CN1202273C - Method for pressureless infiltration preparing high content Si/Al compound material - Google Patents

Method for pressureless infiltration preparing high content Si/Al compound material Download PDF

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CN1202273C
CN1202273C CN 03134422 CN03134422A CN1202273C CN 1202273 C CN1202273 C CN 1202273C CN 03134422 CN03134422 CN 03134422 CN 03134422 A CN03134422 A CN 03134422A CN 1202273 C CN1202273 C CN 1202273C
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silicon
infiltration
content
aluminium alloy
porous
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CN 03134422
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CN1483845A (en
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胡锐
朱冠勇
李金山
傅恒志
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Northwestern Polytechnical University
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Northwestern Polytechnical University
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Abstract

The present invention relates to a process for preparing a composite material with high contents of Si/Al in the field of a material. In the present invention, in order to overcome the defects of collapse or deformation of precast bodies, and no assurance of the near net shapes of product shapes which occur when the prior art is used in the process of preparing and infiltrating silicon-aluminum systems, a porous silicon precast body is precast and formed by adopting isostatic cool pressing, and the particle size and the isostatic cool pressing technological parameters of silicon are regulated so as to enable the porosity to range from 25 to 50%; the precast body is put in a ceramic crucible, an aluminium alloy material comprising the components of 10 to 20% of silicon and 0 to 5% of magnesium is put on the precast body, and the precast body and the aluminium alloy material are cooled in a furnace to a room temperature after being heated in vacuum or nitrogen and insulated so as to obtain a composite material containing 50 to 75% (volume content) of silicon. The present invention effectively inhibits porous frameworks of silicon from being dissolved in the process of infiltration, has the advantages of simple process and high infiltration efficiency, and ensures the integrity of porous frameworks of silicon and the near net shape of the product; the silicon phase of the obtained composite material is in continuous three dimensional networks, and gaps in the aluminium alloy phase of the composite material also are communicated in a three dimensional mode.

Description

The pressure-free impregnation preparation method of high-content Si/Al matrix material
(1) technical field:
The present invention relates to the material field, is a kind of preparation method of Si/Al matrix material of high content silicon.
(2) technical background:
The thermal control material requirements has high heat conductance, the end coefficient of expansion.The heat conductivility of aluminium and aluminium alloy is very good, but thermal expansivity is higher; Silicon not only thermal expansivity is very low, and heat conductivility is also better.Therefore, the advantage of comprehensive two class materials, according to the method for composite Materials Design, it is compound to select for use high-load silicon and aluminium and alloy thereof to carry out, and can obtain the very excellent light-weight thermal control material of thermal characteristics.Because high-content Si/Al material si content very high (weight content is 40~70%) can not adopt the manufacturing of conventional cast method.Mainly adopt special technology for this type of high preparation that strengthens the matrix material of body burden at present.
It is the 40-70%Si/Al material that Britain Osprey company adopts spray deposition technology to prepare weight content.The principle of spray deposition technology is that molten metal flow is atomized into fine drop by the high energy high pressure gas, and drop collided and formed blank with collector on collector before solidifying fully.Spray deposition technology has significant limitation, and its gained material density is low, and the real yield of material is low, can not obtain nearly end form part, and the equipment requirements height, investment is big, cost is very high, environmental pollution is big.
It is the Al/Si of 60-70vol%Si content that the method for employing infiltration by squeeze casting such as the C.W.Chien in Taiwan has been prepared volume content pMatrix material.The metal-base composites that the height that this technological process prepares other system with the pressure method of impregnation strengthens body burden is the same, silicon grain is prefabricated into the porous prefabricated component, again prefabricated component is put into metal mold cavity, utilize pressure die-casting machine equipressure equipment that aluminum alloy melt is under high pressure infiltrated in the hole of prefabricated component, obtain composite product.The production efficiency height of this method, but the problem that exists is the simple shape of metal products, needs special press device and mould etc., thereby has limited its development.
In sum, for the Si/Al matrix material of high volume content silicon, hope can be developed a kind of simple and reliable technology, does not need to rely on means such as impressed pressure and spray deposition, and also not wishing need very complicated preparation equipment or very high preparation temperature.In addition, also wish to reduce the follow-up mechanical workout of matrix material, the composite product shape near-net-shape of trying one's best as far as possible.The pressure-free impregnation preparation technology relevant with the present invention can reach this purpose.
Molten metal infiltration porous insert is a comparatively complicated process, is subjected to the porosity of porous insert, forms particle shape, the size of porous insert, the molten metal influence of various factors that becomes to grade.Wherein, the physics of wetting, dissolving between porous materials and the molten metal or reaction etc., chemical relationship have very important influence to the generation and the process of infiltration.Present prepares the relevant patent of matrix material with pressure-free impregnation, mainly relates to preparation aluminum oxide or silicon carbide enhanced aluminum matrix composite and auxiliary process aspect thereof.
United States Patent (USP) 4,828,008 discloses the technology of preparing that a kind of name is called " metal-base composites " (Metal Matrix Composites), according to this technology, can prepare matrix material by molten metal infiltration weighting material under hot conditions.Being characterized as of this technology: contain 3% magnesium in the aluminium liquid at least; Atmosphere during infiltration is the mixed gas of nitrogen and argon gas; The content of the ceramic phase in the matrix material can be very high; Infiltration 25mm thickness needs 12 hours.
United States Patent (USP) 4,935,055 discloses a kind of " using barrier to prepare the method for metal-base composites " by name.This invention has proposed to utilize graphite or titanium boride to be barrier, and the continuation infiltration of molten metal capable of blocking is to make the processing parts of clean no surplus.Two patents are arranged again subsequently, the technology that stops that this patent is related is improved.
Patent Office of the People's Republic of China discloses on April 7th, 1999 that (publication number: CN 1212915A) name is called the application for a patent for invention of " pressureless penetration casting method of aluminum matrix composite ".A kind of pressureless penetration casting method of aluminum matrix composite is disclosed in this this application.According to this patent, high rigidity ceramic particle stopping composition is aluminium sesquioxide or silicon carbide, need use ferric oxide or Z 250 is made penetration-assisting agent, and al alloy component is silicon 5-20%, calcium 0.1-0.8%, magnesium 0.1-1%, and preparation temperature is 800 ℃-900 ℃.
More than several patents all be about preparation aluminium sesquioxide or silicon carbide enhanced aluminum matrix composite.Very poor of aluminium sesquioxide-aluminium system and silicon carbide-aluminium system, wettability can not dissolved, and more chemical reaction can not take place.Aluminum alloy melt can not dissolve precast body in infiltration process, the precast body skeleton can not destroyed.But for silicon-aluminium system, system is metallurgical wetting, and wetting angle is 0 °, and when temperature was higher, silicon can be dissolved in aluminium in a large number, and during such as 760 ℃, the highest solubility of silicon can reach 20% in the aluminium liquid.Suppress dissolving as not taking measures and take place, precast body then will occur and cave in or be out of shape in infiltration process, the near-net-shape of article shape can't ensure.Therefore, above patent mainly is devoted to adopt various physics, chemical method to promote the wettability of system, and to be not suitable for for the preparation of silicon-aluminium system.
(3) summary of the invention:
Precast body can occur and cave in or be out of shape for overcoming the infiltration process that exists when prior art is used for the preparation of silicon-aluminium system, the deficiency that the near-net-shape of article shape can't ensure, invention has proposed a kind of preparation method of Si/Al matrix material of high content silicon.
For achieving the above object, the present invention has adopted the pressure-free impregnation preparation technology of aluminum matrix composite.Compared with prior art, the invention is characterized in: adopt the method for the prefabricated shaping of isostatic cool pressing that silicon grain is prefabricated into granularity and the isostatic cool pressing processing parameter that the porous silicon precast body is regulated silicon, porosity can change between 25-50%; Porous preform is put into ceramic crucible, be placed to the aluminium alloy material that is divided into silicon 10-20%, magnesium 0-5% thereon, after intensification and the process insulation, stove is chilled to the matrix material that room temperature can obtain silicon volume content 50-75% under vacuum or under the nitrogen; Infiltration temperature is 650-900 ℃, and soaking time is 30-180 minute.
Used silicon grain is silicon single crystal or silicon metal particle among the present invention.
The present invention has realized that successfully the aluminum alloy melt pressure-free impregnation prepares the aluminium silicon composite of high volume content silicon.The impurity element that adds in the aluminum alloy melt is few, and the volatility of Mg is very good, and infiltration finishes the basic noresidue in back, and the intermetallic compound that forms owing to these elements in the matrix material of acquisition is few, the interface cleaning, and the performance of reactionless product material improves.In the infiltration process, suppressed effectively silicon porous insert skeleton by the dissolving of aluminium liquid, guaranteed the integrity of silicon porous insert skeleton and the near-net-shape of composite product.Simultaneously, in the infiltration process, the wettability of system does not have weakened, has guaranteed carrying out smoothly of pressure-free impregnation, and infiltration speed is fast, per hour can reach 30-50mm.The present invention can prepare the aluminium silicon composite material of silicon volume content 50-75%, it is continuous that the matrix material silicon of gained is the three-dimensional network shape mutually, aluminium alloy is also three-dimensional communication of crack betwixt mutually, has guaranteed effective performance of the aluminium silicon composite excellent thermal of high volume content silicon.
(4) embodiment:
Embodiment one:
With 3.5 gram mean particle sizes is the calm porous preform that is prefabricated into Φ 20mm * 10mm of pressing of commercially available silicon single crystal particle of 40 μ m, the porosity of this porous preform is about 53% volume content, the Al alloy block of 4.5 grams is placed on it, put into corundum crucible together No. 5, under nitrogen, be warmed up to 700 ℃ and be incubated 1 hour.The composition of Al alloy block is silicon 15%, magnesium 1%, and surplus is an aluminium.
Embodiment two:
With 5 gram mean particle sizes is the calm porous preform that is prefabricated into Φ 20mm * 10mm of pressing of commercially available silicon single crystal particle of 40 μ m, the porosity of this porous preform is about 75% volume content, the Al alloy block of 3 grams is placed on it, put into corundum crucible together No. 5, under vacuum, be warmed up to 650 ℃ and be incubated 3 hours.The composition of Al alloy block is silicon 15%, magnesium 5%, and surplus is an aluminium.
Embodiment three:
Being that the commercially available silicon metal particle of 40 μ m is calm with 3 gram mean particle sizes presses that to be prefabricated into the bottom surface be 15mm * 10mm, height is the rectangular parallelepiped porous preform of 20mm, the porosity of this porous preform is about 65% volume content, the Al alloy block of 3.5 grams is placed on it, put into corundum crucible together No. 5, under nitrogen, be warmed up to 900 ℃ and be incubated 1 hour.The composition of Al alloy block is silicon 15%, magnesium 1%, and surplus is an aluminium.
Embodiment four:
Being that the commercially available silicon metal particle of 40 μ m is calm with 3.5 gram mean particle sizes presses that to be prefabricated into the bottom surface be 15mm * 10mm, height is the rectangular parallelepiped porous preform of 20mm, the porosity of this porous preform is about 75% volume content, the Al alloy block of 3 grams is placed on it, put into corundum crucible together No. 5, under nitrogen, be warmed up to 900 ℃ and be incubated 1 hour.The composition of Al alloy block is silicon 15%, magnesium 5%, and surplus is an aluminium.

Claims (3)

1. the pressure-free impregnation preparation method of a high-content Si/Al matrix material, put into thermally resistant container after silicon grain is prefabricated into the porous silicon precast body, placing aluminium alloy material thereon, in process furnace, rise to infiltration temperature, insulation under the vacuum or under the nitrogen, stove was chilled to the matrix material that room temperature can obtain silicon volume content 50-75% after infiltration was finished, and it is characterized by:
(1) porous preform adopts the prefabricated shaping of isostatic cool pressing, and granularity and isostatic cool pressing processing parameter, the porosity of regulating silicon can change between 25-50%;
(2) utilize aluminium alloy to infiltrate, its composition and weight content are: silicon 10-20%, magnesium 1-5%, and surplus is an aluminium;
(3) infiltration temperature is 650-900 ℃, and soaking time is 30-180 minute.
2. the pressure-free impregnation preparation method of high-content Si/Al matrix material as claimed in claim 1, it is characterized by described silicon grain is silicon single crystal or silicon metal particle.
3. the pressure-free impregnation preparation method of high-content Si/Al matrix material as claimed in claim 1 is characterized by and adopts the cold mode of stove to cool off after infiltration is finished.
CN 03134422 2003-07-23 2003-07-23 Method for pressureless infiltration preparing high content Si/Al compound material Expired - Fee Related CN1202273C (en)

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Application Number Priority Date Filing Date Title
CN 03134422 CN1202273C (en) 2003-07-23 2003-07-23 Method for pressureless infiltration preparing high content Si/Al compound material

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Application Number Priority Date Filing Date Title
CN 03134422 CN1202273C (en) 2003-07-23 2003-07-23 Method for pressureless infiltration preparing high content Si/Al compound material

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CN1202273C true CN1202273C (en) 2005-05-18

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100455546C (en) * 2007-01-05 2009-01-28 华南理工大学 Ultraporous ceramic base heat accumulating material and its preparation method
CN102114541B (en) * 2009-12-30 2012-12-26 北京有色金属研究总院 Preparation process of high volume fraction silicon particle enhanced aluminum based composite material
CN102009160A (en) * 2010-12-13 2011-04-13 中国航空工业集团公司北京航空材料研究院 Method for preparing high volume fraction particle reinforced metal matrix composites through near net shaping
CN106906388B (en) * 2017-04-06 2018-05-11 合肥工业大学 A kind of preparation method of silumin
CN108441667A (en) * 2018-05-02 2018-08-24 西安朗赛精密机械有限公司 A kind of preparation method of Al-base ceramic composite material
CN110983092B (en) * 2019-12-12 2021-01-15 中国科学院长春光学精密机械与物理研究所 Pressureless infiltration furnace and method for preparing particle reinforced aluminum matrix composite

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