreasing temperature is set to be 500 ℃, and the heat preservation time is 120 min. After the heat preservation is finished, the temperature is reduced to 100 ℃ at the speed of 2 ℃/min, and then the furnace is cooled.
(5) And (3) placing the degreased casting blank into a graphite box containing silicon powder, separating the casting blank from the silicon powder by using a graphite rod, and then placing the whole casting blank into a high-vacuum sintering furnace for vacuum gas phase infiltration. The infiltration temperature is 1600 ℃, the infiltration pressure is 2Pa, and the infiltration time is 3 h. The obtained density is about 3.07g/cm after furnace cooling3And the density is more than 97.5 percent.
The thermal conductivity of the diamond-enhanced silicon carbide substrate prepared in this example was about 136W/(m × k) and the coefficient of thermal expansion was 1.34 × 10-6/K。
Example 6
The preparation process of the diamond-reinforced silicon carbide substrate of the embodiment is specifically as follows:
(1) diamond, graphite, a dispersant (castor oil) and a solvent (isopropanol/toluene) were added to a teflon ball mill tank in a ratio of 50g, 12g, 3.3g and 21.7g, ball milled for 5 hours, and then 6.5g of a binder (PVB), 6.5g of a plasticizer (dioctyl phthalate) were added thereto and ball milling was continued for 7 hours, to finally obtain a casting slurry having a viscosity of about 8340 mPaS.
(2) And (2) carrying out vacuum defoaming on the casting slurry prepared in the step (1) for 40min under a negative pressure environment of-100 KPa, and then filtering.
(3) And (3) carrying out tape casting molding on the tape casting slurry treated in the step (2) by using a tape casting machine, controlling the height of a scraper to be 1.3mm, controlling the tape casting speed to be 0.02m/min, and setting the temperatures of the first drying zone, the second drying zone and the third drying zone to be 40 ℃, 55 ℃ and 70 ℃ respectively to obtain a tape casting blank with the thickness of 0.50 mm. And cutting the casting blank after drying.
(4) And (3) degreasing the casting blank in an argon environment, wherein the degreasing temperature is set to 300 ℃, and the heat preservation time is 180 min. After the heat preservation is finished, the temperature is reduced to 100 ℃ at the speed of 4 ℃/min, and then the furnace is cooled.
(5) And (3) placing the degreased casting blank into a graphite box containing silicon powder, separating the casting blank from the silicon powder by using a graphite rod, and then placing the whole casting blank into a high-vacuum sintering furnace for vacuum gas phase infiltration. The infiltration temperature is 1450 ℃, the infiltration pressure is 10Pa, and the infiltration time is 5 h. The obtained density is about 2.94g/cm after furnace cooling3And the density is more than 83 percent.
The thermal conductivity of the diamond enhanced silicon carbide substrate prepared in this example was about 86W/(m × k) and the coefficient of thermal expansion was 1.12 × 10-6/K。
Example 7
The preparation process of the diamond-reinforced silicon carbide substrate of the embodiment is specifically as follows:
(1) diamond, graphite, a dispersant (castor oil) and a solvent (ethanol/methyl ethyl ketone) were added to a teflon ball mill pot in a ratio of 50g, 12g, 3.3g and 21.7g, ball milled for 7 hours, and then 6.5g of a binder (PVB) and 6.5g of a plasticizer (dioctyl phthalate) were added thereto and ball milling was continued for 5 hours, to finally obtain a casting slurry having a viscosity of about 8340 mPaS.
(2) And (2) carrying out vacuum defoaming on the casting slurry prepared in the step (1) for 50min under a negative pressure environment of-90 KPa, and then filtering.
(3) And (3) carrying out tape casting molding on the tape casting slurry treated in the step (2) by using a tape casting machine, controlling the height of a scraper to be 1.3mm, controlling the tape casting speed to be 0.02m/min, and setting the temperatures of the first drying zone, the second drying zone and the third drying zone to be 40 ℃, 55 ℃ and 70 ℃ respectively to obtain a tape casting blank with the thickness of 0.50 mm. And cutting the casting blank after drying.
(4) And (3) degreasing the casting blank in an argon environment, wherein the degreasing temperature is set to 900 ℃, and the heat preservation time is 60 min. After the heat preservation is finished, the temperature is reduced to 100 ℃ at the speed of 2 ℃/min, and then the furnace is cooled.
(5) And (3) placing the degreased casting blank into a graphite box containing silicon powder, separating the casting blank from the silicon powder by using a graphite rod, and then placing the whole casting blank into a high-vacuum sintering furnace for vacuum gas phase infiltration. The infiltration temperature is 1650 ℃, the infiltration pressure is 15Pa, and the infiltration time is 1 h. The obtained density is about 3.06g/cm after furnace cooling3And the density is more than 94 percent.
The thermal conductivity of the diamond-enhanced silicon carbide substrate prepared in this example was about 109W/(m × k) and the coefficient of thermal expansion was 1.33 × 10-6/K。
Comparative example 1
The process for preparing the diamond enhanced silicon carbide substrate of comparative example 1 is specifically as follows:
(1) adding diamond, a dispersing agent (triethyl phosphate) and a solvent (ethanol and ethyl acetate azeotropic liquid) into a polytetrafluoroethylene ball milling tank according to the proportion of 50g, 3.3g and 21.7g, carrying out ball milling for 6h, adding 6.5g of a bonding agent (PVB) and 6.5g of a plasticizer (dioctyl phthalate) into the polytetrafluoroethylene ball milling tank, and continuing ball milling for 6h to obtain casting slurry with the viscosity of about 6500 mPas.
(2) And (2) carrying out vacuum defoaming on the casting slurry prepared in the step (1) for 30min under a negative pressure environment of-87.5 KPa, and then filtering.
(3) And (3) carrying out tape casting on the tape casting slurry treated in the step (2) by using a tape casting machine, controlling the height of a scraper to be 1.3mm, controlling the tape casting speed to be 0.02m/min, and setting the temperatures of the first drying zone, the second drying zone and the third drying zone to be 40 ℃, 55 ℃ and 70 ℃ respectively to obtain a tape casting blank with the thickness of 0.47 mm. And cutting the casting blank after drying.
(4) And (3) degreasing the casting blank in an argon environment, wherein the degreasing temperature is set to be 500 ℃, and the heat preservation time is 120 min. After the heat preservation is finished, the temperature is reduced to 100 ℃ at the speed of 2 ℃/min, and then the furnace is cooled.
(5) And (3) placing the degreased casting blank into a graphite box containing silicon powder, separating the casting blank from the silicon powder by using a graphite rod, and then placing the whole casting blank into a high-vacuum sintering furnace for vacuum gas phase infiltration. The infiltration temperature is 1575 ℃, the infiltration pressure is 2Pa, and the infiltration time is 3 h. The obtained density is about 2.94g/cm after furnace cooling3And the density of the diamond reinforced silicon carbide substrate is 97.3 percent.
The thermal conductivity of the diamond-reinforced silicon carbide substrate prepared in this comparative example was about 110W/(m × k), and the thermal expansion coefficient was 2.6 × 10-6/K。
Comparative example 2
The process for preparing the diamond enhanced silicon carbide substrate of comparative example 2 is specifically as follows:
(1) adding diamond, graphite, a dispersing agent (triethyl phosphate) and a solvent (ethanol and ethyl acetate azeotropic liquid) into a polytetrafluoroethylene ball milling tank according to the proportion of 50g, 5g, 3.3g and 21.7g, carrying out ball milling for 6 hours, adding 6.5g of a binding agent (PVB) and 6.5g of a plasticizer (dioctyl phthalate) into the ball milling tank, and continuing ball milling for 6 hours to obtain casting slurry with the viscosity of about 8000 mPaS.
(2) And (2) carrying out vacuum defoaming on the casting slurry prepared in the step (1) for 30min under a negative pressure environment of-87.5 KPa, and then filtering.
(3) And (3) carrying out tape casting on the tape casting slurry treated in the step (2) by using a tape casting machine, controlling the height of a scraper to be 1.3mm, controlling the tape casting speed to be 0.02m/min, and setting the temperatures of the first drying zone, the second drying zone and the third drying zone to be 40 ℃, 55 ℃ and 70 ℃ respectively to obtain a tape casting blank with the thickness of 0.47 mm. And cutting the casting blank after drying.
(4) And (3) degreasing the casting blank in an argon environment, wherein the degreasing temperature is set to be 500 ℃, and the heat preservation time is 120 min. After the heat preservation is finished, the temperature is reduced to 100 ℃ at the speed of 2 ℃/min, and then the furnace is cooled.
(5) And (3) performing chemical vapor infiltration on the degreased casting blank to obtain a SiC matrix, wherein Methyltrichlorosilane (MTS), hydrogen and argon are respectively used as a precursor, a carrier gas and a diluent gas in the CVI process. The deposition conditions are MTS/H21/10, Ar flow rate 350ml/min, deposition pressure 5KPa, deposition temperature 1000 deg.C and deposition time 80 h. The obtained density is about 2.94g/cm after furnace cooling3And the density of the diamond reinforced silicon carbide substrate is 87.66%.
The thermal conductivity of the diamond-reinforced silicon carbide substrate prepared in this comparative example was about 82W/(m × k), and the thermal expansion coefficient was 1.2 × 10-6/K。
It can be seen from the comparison between the above examples and comparative examples that, wet ball milling is performed on diamond and graphite to obtain casting slurry, then casting is performed to obtain a casting blank with controllable size and uniform porosity, finally silicon vapor permeates into the casting blank through silicon vapor infiltration, the silicon vapor permeated into the casting blank and graphite contained in the casting blank are subjected to silicon-carbon reaction to generate silicon carbide, and the casting blank is densified to obtain a dense diamond-reinforced silicon carbide substrate. Within a certain range, the density of the prepared diamond enhanced silicon carbide substrate can be improved by increasing the content of graphite; within a certain range, the density of the prepared diamond enhanced silicon carbide substrate can be improved by increasing the infiltration temperature.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A preparation method of a diamond-enhanced silicon carbide substrate is characterized by comprising the following steps:
carrying out wet ball milling on diamond, graphite, a dispersing agent, a binder, a plasticizer and a solvent to obtain casting slurry;
carrying out tape casting on the tape casting slurry to obtain a tape casting blank, wherein the thickness of the tape casting blank is 0.3-0.55 mm; and
and carrying out gas-phase infiltration on the casting blank and the silicon powder to obtain the diamond-enhanced silicon carbide substrate.
2. The method for preparing a diamond-enhanced silicon carbide substrate according to claim 1, wherein in the step of vapor infiltration of the casting blank and the silicon powder, the infiltration temperature is 1450 ℃ to 1650 ℃, and the infiltration time is 1h to 5 h.
3. The method of producing a diamond-enhanced silicon carbide substrate according to claim 1, wherein the mass ratio of the diamond to the graphite is 100: 10-100: 24.
4. the method for producing a diamond-enhanced silicon carbide substrate according to claim 1, wherein the dispersant is one selected from the group consisting of triethyl phosphate and castor oil; and/or the solvent is one of isopropanol/toluene, ethanol/methyl ethyl ketone, ethanol/ethyl acetate, trichloroethylene/methyl ethyl ketone and ethanol/water.
5. The method for preparing a diamond-enhanced silicon carbide substrate according to claim 1, wherein the step of wet ball milling the diamond, the graphite, the dispersant, the binder, the plasticizer and the solvent comprises: firstly, performing ball milling dispersion on the diamond, the graphite and the dispersing agent in the solvent for 5-7 h, then adding the binder and the plasticizer, and continuing ball milling for 5-7 h to obtain the casting slurry.
6. The method of producing a diamond-enhanced silicon carbide substrate according to claim 1, wherein the step of tape casting the tape-cast slurry further comprises: and (3) defoaming the casting slurry, wherein in the step of defoaming, the vacuum degree is-100 KPa to-87.5 KPa, and the defoaming time is 30min to 50 min.
7. The method of producing a diamond-enhanced silicon carbide substrate according to claim 1, wherein the step of vapor phase infiltration of the cast ingot with silicon powder is preceded by the step of: and carrying out degreasing treatment on the casting blank.
8. The method for producing a diamond-enhanced silicon carbide substrate according to claim 7, wherein the step of degreasing comprises: degreasing the casting blank at 300-900 ℃ for 1-3 h under the protective atmosphere, cooling to 100 ℃ at the speed of less than 5 ℃/min, and cooling along with the furnace.
9. A diamond-reinforced silicon carbide substrate produced by the method for producing a diamond-reinforced silicon carbide substrate according to any one of claims 1 to 8.
10. An electronic product, wherein a package substrate of the electronic product is the diamond-enhanced silicon carbide substrate according to claim 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010284460.7A CN111484330A (en) | 2020-04-13 | 2020-04-13 | Diamond-enhanced silicon carbide substrate, preparation method thereof and electronic product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010284460.7A CN111484330A (en) | 2020-04-13 | 2020-04-13 | Diamond-enhanced silicon carbide substrate, preparation method thereof and electronic product |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111484330A true CN111484330A (en) | 2020-08-04 |
Family
ID=71789765
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010284460.7A Pending CN111484330A (en) | 2020-04-13 | 2020-04-13 | Diamond-enhanced silicon carbide substrate, preparation method thereof and electronic product |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111484330A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112694335A (en) * | 2020-12-29 | 2021-04-23 | 北京科技大学广州新材料研究院 | Diamond-silicon carbide substrate and preparation method and application thereof |
| CN113307628A (en) * | 2021-01-28 | 2021-08-27 | 上海德宝密封件有限公司 | Silicon carbide-diamond complex phase ceramic grinding ring material and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102184873A (en) * | 2011-04-21 | 2011-09-14 | 北京科技大学 | Method for preparing diamond-silicon carbide electronic packaging material fast |
| CN103724014A (en) * | 2013-12-26 | 2014-04-16 | 西北工业大学 | Preparation method of diamond doped silicon carbide (SiC) ceramics with high heat conductivity |
| KR20160015851A (en) * | 2014-08-01 | 2016-02-15 | 주식회사 한국씨브이디다이아몬드공구 | The method of producing the diamond-SiC composite under low pressure |
| CN105347799A (en) * | 2015-11-30 | 2016-02-24 | 西北工业大学 | Preparation method of large-particle-diameter Diamond/SiC composite |
| CN107353007A (en) * | 2017-07-13 | 2017-11-17 | 华通信安(北京)科技发展有限公司 | A kind of diamond/silicon carbide composite and preparation method thereof |
| CN110698202A (en) * | 2019-11-08 | 2020-01-17 | 北京科技大学广州新材料研究院 | Diamond-silicon carbide composite material and preparation method and application thereof |
-
2020
- 2020-04-13 CN CN202010284460.7A patent/CN111484330A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102184873A (en) * | 2011-04-21 | 2011-09-14 | 北京科技大学 | Method for preparing diamond-silicon carbide electronic packaging material fast |
| CN103724014A (en) * | 2013-12-26 | 2014-04-16 | 西北工业大学 | Preparation method of diamond doped silicon carbide (SiC) ceramics with high heat conductivity |
| KR20160015851A (en) * | 2014-08-01 | 2016-02-15 | 주식회사 한국씨브이디다이아몬드공구 | The method of producing the diamond-SiC composite under low pressure |
| CN105347799A (en) * | 2015-11-30 | 2016-02-24 | 西北工业大学 | Preparation method of large-particle-diameter Diamond/SiC composite |
| CN107353007A (en) * | 2017-07-13 | 2017-11-17 | 华通信安(北京)科技发展有限公司 | A kind of diamond/silicon carbide composite and preparation method thereof |
| CN110698202A (en) * | 2019-11-08 | 2020-01-17 | 北京科技大学广州新材料研究院 | Diamond-silicon carbide composite material and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| WEI ZHENG，ET AL.: "Graphite addition for SiC formation in diamond/SiC/Si composite preparation", 《INTERNATIONAL JOURNAL OF MINERALS, METALLURGY AND MATERIALS》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112694335A (en) * | 2020-12-29 | 2021-04-23 | 北京科技大学广州新材料研究院 | Diamond-silicon carbide substrate and preparation method and application thereof |
| CN113307628A (en) * | 2021-01-28 | 2021-08-27 | 上海德宝密封件有限公司 | Silicon carbide-diamond complex phase ceramic grinding ring material and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109879669B (en) | High-entropy ceramic composite material with high strength and preparation method and application thereof | |
| CN110655407A (en) | Preparation method of silicon carbide ceramic with controllable resistance | |
| CN103724014B (en) | Preparation method of diamond doped silicon carbide (SiC) ceramics with high heat conductivity | |
| JPH02279575A (en) | Production of sintered ceramic body having dense ceramic film | |
| WO2022222778A1 (en) | Fine ceramic material formed by means of ceramic precursor framework and preparation method therefor and use thereof | |
| CN110407213B (en) | (Ta, nb, ti, V) C high-entropy carbide nano powder and preparation method thereof | |
| CN111925229A (en) | Method for preparing high-performance foamed ceramic by combining template method with chemical vapor infiltration method | |
| JP2015199657A (en) | Method for producing silicon nitride substrate | |
| CN111484330A (en) | Diamond-enhanced silicon carbide substrate, preparation method thereof and electronic product | |
| CN111320476A (en) | Diamond-silicon carbide composite material, preparation method thereof and electronic equipment | |
| CN114315394A (en) | By using Ti3SiC2Preparation method of three-dimensional network porous prefabricated body reinforced SiC ceramic matrix composite material | |
| CN115536403A (en) | High-toughness silicon nitride ceramic material and preparation method thereof | |
| JP3472585B2 (en) | Aluminum nitride sintered body | |
| KR20040002053A (en) | Microporous Ceramics materials and The producing method the same | |
| JP4641845B2 (en) | Coated porous structure and method for producing coated porous structure | |
| CN115594514B (en) | Three-dimensional SiC framework reinforced SiC high-density ceramic and preparation method thereof | |
| CN112694335B (en) | Diamond-silicon carbide substrate and preparation method and application thereof | |
| CN113061040B (en) | Preparation method of porous boron nitride ceramic | |
| CN111792944B (en) | Method for preparing foamed ceramic material by using foamed silica gel and inorganic powder compound as precursor | |
| CN111470866A (en) | Diamond-silicon carbide composite material, preparation method thereof and electronic equipment | |
| CN109608188B (en) | Anti-burning coking zirconium phosphate porous ceramic and preparation method thereof | |
| JP2001354479A (en) | Aluminum nitride sintered compact and its manufacturing method | |
| JP3297547B2 (en) | Method for producing silicon carbide sintered body | |
| CN113979765B (en) | Silicon carbide porous ceramic and preparation method thereof | |
| CN113735594B (en) | Method for preparing high-thermal-conductivity silicon nitride ceramic through hot-pressing sintering |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200804 |
|
| RJ01 | Rejection of invention patent application after publication |