CN115894037B - Al (aluminum) alloy 4 SiC 4 Porous ceramic combined with silicon carbide and preparation method thereof - Google Patents
Al (aluminum) alloy 4 SiC 4 Porous ceramic combined with silicon carbide and preparation method thereof Download PDFInfo
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 106
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 86
- 239000000919 ceramic Substances 0.000 title claims abstract description 65
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 229910003923 SiC 4 Inorganic materials 0.000 title claims description 53
- 229910052782 aluminium Inorganic materials 0.000 title claims description 20
- 229910045601 alloy Inorganic materials 0.000 title claims description 6
- 239000000956 alloy Substances 0.000 title claims description 6
- 238000002156 mixing Methods 0.000 claims abstract description 120
- 239000000463 material Substances 0.000 claims abstract description 82
- 239000000843 powder Substances 0.000 claims abstract description 39
- 229910052751 metal Inorganic materials 0.000 claims abstract description 38
- 239000002184 metal Substances 0.000 claims abstract description 38
- 239000006229 carbon black Substances 0.000 claims abstract description 35
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 31
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000005011 phenolic resin Substances 0.000 claims abstract description 31
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 31
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 28
- 239000000126 substance Substances 0.000 claims abstract description 27
- 239000007788 liquid Substances 0.000 claims abstract description 26
- 238000010438 heat treatment Methods 0.000 claims abstract description 25
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 22
- 239000004850 liquid epoxy resins (LERs) Substances 0.000 claims abstract description 20
- 238000003825 pressing Methods 0.000 claims abstract description 8
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 26
- 239000002245 particle Substances 0.000 claims description 23
- 239000011148 porous material Substances 0.000 claims description 23
- 229910002804 graphite Inorganic materials 0.000 claims description 11
- 239000010439 graphite Substances 0.000 claims description 11
- 238000013001 point bending Methods 0.000 claims description 10
- 238000000465 moulding Methods 0.000 claims description 2
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 abstract description 19
- 239000000758 substrate Substances 0.000 abstract description 18
- 238000000034 method Methods 0.000 abstract description 15
- 230000008569 process Effects 0.000 abstract description 7
- 239000004576 sand Substances 0.000 abstract description 7
- 230000008595 infiltration Effects 0.000 abstract description 4
- 238000001764 infiltration Methods 0.000 abstract description 4
- 239000012071 phase Substances 0.000 description 24
- 229910052799 carbon Inorganic materials 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 11
- 229910052710 silicon Inorganic materials 0.000 description 9
- 239000010703 silicon Substances 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000007789 gas Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000006276 transfer reaction Methods 0.000 description 5
- 238000005336 cracking Methods 0.000 description 4
- 238000011065 in-situ storage Methods 0.000 description 4
- CAVCGVPGBKGDTG-UHFFFAOYSA-N alumanylidynemethyl(alumanylidynemethylalumanylidenemethylidene)alumane Chemical compound [Al]#C[Al]=C=[Al]C#[Al] CAVCGVPGBKGDTG-UHFFFAOYSA-N 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 229910021392 nanocarbon Inorganic materials 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 229910021418 black silicon Inorganic materials 0.000 description 2
- 239000007767 bonding agent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- SBEQWOXEGHQIMW-UHFFFAOYSA-N silicon Chemical compound [Si].[Si] SBEQWOXEGHQIMW-UHFFFAOYSA-N 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 229910000676 Si alloy Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- -1 aluminum-silicon-carbon atoms Chemical group 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 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
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000009715 pressure infiltration Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
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Abstract
The invention discloses an Al4SiC 4-bonded silicon carbide porous ceramic and a preparation method thereof, wherein metal aluminum powder, simple substance silicon powder, liquid phenolic resin and carbon black powder are subjected to first proportioning and mixing to obtain a material W1; taking silicon carbide powder and liquid epoxy resin for secondary proportioning and mixing to obtain a material W2; carrying out third proportioning and mixing on the material W1 and the material W2 to obtain a material W3; the material W3 and the pore-forming agent are subjected to fourth proportioning and mixing to obtain a material W4, wherein the pore-forming agent accounts for 0-20% of the mass of the material W3; and then pressing and forming the material W4 to obtain a product, and placing the product in an argon atmosphere, and carrying out sectional heat treatment to obtain the Al4SiC 4-bonded silicon carbide porous ceramic. Solves the technical problems of low heat conductivity coefficient, sand holes on the surface and failure of silicon carbide powder bonding phase in the infiltration process of the oxide bonding silicon carbide porous ceramic for the existing aluminum silicon carbide substrate.
Description
Technical Field
The invention belongs to the technical field of inorganic nonmetallic materials, and in particular relates to an Al 4 SiC 4 Porous ceramics combined with silicon carbide and a preparation method thereof.
Background
The aluminum silicon carbide substrate is a metal-non-oxide composite material with low density, adjustable thermal expansion coefficient and high thermal conductivity, and is used for solving the problem of thermal failure of chips, transistors or semiconductors and the like caused by high integration of electronic circuits. At the end of the 80 s of the 20 th century, the aluminum silicon carbide substrate is firstly applied to a package shell of a gallium arsenide millimeter wave/microwave integrated circuit receiving/transmitting component of an airborne active phased array radar by the U.S. military, so that the performance of the MMIC T/R component is improved, the cost is reduced, and the weight is reduced. Through development and research in nearly thirty years, aluminum silicon carbide substrates are widely used as substrates for power modules, heat sinks for power amplifiers, covers for microprocessors, heat-dissipating plates, air-cooled and liquid-cooled cooling plate carriers, package substrates, and the like, in addition to being applied to MMIC T/R component package housings. The preparation process of the aluminum silicon carbide substrate mainly comprises the steps of preparing silicon carbide porous ceramics, impregnating the silicon carbide porous ceramics with molten metal aluminum or aluminum alloy liquid and electroplating metal.
Silicon carbide porous ceramic preparation is a key factor affecting the performance of aluminum silicon carbide substrates. Besides being influenced by the morphology and the components of the powder, the granularity of the silicon carbide powder, the heat treatment atmosphere and the bonding agent among the powder are main factors for restricting the performance of the silicon carbide porous ceramic.
At present, oxide-bonded silicon carbide porous ceramics for aluminum silicon carbide substrates are easy to generate defects in the preparation process:
1) The fluctuation range of the grain diameter of the silicon carbide powder is large (10-80 mu m), and the pore diameter is unevenly distributed;
2) The heat treatment atmosphere is an oxidizing atmosphere, silicon dioxide is easy to generate on the surface of silicon carbide, so that the heat transfer path is increased, and the heat conductivity coefficient is reduced;
3) The bonding phase between the silicon carbide powder is oxide bonding (B 2 O 3 -Al 2 O 3 -SiO 2 System or its extension system), is susceptible to chemical reaction with silicon carbide at high temperature to form CO or CO 2 Gas, which causes sand holes during chemical plating.
Disclosure of Invention
The technical problem to be solved by the invention is to provide an Al for overcoming the defects in the prior art 4 SiC 4 The combined silicon carbide porous ceramic and the preparation method thereof are used for solving the technical problems that the oxide combined silicon carbide porous ceramic for the existing aluminum silicon carbide substrate has low heat conductivity coefficient, sand holes exist on the surface and the combined phase of silicon carbide powder fails in the infiltration process.
The invention adopts the following technical scheme:
al (aluminum) alloy 4 SiC 4 The preparation method of the combined silicon carbide porous ceramic comprises the following steps:
s1, carrying out first proportioning and mixing on metal aluminum powder, simple substance silicon powder, liquid phenolic resin and carbon black powder to obtain a material W1;
s2, taking silicon carbide powder and liquid epoxy resin for secondary proportioning and mixing to obtain a material W2;
s3, mixing and blending the material W1 obtained in the step S1 and the material W2 obtained in the step S2 for the third time to obtain a material W3;
s4, proportioning and mixing the material W3 obtained in the step S3 and a pore-forming agent for the fourth time, wherein the pore-forming agent accounts for 0-20wt% of the mass of the material W3, and a material W4 is obtained;
s5, pressing and molding the material W4 obtained in the step S4 under the pressure of 5-30 MPa to obtain a product;
s6, placing the product obtained in the step S5 in an argon atmosphere, and performing sectional heat treatment to obtain Al 4 SiC 4 Bonded silicon carbidePorous ceramics.
Specifically, in step S1, aluminum powder is used as the metal powder: elemental silicon powder: the mass ratio of the liquid phenolic resin to the carbon black powder is 27:7:12, the carbon black powder accounts for 6 to 8 percent of the total mass of the liquid phenolic resin and the carbon black powder, and the particle size of the metal aluminum powder is 15 mu m<D 50 <30 μm, the grain diameter of the simple substance silicon powder is 5 μm<D 50 <10 μm, the particle diameter of the carbon black powder is 50nm<D 50 <100nm。
Specifically, in the step S1, the mixing temperature is 30-40 ℃, and the mixing time is 10-15 min.
Specifically, in step S2, silicon carbide powder: the mass ratio of the liquid epoxy resin is 100: (5-10), the particle size of the silicon carbide powder is as follows: 50 μm<D 90 <70μm，30μm<D 50 <50μm，20μm<D 10 <30μm。
Specifically, in the step S2, the mixing temperature is 30-40 ℃, and the mixing time is 3-5 min.
Specifically, in step S3, the mass ratio of the material W1 to the material W2 is: (15-30): (70-85).
7. Al according to claim 1 4 SiC 4 The preparation method of the combined silicon carbide porous ceramic is characterized in that in the step S3, the mixing temperature is 30-40 ℃ and the mixing time is 10-15 min.
Specifically, in step S4, the pore-forming agent is spherical graphite, and the particle size of the pore-forming agent is 40 μm<D 90 <60μm，30μm<D 50 <40μm，25μm<D 10 <30 mu m, the mixing temperature is 30-40 ℃, and the mixing time is 10-15 min.
Specifically, in step S6, the sectional heat treatment specifically includes:
treating at 0-300 deg.c for 60-100 min; treating at 300-600 deg.c for 120-240 min; treating at 600-600 deg.c for 240-360 min; treating at 600-1000 deg.c for 100-240 min; treating at 1000-1000 deg.c for 180-360 min; treating at 1000-1200 deg.c for 120-180 min; treating at 1200-1200 deg.c for 180-360 min; treating at 1200-1700/1750 deg.c for 240-480 min; treating at 1700/1750-1700/1750 deg.c for 180-480 min.
In another technical scheme of the present invention, the method comprises the following steps,al (aluminum) alloy 4 SiC 4 The combined silicon carbide porous ceramic comprises silicon carbide powder and Al 4 SiC 4 The silicon carbide powder comprises the following components in percentage by mass: al (Al) 4 SiC 4 The mass percentage is (70-85): (15-30), wherein the porosity of the porous ceramic is 45-75%, the pore diameters of the pores are intensively distributed at 30-50 mu m, and the three-point bending strength is more than 5MPa.
Compared with the prior art, the invention has at least the following beneficial effects:
the invention relates to Al 4 SiC 4 By combining the preparation method of the silicon carbide porous ceramic, the full wrapping contact of carbon black powder and phenolic resin pyrolysis carbon on metal aluminum and elemental silicon is realized through the adhesive action of the liquid phenolic resin and the in-situ pyrolysis high-activity carbon effect of the phenolic resin, the reactivity of the carbon material is improved, and the mass transfer distance of aluminum-silicon-carbon atoms is shortened; through premixing of the epoxy resin and the silicon carbide particles, the agglomeration phenomenon of the W1 powder in the mixing process of the step S3 is avoided, and the adhesion effect of the W1 powder on the surfaces of the W2 particles is promoted; the pore diameter and the porosity of the prepared porous ceramic are adjustable by adding a pore-forming agent with proper granularity; the characteristics of the phenolic resin in-situ cracking activated carbon, the aluminum carbide generation reaction characteristic, the silicon carbide generation reaction characteristic and the Al are fully utilized by the gradual heating and sectional heat preservation process 4 SiC 4 Reaction characteristics and Al 4 SiC 4 With the sintering characteristic of silicon carbide particles, successfully realizes the requirement of Al for aluminum silicon carbide production 4 SiC 4 And (3) preparing the combined silicon carbide porous ceramic.
Further, the content of the carbon black powder is strictly controlled, so that the phenomenon that the mixing bonding agglomeration effect is caused by excessive action of a bonding agent during mixing of the phenolic resin material W1 is avoided; the particle sizes of the metal aluminum, the simple substance silicon and the carbon black are strictly limited, and the gradient reaction characteristics of the nano carbon, the metal aluminum and the simple substance silicon are utilized to realize the stepwise formation of the aluminum carbide and the silicon carbide in the heating process, so that the gas phase metal aluminum is avoided.
Furthermore, the viscosity of the liquid phenolic resin is optimally in the range of 30-40 ℃ and can meet the requirements of mixing and cracking carbon in 10-15 min.
Furthermore, the proportion of the epoxy resin is strictly limited based on the condition that the thin coating on the surface of the silicon carbide particles is satisfied, so that excessive addition and increase of cracking carbon are avoided; based on the skeleton effect of the silicon carbide particles, the size of the silicon carbide particles is strictly limited, and the stability of pore diameter and porosity formed by stacking the silicon carbide particles is fully exerted.
Furthermore, the mixing requirement of the silicon carbide particles can be met within 3-5 min by utilizing the optimal viscosity of the liquid phenolic resin within the range of 30-40 ℃, so that the excessive mixing time is avoided, and the production cost is increased.
Further, the mass ratio of the material W1 to the material W2 is strictly limited, so that the reduction of porosity and the reduction of pore diameter caused by excessive content of a bonding phase are avoided; the problem that the strength of the porous ceramic cannot meet the production process requirement of aluminum silicon carbide due to the fact that the content of the bonding phase is too low is avoided.
Furthermore, the mixing requirement of the materials W1 and W2 can be met within 10-15 min by utilizing the optimal viscosity of the liquid phenolic resin within the range of 30-40 ℃, so that the excessive mixing time is avoided, and the production cost is increased.
Further, the mixing requirements of the materials W1, W2 and W2 are met, the excessive mixing time is avoided, and the production cost is increased.
Further, the pore-forming agent is strictly limited to have a size close to that of the silicon carbide particles, so that the characteristics of stable increase of porosity and stable pore size distribution after the pore-forming agent replaces the silicon carbide particles are ensured.
In conclusion, the method successfully prepares the Al with the porosity of 30-80 percent, the pore diameter of the air holes being intensively distributed at 10-50 mu m and the three-point bending strength of more than 5MPa 4 SiC 4 The silicon carbide porous ceramic is combined, so that the technical problems that the existing oxide-combined silicon carbide porous ceramic for the aluminum silicon carbide substrate has low heat conductivity coefficient, sand holes exist on the surface and the silicon carbide powder combined phase fails in the infiltration process are solved.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
FIG. 1 is Al 4 SiC 4 Typical junction of bonded silicon carbide porous ceramicsPatterning;
FIG. 2 is a drawing of the inter-particle bonding phase Al of silicon carbide 4 SiC 4 Is a typical block diagram of (2);
FIG. 3 shows the formation of a combined phase Al for the material W1 4 SiC 4 Is a typical powder diffraction pattern of (2);
FIG. 4 is Al 4 SiC 4 A typical pore size distribution schematic diagram of a bonded silicon carbide porous ceramic;
FIG. 5 is a metallographic view of an aluminum silicon carbide substrate prepared by the method of the present invention, wherein (a) is before improvement and (b) is after improvement.
Detailed Description
The following description of the present invention will be made clearly and fully, and it is apparent that the embodiments described are some, but not all, of the embodiments of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the present invention, all embodiments and preferred methods of implementation mentioned herein may be combined with each other to form new solutions, unless otherwise specified.
In the present invention, all technical features mentioned herein and preferred features may be combined with each other to form new technical solutions, unless otherwise specified.
In the present invention, the percentage (%) or parts refer to weight percentage or parts by weight relative to the composition unless otherwise specified.
In the present invention, the components or preferred components thereof may be combined with each other to form a new technical solution, unless otherwise specified.
In the present invention, unless otherwise indicated, the numerical ranges "a-b" represent shorthand representations of any combination of real numbers between a and b, where a and b are both real numbers. For example, the numerical range "6-22" means that all real numbers between "6-22" have been listed throughout, and "6-22" is only a shorthand representation of a combination of these values.
The "range" disclosed herein may take the form of a lower limit and an upper limit, which may be one or more lower limits and one or more upper limits, respectively.
In the present invention, the term "and/or" as used herein refers to any and all possible combinations of one or more of the associated listed items, and includes such combinations.
In the present invention, each reaction or operation step may be performed sequentially or sequentially unless otherwise indicated. Preferably, the reaction processes herein are performed sequentially.
Unless otherwise defined, the technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. In addition, any method or material similar or equivalent to those described may be used in the present invention.
Referring to FIGS. 1 and 2, the present invention provides an Al 4 SiC 4 The combined silicon carbide porous ceramic comprises a ceramic phase framework and a combined phase, wherein the ceramic phase framework comprises the following components in percentage by mass: the mass ratio of the binding phase is (70-85): (15-30), wherein the ceramic phase framework is silicon carbide powder, and the bonding phase is Al 4 SiC 4 The method comprises the steps of carrying out a first treatment on the surface of the The porosity of the porous ceramic is 45-75%, the pore diameter of the porous ceramic is concentrated and distributed at 30-50 mu m, and the three-point bending strength is more than 5MPa.
Referring to fig. 3 and 4, the data of porosity, pore size distribution and three-point bending strength are obtained according to the methods of ceramic body apparent porosity, bulk density test (QB/T1642-2012), porous ceramic pore diameter test (GB/T1967-1996) and stress strain test (GB/T38978-2020), respectively.
The porous ceramic also comprises a pore-forming agent, wherein the pore-forming agent accounts for 0-20% of the mass of the ceramic phase framework and the bonding phase, namely the pore-forming agent: the mass percentage of the (silicon carbide powder plus the binding phase) is equal to 0-20%.
The invention relates to Al 4 SiC 4 The preparation method of the combined silicon carbide porous ceramic comprises the following steps:
s1, taking a proper amount of metal aluminum powder, simple substance silicon powder, liquid phenolic resin and carbon black powder according to the mass ratio w (Al):w(Si)：w(C 1 +C 2 ) =27: 7:12 (carbon black powder C) 1 +C 2 Mixing the materials in a first proportion of 6-8% of the total mass, and uniformly mixing to obtain a material W1;
the mass percent of the aluminum powder (Al) is more than or equal to 99 percent, the mass percent of the elemental silicon powder (Si) is more than or equal to 99 percent, and the liquid phenolic resin (C) 1 ) The mass percentage of the carbon black powder is more than or equal to 50 percent and the carbon black powder (C) 2 ) The mass percentage of (2) is more than or equal to 99 percent; the grain diameter of the metal aluminum powder is 15 mu m<D 50 <30 μm, the grain diameter of the simple substance silicon powder is 5 μm<D 50 <10 μm, the particle diameter of the carbon black powder is 50nm<D 50 <100nm, the mixing temperature is 30-40 ℃, and the mixing time is 10-15 min.
S2, taking silicon carbide powder and liquid epoxy resin, wherein the mass ratio of the silicon carbide powder to the liquid epoxy resin is 100: (5-10) carrying out secondary proportioning and mixing, and obtaining a material W2 after uniform mixing;
the silicon carbide powder is black silicon carbide or green silicon carbide, and the mass percentage of the black silicon carbide (SiC) is more than or equal to 95%; the mass percentage of the green silicon carbide (SiC) is more than or equal to 97 percent, and the particle size of the silicon carbide powder meets the following conditions: 50 μm<D 90 <70μm，30μm<D 50 <50μm，20μm<D 10 <30μm。
Wherein the mass percentage of the liquid epoxy resin (C) is less than 10 percent, the mixing temperature is 30-40 ℃, and the mixing time is 3-5 min.
S3, taking the material W1 obtained in the step S1 and the material W2 obtained in the step S2 according to the mass ratio (15-30): (70-85) carrying out third proportioning and mixing, and obtaining a material W3 after mixing uniformly;
wherein the mixing temperature is 30-40 ℃, and the mixing time is 10-15 min.
S4, proportioning and mixing the material W3 obtained in the step S3 and the pore-forming agent for the fourth time, and obtaining a material W4 after uniform mixing;
wherein, the pore-forming agent accounts for 0 to 20 percent of the mass of the material W3, the pore-forming agent is spherical graphite, and the particle diameter of the pore-forming agent is 40 mu m<D 90 <60μm，30μm<D 50 <40μm，25μm<D 10 <30 mu m, the mixing temperature is 30-40 ℃, and the mixing time is 10-15 min.
S5, placing the material W4 obtained in the step S4 into a machine pressing die, and forming a product with a required size under the pressure of 5-30 MPa;
s6, placing the product obtained in the step S5 in an argon atmosphere, and performing sectional heat treatment in an electric furnace to obtain Al 4 SiC 4 And silicon carbide porous ceramics are combined.
The sectional heat treatment is specifically as follows:
treating at 0-300 deg.c for 60-100 min;
treating at 300-600 deg.c for 120-240 min;
treating at 600-600 deg.c for 240-360 min;
treating at 600-1000 deg.c for 100-240 min;
treating at 1000-1000 deg.c for 180-360 min;
treating at 1000-1200 deg.c for 120-180 min;
treating at 1200-1200 deg.c for 180-360 min;
treating at 1200-1700/1750 deg.c for 240-480 min;
treating at 1700/1750-1700/1750 deg.c for 180-480 min.
Heat-treating phenolic resin at a low temperature (600-600 ℃); the phenolic resin is subjected to cracking reaction during low-temperature heat treatment to form high-activity nano carbon; the high-activity nano carbon wraps the silicon carbide powder, the metal aluminum powder and the simple substance silicon powder, shortens the reaction distance of the carbon-metal aluminum-simple substance silicon-silicon carbide powder, and activates the mobility of lattice atoms in the carbon-metal aluminum-simple substance silicon-silicon carbide powder.
Medium temperature heat treatment (1000-1000 ℃) of metal aluminum; the metal aluminum liquid phase mass transfer reaction is utilized to avoid the metal aluminum gas phase mass transfer reaction. During low-temperature heat treatment, a carbon-coated core-shell structure is formed on the surface of the metal aluminum, the shell breaking temperature is about 1000 ℃, and the gas phase mass transfer reaction is more remarkable at about 1100 ℃. The heat treatment at 1000-1000 ℃ can fully lead the liquid phase metal aluminum to react with the carbonaceous material to form aluminum carbide, and avoid aluminum element loss and sand hole formation caused by metal aluminum gas phase mass transfer.
Medium temperature heat treatment (1200-1200 ℃) of simple substance silicon; liquid phase mass transfer reaction for forming aluminum-silicon alloy by utilizing metal aluminum and elemental silicon, so that the elemental silicon is prevented from being at melting point temperature (1410℃)The gas phase mass transfer reaction. The metal aluminum can effectively promote the in-situ reaction of the simple substance silicon and the carbonaceous material to form Al at the temperature lower than 1200 DEG C 4 SiC 4 。
Al formed by in-situ reaction of high-temperature heat treatment (1700/1750-1700/1750 ℃) 4 SiC 4 The method comprises the steps of carrying out a first treatment on the surface of the Heat preservation at 1700 or 1750 ℃ to ensure that Al 4 SiC 4 The mutual diffusion of Al, si and C atoms at the interface of the silicon carbide powder is fully generated, and the Al is endowed with 4 SiC 4 Bonding strength of bonded silicon carbide porous ceramics.
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention. The components of the embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the invention, as presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
This example provides an Al for an aluminum silicon carbide substrate 4 SiC 4 The preparation method of the porous ceramic combined with silicon carbide comprises the following components in percentage by mass: 80.00wt% of silicon carbide powder, 10.8wt% of metal aluminum powder, 2.8wt% of simple substance silicon powder, 3.2wt% of carbon black powder, 3.2wt% of liquid phenolic resin, and 0wt% of pore-forming agent and 2wt% of liquid epoxy resin.
Wherein the pore-forming agent is spherical graphite with the granularity of D 90 ＝55μm，D 50 ＝35μm，D 10 =26 μm; the granularity of the silicon carbide powder is D 90 ＝70μm，D 50 ＝45μm，D 10 =28 μm; the granularity of the metal aluminum powder is D 50 =20 μm; simple substance silicon powderThe granularity of the powder is D 50 =8μm; the granularity of the carbon black powder is D 50 =90 nm; residual carbon ratio w (C) =50% of the liquid phenolic resin; the carbon residue ratio w (C) =5% of the liquid epoxy resin.
The preparation method comprises the following specific steps:
(1) Taking metal aluminum powder, simple substance silicon powder, liquid phenolic resin and carbon black powder according to the mass ratio w (Al): w (Si): w (C) 1 +C 2 ) =27: 7:12 (carbon black accounts for 8% of the total mass of C1+C2) and is subjected to primary proportioning and mixing, and a material W1 is obtained after uniform mixing, wherein the mixing temperature is 30 ℃, and the mixing time is 10min;
(2) Taking silicon carbide powder and liquid epoxy resin according to the mass ratio of 100:5, carrying out secondary proportioning and mixing, and obtaining a material W2 after uniform mixing, wherein the mixing temperature is 30 ℃ and the mixing time is 5min;
(3) Taking materials W1 and W2 according to a mass ratio of 15:85, mixing and evenly mixing to obtain a material W3, wherein the mixing temperature is 30 ℃, and the mixing time is 10min;
(4) Mixing the material W3 and spherical graphite accounting for 2wt% of the material W3 for the fourth time, and uniformly mixing to obtain a material W4, wherein the mixing temperature is 30 ℃, and the mixing time is 10min;
(5) Placing a proper amount of material W4 into a machine pressing die, and forming a product with a required size under the pressure of 20 MPa;
(6) Taking the product in the step S5, and placing the product in an electric furnace under argon atmosphere for sectional heat treatment to obtain Al 4 SiC 4 And silicon carbide porous ceramics are combined.
The sectional heat treatment is specifically as follows: treating at 0-300 deg.c for 60min; treating at 300-600 deg.c for 120min; treating at 600-600 deg.c for 240min; treating at 600-1000 deg.c for 100min; treating at 1000-1000 deg.c for 180min; treating at 1000-1200 deg.c for 120min; treating at 1200-1200 deg.c for 180min; treating at 1200-1750 ℃ for 240min; treating at 1750-1750 deg.c for 180min.
Al obtained by the preparation 4 SiC 4 The porosity of the porous ceramic combined with silicon carbide is 45%, the pore diameter of the pores is concentrated and distributed at 30-40 mu m, and the three-point bending strength is more than or equal to 12MPa.
Example 2
This example provides an Al for an aluminum silicon carbide substrate 4 SiC 4 The preparation method of the porous ceramic combined with silicon carbide comprises the following components in percentage by mass: 80 weight percent of silicon carbide powder, 10.8 weight percent of metal aluminum powder, 2.8 weight percent of simple substance silicon powder, 3.2 weight percent of carbon black powder, 3.2 weight percent of liquid phenolic resin, 4 weight percent of pore-forming agent and 2 weight percent of liquid epoxy resin.
Wherein the pore-forming agent is spherical graphite with the granularity of D 90 ＝55μm，D 50 ＝35μm，D 10 =26 μm; the granularity of the silicon carbide powder is D 90 ＝50μm，D 50 ＝35μm，D 10 =20 μm; the granularity of the metal aluminum powder is D 50 =15 μm; the granularity of the simple substance silicon powder is D 50 =6μm; the granularity of the carbon black powder is D 50 =80 nm; residual carbon ratio w (C) =50% of the liquid phenolic resin; the residual carbon ratio w (C) =5% of the liquid epoxy resin.
The preparation method comprises the following specific steps:
(1) Taking metal aluminum powder, simple substance silicon powder, liquid phenolic resin and carbon black powder according to the mass ratio w (Al): w (Si): w (C) 1 +C 2 ) =27: 7:12 (carbon black accounts for 8% of the total mass of C1+C2) and is subjected to primary proportioning and mixing, and a material W1 is obtained after uniform mixing, wherein the mixing temperature is 40 ℃, and the mixing time is 10min;
(2) Taking silicon carbide powder and liquid epoxy resin according to the mass ratio of 100:8, carrying out secondary proportioning and mixing, and obtaining a material W2 after uniform mixing, wherein the mixing temperature is 40 ℃ and the mixing time is 5min;
(3) Taking materials W1 and W2 according to the mass ratio of 16:84, carrying out third proportioning and mixing, and obtaining a material W3 after mixing uniformly, wherein the mixing temperature is 40 ℃ and the mixing time is 10min;
(4) Mixing the material W3 and spherical graphite accounting for 4wt% of the material W3 for the fourth time, and uniformly mixing to obtain a material W4, wherein the mixing temperature is 40 ℃, and the mixing time is 10min;
(5) Placing a proper amount of material W4 into a machine pressing die, and forming a product with a required size under the pressure of 10 MPa;
(6) Placing the product obtained in the step S5 under argon atmospherePerforming sectional heat treatment in an electric furnace to obtain Al 4 SiC 4 And silicon carbide porous ceramics are combined.
The sectional heat treatment is specifically as follows: treating at 0-300 deg.c for 60min; treating at 300-600 deg.c for 120min; treating at 600-600 deg.c for 240min; treating at 600-1000 deg.c for 240min; treating at 1000-1000 deg.c for 180min; treating at 1000-1200 deg.c for 120min; treating at 1200-1200 deg.c for 240min; treating at 1200-1750 ℃ for 240min; treating at 1750-1750 deg.c for 480min.
The Al obtained 4 SiC 4 The porosity of the porous ceramic combined with silicon carbide is 50%, the pore diameter of the pores is concentrated and distributed at 30-45 mu m, and the three-point bending strength is more than 9MPa.
Example 3
This example provides an Al for an aluminum silicon carbide substrate 4 SiC 4 The preparation method of the porous ceramic combined with silicon carbide comprises the following components in percentage by mass: 80 weight percent of silicon carbide powder, 10.8 weight percent of metal aluminum powder, 2.8 weight percent of simple substance silicon powder, 2.4 weight percent of carbon black powder and 4.0 weight percent of liquid phenolic resin; 6wt% of pore-forming agent and 2wt% of liquid epoxy resin are added.
Wherein the pore-forming agent is spherical graphite with the granularity of D 90 ＝50μm，D 50 ＝36μm，D 10 =27 μm; the granularity of the silicon carbide powder is D 90 ＝55μm，D 50 ＝35μm，D 10 =20 μm; the granularity of the metal aluminum powder is D 50 =15 μm; the granularity of the simple substance silicon powder is D 50 =6μm; the granularity of the carbon black powder is D 50 =80 nm; residual carbon ratio w (C) =60% of the liquid phenolic resin; the residual carbon ratio w (C) =5% of the liquid epoxy resin.
The preparation method comprises the following specific steps:
(1) Taking metal aluminum powder, simple substance silicon powder, liquid phenolic resin and carbon black powder according to the mass ratio w (Al): w (Si): w (C) 1 +C 2 ) =27: 7:12 (carbon black accounts for 6% of the total mass of C1+C2) and is subjected to primary proportioning and mixing, and a material W1 is obtained after uniform mixing, wherein the mixing temperature is 35 ℃, and the mixing time is 10min;
(2) Taking silicon carbide powder and liquid epoxy resin according to the mass ratio of 100:10, carrying out secondary proportioning and mixing, and obtaining a material W2 after uniform mixing, wherein the mixing temperature is 35 ℃ and the mixing time is 5min;
(3) Taking materials W1 and W2 according to the mass ratio of 16:84, carrying out third proportioning and mixing, and obtaining a material W3 after mixing uniformly, wherein the mixing temperature is 35 ℃ and the mixing time is 10min;
(4) Mixing and blending the material W3 and spherical graphite accounting for 6% of the mass of the material W3 for the fourth time, wherein the material W4 is obtained after uniform mixing, and the mixing temperature is 35 ℃ and the mixing time is 10min;
(5) Placing a proper amount of material W4 into a machine pressing die, and forming a product with a required size under the pressure of 10 MPa;
(6) Taking the product in the step S5, and placing the product in an electric furnace under argon atmosphere for sectional heat treatment to obtain Al 4 SiC 4 And silicon carbide porous ceramics are combined.
The sectional heat treatment is specifically as follows: treating at 0-300 deg.c for 60min; treating at 300-600 deg.c for 120min; treating at 600-600 deg.c for 210min; treating at 600-1000 deg.c for 240min; treating at 1000-1000 deg.c for 180min; treating at 1000-1200 deg.c for 120min; treating at 1200-1200 deg.c for 210min; treating at 1200-1750 ℃ for 240min; treating at 1750-1750 deg.c for 180min.
The Al obtained 4 SiC 4 The porosity of the combined silicon carbide porous ceramic is 55%, the pore diameter of the pores is concentrated and distributed at 30-50 mu m, and the three-point bending strength is high>7.5MPa。
Example 4
This example provides an Al for an aluminum silicon carbide substrate 4 SiC 4 The preparation method of the porous ceramic combined with silicon carbide comprises the following components in percentage by mass: 80 weight percent of silicon carbide powder, 10.8 weight percent of metal aluminum powder, 2.8 weight percent of simple substance silicon powder, 2.4 weight percent of carbon black powder and 4.0 weight percent of liquid phenolic resin; 20wt% of pore-forming agent and 2wt% of liquid epoxy resin are added.
Wherein the pore-forming agent is spherical graphite with the granularity of D 90 ＝50μm，D 50 ＝36μm，D 10 =27 μm; the granularity of the silicon carbide powder is D 90 ＝55μm，D 50 ＝35μm，D 10 =20 μm; the granularity of the metal aluminum powder is D 50 =15 μm; the granularity of the simple substance silicon powder is D 50 =6μm; the granularity of the carbon black powder is D 50 =80 nm; residual carbon ratio w (C) =60% of the liquid phenolic resin; the residual carbon ratio w (C) =5% of the liquid epoxy resin.
The preparation method comprises the following specific steps:
(1) Taking metal aluminum powder, simple substance silicon powder, liquid phenolic resin and carbon black powder according to the mass ratio w (Al): w (Si): w (C) 1 +C 2 ) =27: 7:12 (carbon black accounts for 6% of the total mass of C1+C2) and is subjected to primary proportioning and mixing, and a material W1 is obtained after uniform mixing, wherein the mixing temperature is 35 ℃, and the mixing time is 10min;
(2) Taking silicon carbide powder and liquid epoxy resin according to the mass ratio of 100:8, carrying out secondary proportioning and mixing, and obtaining a material W2 after uniform mixing, wherein the mixing temperature is 35 ℃ and the mixing time is 5min;
(3) Taking materials W1 and W2, wherein the mass ratio of the materials W1 to W2 is 15:85, mixing and evenly mixing to obtain a material W3, wherein the mixing temperature is 35 ℃, and the mixing time is 10min;
(4) Mixing and kneading the material W3 and spherical graphite accounting for 20% of the mass of the material W3 for the fourth time, wherein the material W4 is obtained after uniform mixing, and the mixing temperature is 35 ℃ and the mixing time is 10min;
(5) Placing the material W3 into a machine pressing die, and forming a product with the required size under the pressure of 10 MPa;
(6) Taking the product in the step S4, and placing the product in an electric furnace under argon atmosphere for sectional heat treatment to obtain Al 4 SiC 4 And silicon carbide porous ceramics are combined.
The sectional heat treatment is specifically as follows: treating at 0-300 deg.c for 100min; treating at 300-600 deg.c for 240min; treating at 600-600 deg.c for 360min; treating at 600-1000 deg.c for 240min; treating at 1000-1000 deg.c for 360min; treating at 1000-1200 deg.c for 180min; treating at 1200-1200 deg.c for 360min; treating at 1200-1750 deg.c for 480min.
The Al obtained 4 SiC 4 The porosity of the porous ceramic combined with silicon carbide is 75%, the pore diameter of the pores is concentrated and distributed at 30-50 mu m, and the three-point bending strength is more than 5MPa.
Referring to FIG. 5, FIG. 5a shows the absence of Al 4 SiC 4 The combined phase silicon carbide porous ceramic is shown in FIG. 5b as Al 4 SiC 4 And the same low-pressure infiltration process is adopted for combining the silicon carbide porous ceramics to obtain the metallographic structure diagram of the aluminum silicon carbide substrate. The comparative observation found that the holes of figure 5b were significantly reduced and reduced in size. Further evidence of the presence of Al 4 SiC 4 The silicon carbide porous ceramic of the bonding phase can effectively inhibit the generation and extension of sand holes.
In conclusion, the invention relates to Al 4 SiC 4 The combined silicon carbide porous ceramic and the preparation method thereof successfully prepare the Al with the porosity of 45-75 percent, the pore diameter of the air holes being intensively distributed at 30-50 mu m and the three-point bending strength of more than 5MPa 4 SiC 4 The silicon carbide porous ceramic is combined, so that the technical problems that the existing oxide-combined silicon carbide porous ceramic for the aluminum silicon carbide substrate has low heat conductivity coefficient, sand holes exist on the surface and the silicon carbide powder combined phase fails in the infiltration process are solved.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (5)
1. Al (aluminum) alloy 4 SiC 4 The preparation method of the combined silicon carbide porous ceramic is characterized by comprising the following steps of:
s1, carrying out first proportioning and mixing on metal aluminum powder, simple substance silicon powder, liquid phenolic resin and carbon black powder to obtain a material W1, wherein the metal aluminum powder is prepared by the following steps of: elemental silicon powder: the mass ratio of the liquid phenolic resin to the carbon black powder is 27:7:12, the carbon black powder accounts for 6% -8% of the total mass of the liquid phenolic resin and the carbon black powder, and the particle size of the metal aluminum powder is 15 mu m<D 50 <30 μm, the grain diameter of the simple substance silicon powder is 5 μm<D 50 <10 μm, the particle diameter of the carbon black powder is 50nm<D 50 <100nm；
S2, taking silicon carbide powder and liquid epoxy resin for secondary proportioning and mixing to obtain a material W2, wherein the silicon carbide powder is prepared by the following steps: the mass ratio of the liquid epoxy resin is 100: (5-10), wherein the particle size of the silicon carbide powder meets the following conditions: 50 μm<D 90 <70μm，30μm<D 50 <50μm，20μm<D 10 <30μm；
S3, mixing and proportioning the material W1 obtained in the step S1 and the material W2 obtained in the step S2 for the third time to obtain a material W3, wherein the mass ratio of the material W1 to the material W2 is as follows: (15-30): (70-85);
s4, carrying out fourth proportioning and mixing on the material W3 obtained in the step S3 and a pore-forming agent, wherein the pore-forming agent accounts for 2wt% -20 wt% of the mass of the material W3, so as to obtain a material W4, the pore-forming agent is spherical graphite, and the particle size of the pore-forming agent is 40 mu m<D 90 <60μm，30μm<D 50 <40μm，25μm<D 10 <30 mu m, the mixing temperature is 30-40 ℃, and the mixing time is 10-15 min;
s5, pressing and molding the material W4 obtained in the step S4 under the pressure of 5-30 MPa to obtain a product;
s6, placing the product obtained in the step S5 in an argon atmosphere, and performing sectional heat treatment to obtain Al 4 SiC 4 The sectional heat treatment is specifically carried out by combining silicon carbide porous ceramics:
treating at 0-300 ℃ for 60-100 min; treating for 120-240 min at 300-600 ℃; treating at 600-600 ℃ for 240-360 min; treating at 600-1000 ℃ for 100-240 min; treating at 1000-1000 ℃ for 180-360 min; treating for 120-180 min at 1000-1200 ℃; treating at 1200-1200 ℃ for 180-360 min; treating 240-480 min at 1200-1700 or 1200-1750 ℃; treating at 1700-1700 ℃ or 1750-1750 ℃ for 180-480 min.
2. Al according to claim 1 4 SiC 4 The preparation method of the combined silicon carbide porous ceramic is characterized in that in the step S1, the mixing temperature is 30-40 ℃, and the mixing time is 10-15 min.
3. Al according to claim 1 4 SiC 4 The preparation method of the combined silicon carbide porous ceramic is characterized in that in the step S2,the mixing temperature is 30-40 ℃, and the mixing time is 3-5 min.
4. Al according to claim 1 4 SiC 4 The preparation method of the combined silicon carbide porous ceramic is characterized in that in the step S3, the mixing temperature is 30-40 ℃ and the mixing time is 10-15 min.
5. Al (aluminum) alloy 4 SiC 4 Porous ceramic in combination with silicon carbide, characterized by the fact that Al according to any one of claims 1 to 4 4 SiC 4 The porous ceramic is prepared by combining silicon carbide porous ceramic preparation method, and comprises silicon carbide powder and Al 4 SiC 4 The silicon carbide powder comprises the following components in percentage by mass: al (Al) 4 SiC 4 The mass percentage of (70-85): (15-30), wherein the porosity of the porous ceramic is 45-75%, the pore diameters of the pores are intensively distributed at 30-50 mu m, and the three-point bending strength is more than 5MPa.
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