CN115259889B - Porous silicon carbide ceramic, preparation method and application thereof, and aluminum silicon carbide composite material - Google Patents
Porous silicon carbide ceramic, preparation method and application thereof, and aluminum silicon carbide composite material Download PDFInfo
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- CN115259889B CN115259889B CN202210948103.5A CN202210948103A CN115259889B CN 115259889 B CN115259889 B CN 115259889B CN 202210948103 A CN202210948103 A CN 202210948103A CN 115259889 B CN115259889 B CN 115259889B
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 152
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 108
- 239000000919 ceramic Substances 0.000 title claims abstract description 105
- 229910021426 porous silicon Inorganic materials 0.000 title claims abstract description 63
- 239000002131 composite material Substances 0.000 title claims abstract description 38
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000002245 particle Substances 0.000 claims abstract description 31
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 24
- 238000005245 sintering Methods 0.000 claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000005469 granulation Methods 0.000 claims abstract description 15
- 230000003179 granulation Effects 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 15
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 15
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 11
- 235000015895 biscuits Nutrition 0.000 claims abstract description 11
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 11
- 238000003825 pressing Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000005303 weighing Methods 0.000 claims abstract description 5
- 125000003158 alcohol group Chemical group 0.000 claims abstract description 4
- 238000005452 bending Methods 0.000 claims description 13
- 239000011148 porous material Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 12
- 229910052782 aluminium Inorganic materials 0.000 claims description 11
- 229910052751 metal Inorganic materials 0.000 claims description 11
- 239000002184 metal Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- 239000011159 matrix material Substances 0.000 claims 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 6
- 238000004073 vulcanization Methods 0.000 abstract description 5
- 239000000843 powder Substances 0.000 description 17
- 230000000052 comparative effect Effects 0.000 description 11
- 229910004298 SiO 2 Inorganic materials 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000013329 compounding Methods 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 238000005538 encapsulation Methods 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 238000009715 pressure infiltration Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000001694 spray drying Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 239000002562 thickening agent Substances 0.000 description 2
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical class CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 241000863480 Vinca Species 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
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- 238000009826 distribution Methods 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000010808 liquid waste Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000007655 standard test method Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
- C04B38/0635—Compounding ingredients
- C04B38/0645—Burnable, meltable, sublimable materials
- C04B38/067—Macromolecular compounds
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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
- C04B35/565—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 based on silicon carbide
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
- C22C29/065—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds based on SiC
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- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
- C22C29/067—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds comprising a particular metallic binder
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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Abstract
The application provides a preparation method of porous silicon carbide ceramic, which comprises the following steps: (1) Weighing materials according to the following aggregate formula, wherein the aggregate formula comprises the following components by taking the mass of the aggregate as 100 percent: 95% -99.5% of silicon carbide; 0.5% -5% of silicon dioxide; (2) mixing and dispersing the weighed aggregate; (3) Putting the dispersed aggregate into a vulcanization granulation bed for granulation to obtain ceramic particles, wherein a forming agent is added according to 40% -60% of the total mass of the aggregate, and the forming agent is an alcohol solution of polyvinyl alcohol Ding Quanzhi; (4) pressing the ceramic particles into a ceramic preform biscuit; (5) Sintering the ceramic preform into a porous silicon carbide ceramic. According to the application, the silicon dioxide is added to effectively promote the adhesion between silicon carbide particles; through the control of the process and the formula, the silicon dioxide is concentrated at the bonding position among the silicon carbide particles, so that the heat conductivity of the aluminum silicon carbide composite material is effectively improved.
Description
Technical Field
The application relates to a porous silicon carbide ceramic, a preparation method and application thereof, and an aluminum silicon carbide composite material.
Background
With the development of power electronics and semiconductor technology, chips are being developed along the direction of high power and high frequency, the integration level of high power module chips is continuously improved, for example, the integration level of Insulated Gate Bipolar Transistor (IGBT) power modules is continuously improved, and the power is continuously increased, so that the working temperature of the high power module chips is continuously increased, and accordingly, the requirements on electronic packaging materials, particularly on heat dissipation substrates, are higher and higher, and the heat dissipation substrates are required to have lower thermal expansion coefficients matched with the chips, and are also required to have higher thermal conductivity. The aluminum silicon carbide (Al-SiC) composite material is widely applied to the encapsulation of high-power module chips as a novel electronic encapsulation material with high heat conduction and low expansion.
The aluminum silicon carbide composite material is mainly prepared from metal aluminum and porous silicon carbide (SiC) ceramic, wherein one of the keys affecting the performance of the aluminum silicon carbide composite material is the performance of the porous silicon carbide ceramic, the content of the silicon carbide ceramic directly determines the thermal conductivity and thermal expansion of the composite material, and when the content of the silicon carbide ceramic is higher, the thermal expansion of the composite material is lower, but the thermal conductivity of the composite material is also reduced. In order to solve the contradiction, the formula and sintering process of the porous silicon carbide ceramic are started, and the thermal expansion and heat conduction performance of the composite material are ensured.
At present, two main methods exist for preparing the porous silicon carbide ceramic, namely, sintering by adding a low-temperature adhesive and sintering by a high-temperature oxidation method. In practical studies, it has been found that both methods produce a relatively large amount of binder phase of low thermal conductivity on the silicon carbide ceramic surface during sintering. For example, when sintering is performed by oxidation, an oxide-silicon dioxide layer is formed on the surface of silicon carbide due to high temperature (higher than 1000 ℃), and when aluminum and silicon carbide are compounded in the later stage, the contact area between aluminum and silicon carbide is reduced due to the existence of the silicon dioxide layer, and the thermal expansion coefficient of silicon dioxide is far lower than that of silicon carbide, so that the existence of the silicon dioxide layer seriously affects the thermal conductivity of the later stage composite material.
Disclosure of Invention
The application aims to provide a preparation method of porous silicon carbide ceramic, and an aluminum silicon carbide composite material prepared from the porous silicon carbide ceramic has low expansion rate and high thermal conductivity.
In order to achieve the above purpose, the application adopts the following technical scheme:
the application provides a preparation method of porous silicon carbide ceramic, which comprises the following steps: (1) Weighing materials according to the following aggregate formula, wherein the aggregate formula comprises the following components in percentage by mass of 100 percent: 95% -99.5% of silicon carbide; 0.5% -5% of silicon dioxide; (2) mixing and dispersing the weighed aggregate; (3) Putting the dispersed aggregate into a vulcanization granulation bed for granulation to obtain ceramic particles, wherein a forming agent is added according to 40% -60% of the total mass of the aggregate, and the forming agent is an alcohol solution of polyvinyl alcohol Ding Quanzhi; (4) pressing the ceramic particles into a ceramic preform biscuit; (5) Sintering the ceramic preform into the porous silicon carbide ceramic.
Preferably, the formula of the aggregate comprises the following components in percentage by mass of 100 percent: 98% -99.2% of silicon carbide; 0.8% -2% of silicon dioxide.
Further preferably, the silicon carbide comprises, based on 100% by mass of the silicon carbide: 5% -15% of first silicon carbide, wherein the median diameter of the first silicon carbide is 1-10 mu m; 20% -35% of second silicon carbide, wherein the median diameter of the second silicon carbide is 25-35 mu m; 55% -65% of third silicon carbide, wherein the median diameter of the third silicon carbide is 70-90 mu m.
Preferably, the feeding amount of the forming agent is 45% -55% of the total mass of the aggregate.
Preferably, the alcohol comprises one or more of ethanol, methanol, ethylene glycol.
Further preferably, the mass concentration of the polyvinyl butyral ester in the alcohol solution is 10% -20%.
Preferably, the step of mixing and dispersing comprises the steps of dispersing by using a double vertical high-speed reamer, wherein the stirring speed of the high-speed reamer is 1500-2000 rpm, and the stirring speed of the low-speed reamer is 400-500 rpm; the dispersing time is 25-35 minutes.
Preferably, the step of pressing the ceramic particles into a ceramic preform biscuit comprises the step of paving the ceramic particles layer by layer, and dry-pressing the ceramic particles into the ceramic preform biscuit with the thickness of 10-100 mm under the pressure of 40-50 MPa.
Preferably, the sintering temperature is 850-900 ℃, and the sintering is performed in an atmospheric environment.
Further preferably, the sintering is performed according to a temperature increase profile including: a. the temperature is kept at room temperature to 300 ℃, the temperature rising rate is 3 to 10 ℃/min, and the temperature is kept for 1 to 3 hours; b. the temperature is 300-900 ℃, the heating rate is 3-10 ℃/min, and the temperature is kept for 1-3 h; c. naturally cooling to room temperature.
In a second aspect the present application provides a porous silicon carbide ceramic prepared according to the preparation method described above.
Preferably, the volume content of aggregate in the porous silicon carbide ceramic is 55% -65% in unit volume; the average pore diameter of the porous silicon carbide ceramic is 15-20 microns, and the bending strength is not lower than 10Mpa.
In a third aspect, the present application provides the use of a porous silicon carbide ceramic in the preparation of a metallic silicon carbide composite material, the porous silicon carbide ceramic being prepared according to the preparation method described above.
Preferably, the composite material comprises a metal silicon carbide composite material, the metal in the metal silicon carbide composite material comprising aluminum and/or copper.
In a fourth aspect, the present application provides an aluminum silicon carbide composite material prepared from aluminum and a porous silicon carbide ceramic prepared by the preparation method described above.
Preferably, the mass ratio of the aluminum in the aluminum silicon carbide composite material to the porous silicon carbide ceramic is 1: (1-2).
Preferably, the thermal conductivity of the aluminum silicon carbide composite material is 150-210W/(m.k), and the thermal expansion coefficient is (7.5-11) multiplied by 10 -6 K。
Due to the application of the technical scheme, compared with the prior art, the application has the following advantages:
according to the application, the silicon dioxide is added to effectively promote the adhesion between silicon carbide particles; further, through the control of the process and the formula, silicon dioxide is concentrated at the bonding position among silicon carbide particles, and the surface of the silicon carbide ceramic is almost free of a bonding phase-silicon dioxide layer with low heat conductivity, so that the contact area between aluminum and silicon carbide ceramic can be increased during the subsequent compounding of the aluminum and silicon carbide ceramic, the silicon dioxide layer at the two-phase interface is eliminated greatly, and the heat conductivity of the aluminum silicon carbide composite material is further improved effectively.
Detailed Description
The traditional oxidation process for preparing porous silicon carbide ceramics requires that silicon carbide powder is subjected to surface oxidation at high temperature (generally more than 1000 ℃), and the mode can generate a binding phase-silicon dioxide layer with low thermal conductivity on the surface of silicon carbide, so that the thermal conductivity of the subsequent aluminum silicon carbide composite material is seriously influenced. The inventors have unexpectedly found that by adding a certain amount of silica to the silicon carbide powder and by controlling the process and formulation, the silica can be concentrated at the bonding sites between the silicon carbide particles, avoiding the formation of a silica layer on the silicon carbide surface, and thus greatly improving the thermal conductivity of the aluminum silicon carbide composite material in the later stage.
The application provides a preparation method of porous silicon carbide ceramic, which comprises the following steps:
(1) Weighing materials according to the following aggregate formula, wherein the aggregate formula comprises the following components by taking the mass of the aggregate as 100 percent:
95% -99.5% of silicon carbide;
0.5% -5% of silicon dioxide;
(2) Mixing and dispersing the weighed aggregate;
(3) Putting the dispersed aggregate into a vulcanization granulation bed for granulation to obtain ceramic particles, wherein a forming agent is added according to 40% -60% of the total mass of the aggregate, and the forming agent is an alcohol solution of polyvinyl alcohol Ding Quanzhi;
(4) Pressing the ceramic particles into a ceramic preform biscuit;
(5) Sintering the ceramic preform into a porous silicon carbide ceramic.
According to the present application, the mass content of silica in the aggregate is preferably 0.8% to 5%, for example, 0.8%, 1.0%, 1.2%, 1.4%, 1.6%, 1.8%, 2.0%, 3.0%, 4.0%, etc. The particle size of the silica is preferably 0.3 to 5.0. Mu.m.
According to the present application, it comprises, based on 100% by mass of silicon carbide:
5% -15% of first silicon carbide, wherein the median diameter of the first silicon carbide is 1-10 mu m;
20% -35% of second silicon carbide, wherein the median diameter of the second silicon carbide is 25-35 mu m;
55% -65% of third silicon carbide, wherein the median diameter of the third silicon carbide is 70-90 mu m.
Further, it comprises, based on 100% by mass of silicon carbide:
8% -12% of first silicon carbide, wherein the median diameter of the first silicon carbide is 3-8 mu m;
25% -30% of second silicon carbide, wherein the median diameter of the second silicon carbide is 28-32 mu m;
58% -62% of third silicon carbide, wherein the median diameter of the third silicon carbide is 75-85 mu m.
According to the application, the amount of the molding agent added is preferably 45% -55% of the total mass of the aggregate, for example 45%, 47%, 50%, 52%, 55% and so on.
The scheme of the application has at least the following advantages:
(1) According to the application, a certain amount of silica micropowder is added into silicon carbide powder, and the micropowder is used as an adhesive, so that high-temperature sintering is not needed, and silicon carbide particles can be bonded together at a lower temperature (less than 1000 ℃); due to the reduction of the sintering temperature, a silicon dioxide layer is not generated on the surface of the silicon carbide (generally, when the temperature is 1350-1460 ℃, an obvious oxide layer is gradually formed on the surface of the silicon carbide particles along with the increase of the temperature), so that a low heat conductivity layer is not arranged between two phases when the silicon carbide particles are compounded with metal, and the heat conductivity of the composite material is greatly improved.
(2) Compared with manual granulation, the method has the advantages of higher efficiency and better uniformity; the efficiency is also higher compared to spray granulation, the equipment and personnel investment is low, the uniformity is also more uniform, and little solid waste and liquid waste are generated compared to spray granulation, and the environment is hardly affected.
(3) The present application uses an alcoholic solution of polyvinyl alcohol Ding Quanzhi as a forming agent, which is easier to granulate than a water-based forming agent (e.g., an aqueous solution of polyvinyl alcohol), and can further increase the efficiency of granulation.
(4) The aluminum silicon carbide composite material has both low expansion rate and high heat conductivity.
The application is further described below with reference to examples. The present application is not limited to the following examples. The implementation conditions adopted in the embodiments can be further adjusted according to different requirements of specific use, and the implementation conditions which are not noted are conventional conditions in the industry. The technical features of the various embodiments of the present application may be combined with each other as long as they do not collide with each other.
Unless otherwise specified, d50 refers to median or median particle diameter, specifically to the particle diameter corresponding to a cumulative particle size distribution percentage of one sample reaching 50%. .
The starting materials in the following examples and comparative examples are all commercially available, wherein:
polyvinyl butyral esters (PVB) were purchased from Isman (Eastman) under the designation B98;
polyvinyl alcohol (PVA) is purchased from vinca chemical industry under the trademark 2088.
Example 1
A preparation method of porous silicon carbide ceramic comprises the following steps:
(1) Weighing materials according to the following aggregate formula, wherein the aggregate formula is that the mass of the aggregate is 100 percent:
SiC（d50=5μm） 11%；
SiC（d50=30μm） 28%；
SiC（d50=80μm） 60%；
SiO 2 1% of powder (0.3-5.0 μm);
(2) Dispersing the aggregate by using a double vertical high-speed reamer, wherein the stirring speed of the high-speed reamer is 1500 rpm, and the stirring speed of the low-speed reamer is 500 rpm; the dispersion time was 30 minutes;
(3) Introducing the mixed materials in the step (2) into a vulcanization granulation bed, adding a forming agent which is a mixed solution of polyvinyl butyral Ding Quanzhi and ethanol according to 50% of the mass of aggregate, wherein the mass concentration of polyvinyl butyral in the mixed solution is 20%, and the rotating speed of a turntable of the vulcanization granulation bed is 1500-2000 rpm, so as to prepare ceramic particles with the diameter of 150-200 mu m;
(4) The ceramic particles are paved layer by layer and dry pressed into a ceramic preform biscuit with the thickness of 10mm under the pressure of 40 MPa;
(5) Sintering the ceramic preform biscuit in the atmospheric environment at the sintering temperature of 850-900 ℃, wherein the sintering curve is as follows:
a. the temperature is between room temperature and 300 ℃, the heating rate is 5 ℃/min, and the temperature is kept for 2 hours, and the stage is called a degumming stage;
b. and (3) heating at 300-900 ℃ at a speed of 5 ℃/min, preserving heat for 2 hours, and naturally cooling to room temperature to finally obtain the porous silicon carbide ceramic.
In this example, the powder yield of the porous silicon carbide ceramic was 95%, wherein the powder yield= [ (total mass of the produced porous silicon carbide ceramic×content of silicon carbide in the porous silicon carbide ceramic)/total charged mass of silicon carbide ] ×100%; the volume fraction is 65%, wherein the volume fraction refers to the volume ratio of aggregate in the porous silicon carbide ceramic per unit volume; the average pore diameter is 16 mu m; the flexural strength was 16MPa.
The porous silicon carbide ceramic prepared by the embodiment has good uniformity and small fluctuation of volume fraction, aperture and bending strength.
Example 2
This example differs from example 1 as follows:
(1) The material is changed according to the following aggregate formula, wherein the aggregate formula is that the mass of the aggregate is 100 percent:
SiC（d50=12μm） 11%；
SiC（d50=30μm） 28%；
SiC（d50=80μm） 60%；
SiO 2 1% of powder (0.3-5.0 μm);
in the embodiment, the powder yield of the porous silicon carbide ceramic is 95%, the volume fraction is 60%, and the average pore diameter is 18 mu m; the bending strength was 10MPa.
The porous silicon carbide ceramic prepared by the embodiment has good uniformity and small fluctuation of volume fraction, aperture and bending strength.
Example 3
This example differs from example 1 as follows:
(1) The material is changed according to the following aggregate formula, wherein the aggregate formula is that the mass of the aggregate is 100 percent:
SiC（d50=5μm） 11.2%；
SiC（d50=30μm） 28%；
SiC（d50=80μm） 60%；
SiO 2 0.8% of powder (0.3-5.0 μm).
In the embodiment, the powder yield of the porous silicon carbide ceramic is 95%, the volume fraction is 65%, and the average pore diameter is 16 mu m; the flexural strength was 8MPa.
The porous silicon carbide ceramic prepared by the embodiment has good uniformity and small fluctuation of volume fraction, aperture and bending strength.
Example 4
This example differs from example 1 as follows:
(1) The material is changed according to the following aggregate formula, wherein the aggregate formula is that the mass of the aggregate is 100 percent:
SiC（d50=5μm） 10%；
SiC（d50=30μm） 28%；
SiC（d50=80μm） 60%；
SiO 2 powder (0.3-5.0 μm) 2%.
In the embodiment, the powder yield of the porous silicon carbide ceramic is 95%, the volume fraction is 65%, and the average pore diameter is 16 mu m; the flexural strength was 17MPa.
The porous silicon carbide ceramic prepared by the embodiment has good uniformity and small fluctuation of volume fraction, aperture and bending strength.
Example 5
This example differs from example 1 as follows:
(3) And adding a forming agent according to 40% of the aggregate mass.
In the embodiment, the ceramic particles prepared in the step (3) contain more powder, the materials do not form ceramic particles completely, the powder yield of the porous silicon carbide ceramic is 80%, the body is 65%, and the average pore diameter is 16 mu m; the flexural strength was 16MPa.
The porous silicon carbide ceramic prepared by the embodiment has good uniformity and small fluctuation of volume fraction, aperture and bending strength.
Example 6
This example differs from example 1 as follows:
(3) And adding the forming agent according to 60% of the aggregate mass.
In the embodiment, obvious particle growth and agglomeration phenomena occur in the step (3), the powder yield of the porous silicon carbide ceramic is 75%, the body is 62%, and the average pore diameter is 16 mu m; the flexural strength was 16MPa.
The porous silicon carbide ceramic prepared by the embodiment has good uniformity and small fluctuation of volume fraction, aperture and bending strength.
Comparative example 1
The difference between this comparative example and example 1 is as follows:
(1) The material is changed according to the following aggregate formula, wherein the aggregate formula is that the mass of the aggregate is 100 percent:
SiC（d50=5μm） 10.20%；
SiC（d50=30μm） 28.58%；
SiC（d50=80μm） 61.22%；
(5) Sintering the ceramic preform biscuit in an atmospheric environment at 1350 ℃, wherein the sintering curve is as follows:
a. the temperature is between room temperature and 300 ℃, the heating rate is 5 ℃/min, and the temperature is kept for 2 hours, and the stage is called a degumming stage;
b. and (3) heating at a temperature rising rate of 3 ℃/min at 300-1350 ℃, preserving heat for 3 hours, and naturally cooling to room temperature to finally obtain the porous silicon carbide ceramic.
In the comparative example, the body of the porous silicon carbide ceramic is divided into 62 percent, and the average pore diameter is 16-20 mu m; the bending strength is 15-17 mpa.
Comparative example 2
The difference between this comparative example and example 1 is as follows:
(2) Adding a forming agent (carboxymethyl cellulose), a dispersing agent (Nantong Tatai chemical HT A30) and water according to 50% of the mass of aggregate, and stirring for 2h in a vertical stirrer, wherein the forming agent is a mixed solution of polyvinyl alcohol and water, and the mass concentration of the polyvinyl alcohol in the mixed solution is 30%; the feeding amount of the thickener, the dispersing agent and the water is controlled so that the mass concentration of the polyvinyl alcohol in the system is 1%, the mass concentration of the thickener is 0.3% and the mass concentration of the dispersing agent is 0.4%;
(3) And (3) introducing the mixed materials in the step (2) into spray drying equipment, and performing spray drying granulation.
In the comparative example, the powder yield of the porous silicon carbide ceramic is 75%, the volume fraction is 62%, and the average pore diameter is 16 mu m; the flexural strength was 16MPa.
The porous silicon carbide ceramics prepared in this comparative example were poor in uniformity and large in fluctuation of volume fraction, pore diameter and bending strength.
Comparative example 3
(1) The material is changed according to the following aggregate formula, wherein the aggregate formula is that the mass of the aggregate is 100 percent:
SiC（d50=5μm） 11.5%；
SiC（d50=30μm） 28%；
SiC（d50=80μm） 60%；
SiO 2 0.5% of powder (0.3-5.0 μm).
In the embodiment, the powder yield of the porous silicon carbide ceramic is 95%, the volume fraction is 65%, and the average pore diameter is 16Mpa; the bending strength is lower than 3Mpa.
Comparative example 4
This example differs from example 1 as follows:
(1) The material is changed according to the following aggregate formula, wherein the aggregate formula is that the mass of the aggregate is 100 percent:
SiC（d50=5μm） 6%；
SiC（d50=30μm） 28%；
SiC（d50=80μm） 60%；
SiO 2 6% of powder (0.3-5.0 μm).
In the embodiment, the powder yield of the porous silicon carbide ceramic is 95%, the volume fraction is 16%, and the average pore diameter is 16 mu m; the bending strength was 20MPa.
Application verification
The porous silicon carbide ceramics in the above comparative examples and examples were mixed with aluminum metal in a ratio of 2:1, and preparing an aluminum silicon carbide composite material by compounding, wherein the compounding process is a reverse vacuum pressure infiltration process, and the specific reference can be made to the literature: preparation of high volume fraction SiC by vacuum variable pressure infiltration method p The application is not particularly limited by the Al composite, chinese nonferrous metals journal, vol.16, no. 9, stages 1551-1557, and the properties of the aluminum silicon carbide composite are shown in Table 1.
TABLE 1
The standard on which the thermal conductivity test method is based is the standard test method for measuring thermal diffusivity by a flash method according to ASTM E1461; the national standard on which the thermal expansion rate test method is based is a GB/T16535-1996 engineering ceramic linear thermal expansion coefficient test method.
The present application has been described in detail with the purpose of enabling those skilled in the art to understand the contents of the present application and to implement the same, but not to limit the scope of the present application, and all equivalent changes or modifications made according to the spirit of the present application should be included in the scope of the present application.
Claims (11)
1. A preparation method of porous silicon carbide ceramic is characterized in that: the preparation method comprises the following steps:
(1) Weighing materials according to the following aggregate formula, wherein the aggregate formula comprises the following components in percentage by mass of 100 percent:
95% -99% of silicon carbide;
1% -5% of silicon dioxide;
the silicon carbide comprises, based on 100% of the silicon carbide mass:
5% -15% of first silicon carbide, wherein the median diameter of the first silicon carbide is 1-10 mu m;
20% -35% of second silicon carbide, wherein the median diameter of the second silicon carbide is 25-35 mu m;
55% -65% of third silicon carbide, wherein the median diameter of the third silicon carbide is 70-90 mu m;
(2) Mixing and dispersing the weighed aggregate;
(3) Putting the dispersed aggregate into a fluidized granulation bed for granulation to obtain ceramic particles, wherein a forming agent is added according to 40% -60% of the total mass of the aggregate, and the forming agent is an alcohol solution of polyvinyl alcohol Ding Quanzhi;
(4) Pressing the ceramic particles into a ceramic preform biscuit;
(5) Sintering the ceramic preform into the porous silicon carbide ceramic, and performing the sintering in an atmospheric environment according to a temperature rise curve comprising:
a. the temperature is kept at room temperature to 300 ℃, the temperature rising rate is 3 to 10 ℃/min, and the temperature is kept for 1 to 3 hours;
b. the temperature is 300-900 ℃, the heating rate is 3-10 ℃/min, and the temperature is kept for 1-3 h;
c. naturally cooling to room temperature.
2. The method for preparing porous silicon carbide ceramic according to claim 1, wherein: the formula of the aggregate comprises the following components by mass of 100 percent:
98% -99% of silicon carbide;
1% -2% of silicon dioxide.
3. The method for preparing porous silicon carbide ceramic according to claim 1, wherein: the feeding amount of the forming agent is 45% -55% of the total mass of the aggregate.
4. The method for preparing porous silicon carbide ceramic according to claim 1, wherein: the alcohol is one or more of ethanol, methanol and glycol; and/or the number of the groups of groups,
the mass concentration of the polyvinyl butyral ester in the alcohol solution is 10% -20%.
5. The method for preparing porous silicon carbide ceramic according to claim 1, wherein: the steps of mixing and dispersing comprise dispersing by using a double vertical high-speed reamer, wherein the stirring speed of the high-speed reamer is 1500-2000 rpm, and the stirring speed of the low-speed reamer is 400-500 rpm; the dispersing time is 25-35 minutes; and/or the number of the groups of groups,
the step of pressing the ceramic particles into ceramic preform biscuit comprises the steps of laying the ceramic particles layer by layer and dry pressing the ceramic particles into ceramic preform biscuit with the thickness of 10-100 mm under the pressure of 40-50 MPa.
6. A porous silicon carbide ceramic, characterized by: the porous silicon carbide ceramic is produced according to the production method as claimed in any one of claims 1 to 5.
7. The porous silicon carbide ceramic according to claim 6, wherein: the volume content of aggregate in the porous silicon carbide ceramic is 55% -65% in unit volume; the average pore diameter of the porous silicon carbide ceramic is 15-20 microns, and the bending strength is not lower than 10Mpa.
8. The application of porous silicon carbide ceramic in preparing metal silicon carbide composite material is characterized in that: the porous silicon carbide ceramic is produced according to the production method as claimed in any one of claims 1 to 5.
9. The use of the porous silicon carbide ceramic according to claim 8 for the preparation of a metal silicon carbide composite material, wherein: the composite material comprises a metal matrix ceramic composite material, wherein the metal in the metal matrix ceramic composite material comprises aluminum and/or copper.
10. An aluminum silicon carbide composite material, characterized in that: the aluminum silicon carbide composite material is prepared from aluminum and the porous silicon carbide ceramic prepared by the preparation method according to any one of claims 1 to 5.
11. An aluminum silicon carbide composite material according to claim 10 wherein: the feeding volume ratio of aluminum to porous silicon carbide ceramic in the aluminum silicon carbide composite material is 1: (1-2); and/or the number of the groups of groups,
the thermal conductivity of the aluminum silicon carbide composite material is 150-210W/(m.k), and the thermal expansion coefficient is 7.5-11 multiplied by 10 -6 K。
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| CN103288420A (en) * | 2013-05-16 | 2013-09-11 | 陕西科技大学 | Method for preparing fracturing propping agent special for shale gas from fly ash |
| CN106463484A (en) * | 2014-03-18 | 2017-02-22 | 电化株式会社 | Aluminium-silicon carbide composite, and power-module base plate |
| CN111138198A (en) * | 2019-12-30 | 2020-05-12 | 珠海凯利得新材料有限公司 | Preparation method and application of aluminum silicon carbide composite material |
| CN112552052A (en) * | 2020-12-22 | 2021-03-26 | 珠海亿特立新材料有限公司 | Microwave-assisted silicon carbide porous ceramic, aluminum silicon carbide composite preparation method and aluminum silicon carbide composite |
| JP2021176813A (en) * | 2020-05-08 | 2021-11-11 | 武漢工程大学Wuhan Institute of Technology | Method for preparing porous silicon carbide ceramic carrier |
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| CN106463484A (en) * | 2014-03-18 | 2017-02-22 | 电化株式会社 | Aluminium-silicon carbide composite, and power-module base plate |
| CN111138198A (en) * | 2019-12-30 | 2020-05-12 | 珠海凯利得新材料有限公司 | Preparation method and application of aluminum silicon carbide composite material |
| JP2021176813A (en) * | 2020-05-08 | 2021-11-11 | 武漢工程大学Wuhan Institute of Technology | Method for preparing porous silicon carbide ceramic carrier |
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