CN103276277B - Preparation method and device of high-volume fraction and high-intensity aluminum silicon carbide composite material - Google Patents

Preparation method and device of high-volume fraction and high-intensity aluminum silicon carbide composite material Download PDF

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CN103276277B
CN103276277B CN201310185323.8A CN201310185323A CN103276277B CN 103276277 B CN103276277 B CN 103276277B CN 201310185323 A CN201310185323 A CN 201310185323A CN 103276277 B CN103276277 B CN 103276277B
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silicon carbide
mould
heat
transfer device
composite material
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CN103276277A (en
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崔葵馨
金胜明
杜吉喜
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Changsha Aisike New Material Science & Technology Co Ltd
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Changsha Aisike New Material Science & Technology Co Ltd
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Abstract

The invention discloses a preparation method and device of a high-volume fraction and high-intensity aluminum silicon carbide composite material. A silicon carbide porous preformed blank with the porosity of 20%-80% is degassed in vacuum in a mold with an insulation device, then melt aluminum liquid permeates into pores of the silicon carbide porous preformed blank under the co-action of a capillary force, an external pressure and a solidification contraction force, and then heat in the melt aluminum liquid is quickly conducted out by using a directional heat conduction technique so that the melt aluminum liquid is solidified along a direction opposite to the heat conduction direction; the melt aluminum liquid forms a great number of microcrystal in the micro-pores, and a stretch prestress is generated on the surface of a SiC frame after the melt aluminum liquid is solidified completely, and thus the mechanical properties, density and thermo-physical properties of the material are greatly improved; the method is simple in technique; and the prepared material has high density, good mechanical properties, high heat conductivity, low thermal expansion coefficient and good dimensional stability.

Description

A kind of preparation method of high-volume fractional high strength aluminum silicon carbide composite material and device
Technical field
The invention belongs to metal-base composites forming technique category, specifically provide and a kind ofly prepare high-volume fractional, the method for high strength aluminum silicon carbide composite material and device.
Background technology
Aluminum silicon carbide composite material is widely used in structure and material and the electronic package material of aerospace, special equipment, precision instrument etc. due to its density is little, thermal conductivity is high, thermal expansivity is adjustable, specific rigidity is high, specific modulus is high and good stability of the dimension etc. is excellent heat physical properties and mechanical mechanics property.20% is usually less than at present as silicon carbide volume fraction in the aluminum silicon carbide composite material of structured material use, powder metallurgic method and stirring casting method is adopted to be prepared from, material compactness prepared by these two kinds of methods is not good enough, thermal conductivity is low, thermal expansivity is high, still can not reach the requirement of the special dimension such as aerospace and precision instrument to structured material completely.The research of high-volume fractional aluminum silicon carbide composite material mainly lays particular emphasis on its heat physical properties, for Electronic Packaging, its preparation method is pressure-free impregnation method and vacuum pressure infiltration method mainly, by shaping silicon carbide porous biscuits of traditional ceramics preparation method such as compression molding, injection molding or injection formings, biscuit carries out pressure-free impregnation or vacuum pressure infiltration aluminium liquid after sintering in heat treatment furnace, obtains high-volume fractional aluminum silicon carbide composite material after furnace cooling.Due to silicon carbide and molten aluminium nonwetting, pressure-free impregnation legal system for time need add silicon addition, Mg etc. to improve its wettability, and mold temperature is high, soaking time is long, the aluminium silicon carbide material interalloy coarse grains of preparation, have shrinkage cavity, pore, impurity and high temperature time easily produce Al 4c 3brittlement phase, thus the mechanical property and the heat physical properties that greatly reduce material; Comparatively speaking, the mold temperature of vacuum pressure infiltration method is lower, avoid a large amount of generations of brittlement phase, the heat physical properties of product is better, but adopt this legal system to be cool (as schematic diagram 1) by four circumferential centers for the cooling direction of molten aluminum liquid in silicon carbide precast billet hole of aluminium silicon carbide, speed of cooling is uncontrollable, and the alloy grain of generation is uneven, and aluminium liquid solidifies the stress producing remaining stochastic distribution completely at material internal; And because peripheral aluminium liquid preferentially solidifies in process of cooling, center is in liquid state, the contraction produced during the cooling of center molten aluminium, the combination of aluminium and SiC skeleton is deteriorated, and produces pore, causes the mechanical property of matrix material and heat physical properties to decline.This technique is difficult to soak into when infiltrating large size SiC sheet material, and heat physical properties, the mechanical property of product do not reach perfect condition.
Summary of the invention
The object of the invention is to the deficiency overcoming prior art existence, there is provided a kind of and adopt vacuum pressure aluminising-directed heat conduction crystallite curing technology, preparation has method and the corollary apparatus thereof of the large size aluminum silicon carbide composite material of high-volume fractional, high compactness, high heat conductance and high strength, the method avoids pressure-free impregnation method and vacuum pressure infiltration method preparation technology furnace cooling process interalloy grain-size is uncontrollable, crystal grain skewness, there is the shortcomings such as pore in material internal, thus improves mechanical mechanics property and the heat physical properties of aluminum silicon carbide composite material.
In order to realize above-mentioned technical purpose, technical scheme of the present invention is, a kind of preparation method of high-volume fractional high strength aluminum silicon carbide composite material, first the silicon carbide porous precast billet of porosity 20-80% is assemblied in mould, molten metal aluminium liquid or alloy aluminum liquid is filled after high-temperature degassing, then cooling curing is carried out and the demoulding, the outer wall of mould wraps up thermal insulation layer, and use heat-transfer device to carry out directed quick conductive to molten metal aluminium liquid or alloy aluminum liquid in mould outer wall being enclosed with thermal insulation layer to solidify when cooling curing, heat conduction place that molten metal aluminium liquid or alloy aluminum liquid are contacted with heat-transfer device is solidified gradually for solidifying starting point.
The heat conduction place cooling rate that heat-transfer device contacts 200 DEG C/min ~ 900 DEG C/min, the cooling rate at thermal insulation layer parcel place is no more than 100 DEG C/min.
The process of assembling precast billet and filling aluminum liquid is as follows:
A) the silicon carbide porous precast billet of porosity 20-80% is carried out surface treatment, be placed in mould, then mould is fixed in vacuum pressure aluminizing furnace, be warming up to 600-800 DEG C of insulation 2-6 hour;
B) by the porous SiC precast billet of above-mentioned isothermal holding, degassed under vacuum conditions, degassing temperature 500-800 DEG C, degassing time 0.1-2 hour; Degassing pressure 0.01-100Pa in stove;
C) molten metal aluminium liquid or alloy aluminum liquid is made fully to penetrate among the hole of silicon carbide porous precast billet by impressed pressure, capillary pressure and the acting in conjunction of cooling meat power, infiltrate in the process of porous SiC at molten aluminium or alloy aluminum melt, whole system continues at 600-800 DEG C of temperature, to keep 0.1-15 minute to ensure to be full of molten aluminium or alloy aluminum melt in micropore.
The direction of solidifying of molten metal aluminium liquid or alloy aluminum liquid is solidified by heat-transfer device contact position, and rapid solidification direction is contrary with direction of heat flow, and in the inner micritization of SiC precast billet micropore, produce stretching prestress.
Quick conductive device comprises gas conduction as air, nitrogen, argon gas, carbonic acid gas etc., liquid thermal conductivity as water, thermal oil, paraffinic hydrocarbon, alcohols etc., heat conduction with phase change, the modes such as heat pipe for thermal conductivity and semi-conductor heat conduction.
Cooling direction controlling can control according to product design, and regular square structure is from end face or side cooling, and cylindrical structural cools from end face, and tubular structure radially cools from tube hub, and hollow hemisphere structure radially cools inside ball.
A kind of preparation facilities of high-volume fractional high strength aluminum silicon carbide composite material, comprise the mould for holding silicon carbide porous precast billet, described outer mold wall is enclosed with thermal insulation layer, also comprise the heat-transfer device for directed cooling molten metal aluminium liquid or alloy aluminum liquid, described heat-transfer device is arranged in mould or is close to outer mold wall.
Described mould is cubes, and mould each outer wall is enclosed with thermal insulation layer, and the wherein outer wall that described heat-transfer device is close to mould is arranged.
Described mould is tubular body arranged inside, and mold cylinder outer wall is enclosed with thermal insulation layer, and heat-transfer device penetrates and arranges to mold axis position.
Described mould is Loadings On Hemispherical Shell, and mould housing outer side wall is enclosed with thermal insulation layer, and heat-transfer device is close to case inside wall and is arranged.
The present invention passes through vacuum outgas in the silicon carbide porous precast billet with porosity 20-80%, molten aluminum liquid is filled in constant temperature and pressure aluminising, form external phase, utilize the directed heat conduction of heat pipe to cool fast simultaneously, molten aluminium or alloy aluminum melt form crystallite to the cooling of insulation end fast from heat conduction end, thus make metallic aluminium be distributed in SiC micropore with microlitic structure, and in whole material internal directional retraction, stretching prestress is formed on silicon carbide skeleton surface, reduce material internal Residual Porosity, improve the compactness of aluminum silicon carbide composite material, mechanical mechanics property and heat physical properties (as schematic diagram 2), its progress is significantly: adopt directed quick conductive technology to make metallic aluminium melt or alloy aluminum melt form crystallite in SiC micropore, reduce matrix material residual porosity rate, improve the bonding strength of aluminium crystallite and SiC skeleton, stretching prestress is formed on SiC skeleton surface after molten aluminium or alloy aluminum melt solidifying complete, directed heat conduction technology can prepare sheet material, bar, the AlSiC matrix material of tubing and hollow hemisphere structure.This technology can prepare the aluminum silicon carbide composite material that silicon carbide volume fraction is high, density is high, physical strength is high, heat physical properties is excellent.
The present invention compared with prior art, has following advantage:
A. the directed quick conductive technology of heat pipe is adopted to replace traditional furnace cooling after porous SiC precast billet filling aluminum melt or alloy aluminum melt, be conducive to molten aluminium or alloy aluminum melt forms a large amount of crystallite in micropore, and combine closely on SiC skeleton surface, produce stretching prestress, thus greatly improve the physical strength of aluminium silicon carbide.
B. adopt constant temperature and pressure aluminizing technology, for the precast billet of thickness more than 15mm, be conducive to forming external phase, reduce aluminium silicon carbide Residual Porosity, improve density.
C. quick conductive technology adapts to the shaped piece aluminising of different geometric shape, and prestress square is to controlled.
D. material density is high, is conducive to improving the mechanical mechanics property of aluminum silicon carbide composite material and heat physical properties, meets the requirement of the field such as aerospace, precision instrument to materials thermophysics performance and mechanical mechanics property.
Accompanying drawing explanation
Fig. 1 is existing solidification mode schematic diagram;
Fig. 2 is cubes class mold solidification schematic diagram of the present invention;
Fig. 3 is that tubular die of the present invention solidifies schematic diagram;
Fig. 4 is Loadings On Hemispherical Shell class mold solidification schematic diagram of the present invention;
1 be mould, 2 be wherein thermal insulation layer, 3 be aluminium liquid entrance, 4 be silicon carbide green body, 5 be aluminium liquid passage, 6 be heat-transfer device, 7 for heat conduction direction.
Embodiment
Be intended to further illustrate the present invention below in conjunction with embodiment, and unrestricted the present invention.
Embodiment 1
By porosity 37%, thickness is die-filling after the rectangular parallelepiped silicon carbide porous precast billet of 15mm carries out surface treatment; The mould that porous silicon carbide precast billet is housed is placed in vacuum pressure is heavy oozes stove, being evacuated to furnace pressure is 10Pa, and displacement furnace atmosphere is argon gas, is warming up to 750 DEG C, insulation 2 hours at 750 DEG C; Open vacuum system, temperature 750 DEG C, under furnace pressure 15Pa degassed 20 minutes; Add molten aluminium, under additional gas liquid blend pressure, molten aluminium infiltrated in porous silicon carbide precast billet, during aluminising temperature keep 750 DEG C 1 minute.By heat pipe and mould one end face close contact, all the other bread of mould wrap up in thermal insulation layer; Die face temperature is with the cooling of the speed of 600 DEG C/min, and its lap cooling rate of mould is less than 100 DEG C/min; Molten aluminium forms aluminium crystallite in fast cooling face, and along thermograde reverse direction rapid solidification, lowers the temperature after 5 minutes, the furnace cooling demoulding, aluminium silicon carbide yield strength is 620MPa, thermal conductivity 205W/mK, the thermal expansivity 7.5 × 10 between room temperature to 150 DEG C -6/ K.
Embodiment 2
By porosity 50%, thickness is die-filling after the silicon carbide porous precast billet of 20mm rectangular parallelepiped carries out surface treatment; The mould that porous silicon carbide precast billet is housed is placed in vacuum pressure is heavy oozes stove, being evacuated to furnace pressure is 10Pa, and displacement furnace atmosphere is argon gas, is warming up to 750 DEG C, insulation 2 hours at 750 DEG C; Open vacuum system, temperature 750 DEG C, under furnace pressure 0.1Pa degassed 1 minute; Add molten aluminium, under additional gas liquid blend pressure, molten aluminium infiltrated in porous silicon carbide precast billet, during aluminising temperature keep 750 DEG C 2 minutes.By heat pipe and mould one end face close contact, all the other bread of mould wrap up in thermal insulation layer; Die face temperature is with the cooling of the speed of 400 DEG C/min, and its lap cooling rate of mould is less than 100 DEG C/min; Molten aluminium forms aluminium crystallite in fast cooling face, and along thermograde reverse direction rapid solidification, lowers the temperature after 5 minutes, the furnace cooling demoulding, aluminium silicon carbide yield strength is 500MPa, thermal conductivity 218W/mK, the thermal expansivity 8.5 × 10 between room temperature to 150 DEG C -6/ K.
Embodiment 3
By porosity 25%, thickness is die-filling after the silicon carbide porous precast billet of 15mm rectangular parallelepiped carries out surface treatment; The mould that porous silicon carbide precast billet is housed is placed in vacuum pressure is heavy oozes stove, being evacuated to furnace pressure is 1.0Pa, and displacement furnace atmosphere is argon gas, is warming up to 700 DEG C, insulation 4 hours at 700 DEG C; Open vacuum system, under 700 DEG C of temperature 50Pa furnace pressures degassed 30 minutes; Add 102 alloy aluminum melts, under gas-liquid mixed pressure, 102 alloy aluminum melts infiltrated in porous silicon carbide precast billet, during aluminising temperature keep 700 DEG C 1 minute.By heat pipe and mould one end face close contact, all the other bread of mould wrap up in thermal insulation layer; Die face temperature is with the cooling of the speed of 800 DEG C/min, and its lap cooling rate of mould is less than 100 DEG C/min; 102 alloy aluminum melts form alloy aluminum crystallite in fast cooling face, and along thermograde reverse direction rapid solidification, lower the temperature after 2 minutes, the furnace cooling demoulding, aluminium silicon carbide yield strength is 580MPa, thermal conductivity 205W/mK, the thermal expansivity 7.0 × 10 between room temperature to 150 DEG C -6/ K.
Embodiment 4
By porosity 50%, wall thickness is die-filling after the tubular silicon carbide porous preforming base of 10mm carries out surface treatment; The mould that tubular porous silicon carbide precast billet is housed is placed in vacuum pressure is heavy oozes stove, being evacuated to furnace pressure is 10Pa, and displacement furnace atmosphere is argon gas, is warming up to 750 DEG C, insulation 2 hours at 750 DEG C; Open vacuum system, temperature 750 DEG C, under furnace pressure 0.1Pa degassed 1 minute; Add molten aluminium, under additional gas liquid blend pressure, 102 alloy aluminum melts infiltrated in porous silicon carbide precast billet, during aluminising temperature keep 750 DEG C 2 minutes.Mold cylinder outer wall is enclosed with thermal insulation layer, and by heat pipe through mold center's close contact, mold center's temperature is with the cooling of the speed of 600 DEG C/min, and the peripheral cooling rate of mould is less than 100 DEG C/min; Molten aluminium radially wall forms aluminium crystallite, and rapid solidification, lowered the temperature after 5 minutes, the furnace cooling demoulding, and aluminium silicon carbide yield strength is 680MPa, thermal conductivity 221W/mK, the thermal expansivity 8.5 × 10 between room temperature to 150 DEG C -6/ K.
Embodiment 5
By porosity 30%, wall thickness is die-filling after the silicon carbide hollow hemispheric porous preforming base of 10mm carries out surface treatment; The mould that semisphere porous silicon carbide precast billet is housed is placed in vacuum pressure is heavy oozes stove, being evacuated to furnace pressure is 10Pa, and displacement furnace atmosphere is argon gas, is warming up to 750 DEG C, insulation 2 hours at 750 DEG C; Open vacuum system, temperature 750 DEG C, under furnace pressure 0.1Pa degassed 1 minute; Add molten aluminium, under additional gas liquid blend pressure, 102 alloy aluminum melts infiltrated in porous silicon carbide precast billet, during aluminising temperature keep 750 DEG C 2 minutes, mould sphere arranges thermal insulation layer insulation.By semisphere heat pipe and mould curved surface close contact, mold center's temperature is with the cooling of the speed of 800 DEG C/min, and the peripheral cooling rate of hemisphere of mould is less than 50 DEG C/min; Molten aluminium radially wall forms aluminium crystallite, and rapid solidification, lowered the temperature after 5 minutes, the furnace cooling demoulding, and aluminium silicon carbide yield strength is 590MPa, thermal conductivity 205W/mK, the thermal expansivity 7.5 × 10 between room temperature to 150 DEG C -6/ K.
Embodiment 6
By porosity 37%, thickness is die-filling after the rectangular parallelepiped silicon carbide porous precast billet of 15mm carries out surface treatment, the mould that porous silicon carbide precast billet is housed is placed in vacuum pressure is heavy oozes stove, being evacuated to furnace pressure is 10Pa, displacement furnace atmosphere is argon gas, be warming up to 750 DEG C, at 750 DEG C, be incubated 2 hours; Open vacuum system, temperature 750 DEG C, under furnace pressure 15Pa degassed 20 minutes; Add molten aluminium, under additional gas liquid blend pressure, molten aluminium infiltrated in porous silicon carbide precast billet, during aluminising temperature keep 750 DEG C 1 minute.Nitrogen is from mould one end face fast-refrigerating, and all the other bread of mould wrap up in thermal insulation layer; Die face temperature is with the cooling of the speed of 600 DEG C/min, and its lap cooling rate of mould is less than 100 DEG C/min; Molten aluminium forms aluminium crystallite in fast cooling face, and along thermograde reverse direction rapid solidification, lowers the temperature after 5 minutes, the furnace cooling demoulding, aluminium silicon carbide yield strength is 600MPa, thermal conductivity 203W/mK, the thermal expansivity 7.3 × 10 between room temperature to 150 DEG C -6/ K.
Embodiment 7
By porosity 37%, thickness is die-filling after the rectangular parallelepiped silicon carbide porous precast billet of 15mm carries out surface treatment, the insulation of 5, mould; The mould that porous silicon carbide precast billet is housed is placed in vacuum pressure is heavy oozes stove, being evacuated to furnace pressure is 10Pa, and displacement furnace atmosphere is argon gas, is warming up to 750 DEG C, insulation 2 hours at 750 DEG C; Open vacuum system, temperature 750 DEG C, under furnace pressure 15Pa degassed 20 minutes; Add molten aluminium, under additional gas liquid blend pressure, 6061 molten aluminiums infiltrated in porous silicon carbide precast billet, during aluminising temperature keep 750 DEG C 1 minute.Water coolant is from mould one end face fast-refrigerating, and all the other bread of mould wrap up in thermal insulation layer; Die face temperature is with the cooling of the speed of 600 DEG C/min, and its lap cooling rate of mould is less than 100 DEG C/min; Molten aluminium forms aluminium crystallite in fast cooling face, and along thermograde reverse direction rapid solidification, lowers the temperature after 5 minutes, the furnace cooling demoulding, aluminium silicon carbide yield strength is 580MPa, thermal conductivity 203W/mK, the thermal expansivity 10.3 × 10 between room temperature to 150 DEG C -6/ K.

Claims (6)

1. the preparation method of a high-volume fractional high strength aluminum silicon carbide composite material, first the silicon carbide porous precast billet of porosity 20-80% is assemblied in mould, molten metal aluminium liquid or alloy aluminum liquid is filled after high-temperature degassing, then cooling curing is carried out and the demoulding, it is characterized in that, the outer wall of mould wraps up thermal insulation layer, and use heat-transfer device to carry out directed quick conductive to molten metal aluminium liquid or alloy aluminum liquid in mould outer wall being enclosed with thermal insulation layer to solidify when cooling curing, heat conduction place that molten metal aluminium liquid or alloy aluminum liquid are contacted with heat-transfer device is solidified gradually for solidifying starting point,
The process of assembling precast billet and filling aluminum liquid is as follows:
A) the silicon carbide porous precast billet of porosity 20-80% is carried out surface treatment, be placed in mould, then mould is fixed in vacuum pressure aluminizing furnace, be warming up to 600-800 DEG C of insulation 2-6 hour;
B) by the porous SiC precast billet of above-mentioned isothermal holding, degassed under vacuum conditions, degassing temperature 500-800 DEG C, degassing time 0.1-2 hour; Degassing pressure 0.01-100Pa in stove;
C) molten metal aluminium liquid or alloy aluminum liquid is made fully to penetrate among the hole of silicon carbide porous precast billet by impressed pressure, capillary pressure and the acting in conjunction of cooling meat power, infiltrate in the process of porous SiC at molten aluminium or alloy aluminum melt, whole system continues at 600-800 DEG C of temperature, to keep 0.1-15 minute to ensure to be full of molten aluminium or alloy aluminum melt in micropore.
2. preparation method according to claim 1, is characterized in that,
The heat conduction place cooling rate that heat-transfer device contacts 200 DEG C/min ~ 900 DEG C/min, the cooling rate at thermal insulation layer parcel place is no more than 100 DEG C/min.
3. the preparation facilities of a high-volume fractional high strength aluminum silicon carbide composite material, comprise the mould for holding silicon carbide porous precast billet, it is characterized in that, described outer mold wall is enclosed with thermal insulation layer, also comprise the heat-transfer device for directed cooling molten metal aluminium liquid or alloy aluminum liquid, described heat-transfer device is arranged in mould or is close to outer mold wall.
4. the preparation facilities of a kind of high-volume fractional high strength aluminum silicon carbide composite material according to claim 3, it is characterized in that, described mould is cubes, and mould each outer wall is enclosed with thermal insulation layer, and the wherein outer wall that described heat-transfer device is close to mould is arranged.
5. the preparation facilities of a kind of high-volume fractional high strength aluminum silicon carbide composite material according to claim 3, it is characterized in that, described mould is tubular body arranged inside, and mold cylinder outer wall is enclosed with thermal insulation layer, and heat-transfer device penetrates and arranges to mold axis position.
6. the preparation facilities of a kind of high-volume fractional high strength aluminum silicon carbide composite material according to claim 3, it is characterized in that, described mould is Loadings On Hemispherical Shell, and mould housing outer side wall is enclosed with thermal insulation layer, and heat-transfer device is close to case inside wall and is arranged.
CN201310185323.8A 2013-05-20 2013-05-20 Preparation method and device of high-volume fraction and high-intensity aluminum silicon carbide composite material Expired - Fee Related CN103276277B (en)

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CN103939509B (en) * 2014-04-22 2018-04-17 浙江天乐新材料科技有限公司 A kind of Al/Sic and Cu/Sic composite materials friction pair for rail vehicle and preparation method thereof
TWI588436B (en) * 2014-05-02 2017-06-21 遠東科技大學 Heat transmitting structure as well as manufacturing method and heat dissipation method of the same
CN105331854A (en) * 2015-11-30 2016-02-17 无锡大塘复合材料有限公司 Aluminum alloy composite material and preparation method thereof
CN107012346B (en) * 2017-03-14 2018-11-23 广东鸿邦金属铝业有限公司 A kind of preparation method of the aluminium base of high temperature resistant low thermal coefficient of expansion/PMOS base complex layered materials
WO2019123223A1 (en) * 2017-12-20 2019-06-27 Freni Brembo S.P.A. Method of making a porous preform in silicon carbide with controlled porosity and silicon carbide porous preform

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CN102500748A (en) * 2011-10-25 2012-06-20 中南大学 Method for preparing aluminum silicon carbide composite material
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