CN101016591A - Method of preparing SiCp/Al composite material with complicated shape and high volume percent ratio - Google Patents
Method of preparing SiCp/Al composite material with complicated shape and high volume percent ratio Download PDFInfo
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- CN101016591A CN101016591A CN 200710064281 CN200710064281A CN101016591A CN 101016591 A CN101016591 A CN 101016591A CN 200710064281 CN200710064281 CN 200710064281 CN 200710064281 A CN200710064281 A CN 200710064281A CN 101016591 A CN101016591 A CN 101016591A
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Abstract
The invention discloses a preparing method of SiCp/Al composite with complete shape and high analytic in metal base composite material researching domain, which comprises the following steps: allocating pre-mixing liquid with monomer, cross linker and disperser; adding into SiC powder; balling; getting stable suspension with SiC volume content at 50-70%; adding into trigger and activator; stirring evenly; injecting into unapertured mold; solidifying and shaping in incubator with temperature at 50-70 deg.c; getting green compact; drying; discharging glue; presintering; getting SiC bone; placing Al alloy of 4-8% Mg, 6-12% Si on the adaptive position of bone; putting into heater; heating-up at 900-1200 deg.c under the protection of inert gas; inflating high pure nitrogen; keeping the temperature at 1-6 h; cooling; getting the product. This invention possesses the merit of cheap cost.
Description
Technical field
The invention belongs to field of research of metal, provide a kind of complicated shape high volume fraction ratio SiC especially
pThe preparation method of/Al matrix material.
Background technology
High-volume fractional (50～70%) SiC
p/ Al matrix material combines the premium properties of metallic aluminium and SiC, have excellent physics and mechanical property, as higher modulus of elasticity, high specific tenacity, characteristics such as good heat-conducting, in Electronic Packaging, fields such as aerospace are with a wide range of applications, no matter still be that the practical application direction always is one of problem of field of research of metal hottest point theoretically, emerged a large amount of preparation methods, as casting, jet deposition, powder metallurgic method etc., but because that these methods generally have a cost is too high, the not enough homogeneous of material structure, shortcomings such as poor performance, and only be applicable to the situation of low volume fraction.In addition, because SiC
pThe extremely difficult mechanical workout of carrying out of/Al matrix material has also limited its further development to a great extent.Therefore, the advanced near-net-shape technology of preparing of development remains one of main direction of its research.
At present, can prepare high-volume fractional SiC
pThe method of/Al matrix material has only method of impregnation.Whether rely on the effect of external force according to infiltration process, method of impregnation is divided into pressure infiltration and two research directions of pressure-free impregnation substantially.The pressure method of impregnation need apply extra pressure or vacuum condition in infiltration process, therefore to the requirement harshness of equipment, complicated operation, cost are very high.Advantages such as and pressure-free impregnation need not complex apparatus, and it is simple to have technology, with low cost have the better development prospect.The liquid metal Infiltration Technics is divided into two steps of skeleton preparation-infiltration, and the preparation of skeleton is the precondition of all technologies.At present, the preparation method of SiC skeleton mainly contains powder compression, injection molding etc.The SiC preform of pressing preparation exists density unevenness even, is subjected to mould to limit the simple shape that can only be shaped.And injection molding technology can only be applied to make small-sized component.Advantages such as the gel casting forming technology is a kind of new ceramic material colloidal shaping method, has plastic complicated shape large-scale component, and the molding blank quality is good, precision is high, equipment is simple, cost of investment is low all have the potential using value in a lot of fields.The gel injection volume content and the high volume fraction ratio SiC of solid particulate in the slurry
pThe volume fraction of SiC is more identical in the/Al matrix material.Based on above reason, the present invention at first utilizes the gel casting forming technology to prepare porous SiC skeleton, combines with pressure-free impregnation technology cheaply then, has successfully prepared the high volume fraction ratio SiC of complicated shape
p/ Al matrix material has solved the technical barrier of its low-cost preparation effectively.
Summary of the invention
The object of the present invention is to provide the high volume fraction ratio SiC of a kind of complicated shape
pThe preparation method of/Al matrix material has solved high volume fraction ratio complicated shape SiC
pThe low-cost near-net-shape technology of preparing difficult problem of/Al matrix material.
The present invention utilizes gel casting forming and pressure-free impregnation two step process to prepare complicated shape high-volume fractional silicon-carbide particle reinforced aluminium-base (SiC
p/ Al) matrix material.The specific implementation method is:
(1) slurry preparation: at first preparation contains the aqueous solution (premixed liquid) of monomer, linking agent, and wherein monomeric massfraction is 10～20%, and the mass ratio of monomer and linking agent is (30: 1)～(120: 1); (for guaranteeing high dimension precision, solid content is 50～70%, and this volume content is final SiC to pre-determined volume content to add SiC powder and dispersion agent in above-mentioned premixed liquid
pThe volume fraction of SiC in the/Al matrix material), obtain original slurry.Adopt means such as vibration, ball milling to make SiC homodisperse in slurry then, obtain the stable suspension of high solid loading.
(2) curing molding: add the initiator and the catalyzer of cumulative volume 0.5～1.O% and 0.05～0.1% in above-mentioned suspensoid, be injected into after stirring in the no punch die, the insulation can that moves into 50～70 ℃ is realized curing molding, obtains the SiC green compact, drying.
(3) skeleton is prepared: the above-mentioned dried of heating below 600 ℃, and the whole organic phases of burn off, and continue to be warming up to 800～1100 ℃, and be incubated 1～4 hour, skeleton is carried out presintering, but possessed the porous SiC prefabrication type skeleton of manipulation strength.
(4) pressure-free impregnation: will contain massfraction and be 4～8% Mg and the Al alloy of 6～12%Si and place SiC skeleton correct position to put into holding furnace together; be warming up to 900～1200 ℃ under the inert atmosphere protection; conversion atmosphere is incubated and naturally cools to room temperature after 1～6 hour to high pure nitrogen, obtains SiC
p/ Al matrix material.
Solvent in the premixed liquid of the present invention is not limited only to water, can be other organic medium such as ethanol etc., and monomer needs to have bigger solubleness in selected solvent.As water base acrylamide system, water-based acrylic hydroxyl ethyl ester system, ethanol based acrylamide system etc.
The particle diameter of SiC raw material powder of the present invention can be chosen in relative broad range, different proportionings has determined that the volume fraction of SiC can be controlled between 50～70% in the matrix material, can guarantee that like this green compact have very little shrinkage in drying process, formed precision is higher.
Major advantage of the present invention is:
1, the moulding process of SiC skeleton is simple, and its shape and size are unrestricted, and moulding process is very low to the requirement of mold material.
2, can prepare the complicated shape high volume fraction SiC
p/ Al matrix material, with low cost, functional.
The SiC that 3, can directly prepare nearly end form
p/ Al matrix material need not machining, the dimensional precision height.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Embodiment 1: the preparation volume fraction is 50% SiC
p/ Al composite material parts
With the deionized water is solvent, and acrylamide (AM) is a monomer, and methylene-bisacrylamide (MBAM) is for linking agent preparation monomer mass mark is 10%, MBAM and AM mass ratio are 1: 30 premixed liquid.The powder that with particle diameter is 2.5 μ m and 28 μ m is that 1: 4 ratio joins in the above-mentioned premixed solution with mass ratio, tetramethyl-oxyammonia 10% (TMAH) aqueous solution that adds powder quality mark 1.5% simultaneously makes SiC account for 50% of total volume fraction as dispersion agent.With the aluminum oxide is ball-milling medium, is mixed in the ball milling bucket 2 hours, obtains homogeneous dispersive SiC slurry.In above-mentioned slurry, add cumulative volume O.8% Ammonium Persulfate 98.5 5% aqueous solution (ASP) and 0.08% Tetramethyl Ethylene Diamine (TEMED) as catalyzer, back injection nonporous plastic mould stirs, the thermostat container of putting into 70 ℃ is incubated 40 minutes, continues insulation 6 hours after the demoulding under the atmosphere of high humidity.Improve temperature and accelerate rate of drying, till no longer changing to quality.Put into process furnace and be warming up to 400 ℃, be incubated 1 hour, continue to be warming up to 600, insulation post-heating to 1000 half an hour insulation carrying out in 2 hours presintering processing places SiC skeleton top with the aluminium alloy that accounts for SiC skeleton cumulative volume 50% required quality, feeds argon gas and is warming up to 1000 ℃, conversion atmosphere is to high pure nitrogen, be incubated 1 hour, furnace cooling obtains 50% SiC
p/ Al matrix material.
Embodiment 2: the preparation volume fraction is 60% SiC
p/ Al composite material parts
With water is solvent, acrylamide (AM) is a monomer, methylene-bisacrylamide (MBAM) is 15% for linking agent preparation monomer mass mark, MBAM and AM mass ratio are 1: 70 premixed liquid, the powder that with particle diameter is 7 μ m and 63 μ m is that 1: 2 ratio joins in the above-mentioned premixed solution with mass ratio, tetramethyl-oxyammonia 10% (TMAH) aqueous solution that adds powder quality mark 2.0% simultaneously is as dispersion agent, ball milling 4 hours, stir and obtain homogeneous dispersive SiC slurry, stir and in above-mentioned suspensoid, add Ammonium Persulfate 98.5 5% aqueous solution (ASP) of slurry volume mark 0.6% and 0.06% ‰ Tetramethyl Ethylene Diamine (TEMED) as catalyzer, back injection nonporous plastic mould stirs, the thermostat container of putting into 60 ℃ of high humidity is incubated 40 minutes, the follow-up continuation of insurance temperature of the demoulding 5 hours.Accelerate rate of drying, till no longer changing to quality.Put into process furnace and be warming up to 400 ℃, be incubated 2 hours, continue to be warming up to 600 ℃, insulation post-heating to 900 ℃ presintering half an hour 2 hours places SiC skeleton correct position with the aluminium that accounts for SiC skeleton cumulative volume 40% required aluminium alloy quality, feeds high pure nitrogen, be warming up to 1100 ℃, be incubated 3 hours, furnace cooling obtains 60% SiC
p/ Al matrix material.
Embodiment 3: the preparation volume fraction is 70% SiC
p/ Al composite material parts
With the deionized water is solvent, acrylamide (AM) is a monomer, methylene-bisacrylamide (MBAM) is 20% for linking agent preparation monomer mass mark, MBAM and AM mass ratio are 1: 120 premixed liquid, with particle diameter is 0.8 μ m, the powder of 7 μ m and 63 μ m is that 1: 2: 4 ratio joins in the above-mentioned premixed solution with mass ratio, make the volume of SiC account for 70% of cumulative volume, tetramethyl-oxyammonia 10% (TMAH) aqueous solution that adds powder quality mark 2.8% simultaneously is as dispersion agent, ball milling 6 hours, stir and obtain homogeneous dispersive SiC suspensoid, in above-mentioned suspensoid, add Ammonium Persulfate 98.5 5% aqueous solution (ASP) of slurry volume mark 0.4% and 0.04% Tetramethyl Ethylene Diamine (TEMED) as catalyzer, the no punch die of back injection stirs, the thermostat container of putting into 50 ℃ is incubated 40 minutes, the follow-up continuation of insurance temperature of the demoulding 5 hours, improve temperature and accelerate rate of drying, till no longer changing to quality.Put into process furnace and be warming up to 400 ℃, be incubated 1 hour, continue to be warming up to 600 ℃, insulation post-heating half an hour is to pre-sintering temperature insulation 2 hours, naturally cooling.Calculating accounts for the quality of above-mentioned SiC skeleton cumulative volume 30% required aluminium alloy, is placed on SiC skeleton top and puts into the controlled process furnace of atmosphere together, feeds high pure nitrogen, is warming up to 1200 ℃, is incubated 4 hours, and furnace cooling obtains 70% SiC
p/ Al matrix material.
Claims (3)
1, the high volume fraction ratio SiC of a kind of complicated shape
pThe preparation method of/Al matrix material, gel injection-pressure-free impregnation prepared SiC
p/ Al matrix material is characterized in that, processing step is:
(1) slurry preparation: preparation contains the premixed liquid of monomer, linking agent and dispersion agent, and wherein monomeric massfraction is 10～20%, and the mass ratio of monomer and linking agent is (30: 1)～(120: 1); In premixed liquid, add the SiC powder and make it account for 50～70% of premixed liquid volume content, obtain original slurry; Adopt vibration, ball milling means to make SiC homodisperse in slurry then, obtain the stable suspension of high solid loading;
(2) curing molding: the initiator and the catalyzer that in above-mentioned suspensoid, add cumulative volume 0.5～1.0% and 0.05～0.1% respectively, be injected into after stirring in the no punch die, the insulation can that moves into 50～70 ℃ is realized curing molding, obtains the SiC green compact, and it is carried out drying;
(3) skeleton is prepared: the whole organic phases of burn off below 600 ℃, and continue to be warming up to 800～1100 ℃, and be incubated 1～4 hour, skeleton is carried out presintering, but possessed the porous SiC prefabrication type skeleton of manipulation strength;
(4) pressure-free impregnation: will contain massfraction and be 4～8% Mg and the Al alloy of 6～12%Si and place SiC skeleton correct position to put into process furnace together; be warming up to 900～1200 ℃ under the inert atmosphere protection; conversion atmosphere is incubated and naturally cools to room temperature after 1～6 hour to high pure nitrogen, obtains SiC
p/ Al matrix material.
2, according to claims 1 described method, it is characterized in that: the solvent in the described premixed liquid is water or ethanol, and monomer is acrylamide system, Hydroxyethyl acrylate system or ethanol based acrylamide system.
3, according to claims 1 described method, it is characterized in that: the volume fraction of SiC is controlled between 50～70% in the matrix material.
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| CN101898240A (en) * | 2010-08-09 | 2010-12-01 | 西安科技大学 | Preparation method of SiC/Al composite material for electronic packaging |
| CN101941231A (en) * | 2010-09-09 | 2011-01-12 | 中国科学院长春光学精密机械与物理研究所 | Gel injection molding technology of large-sized and complicated-shape silicon carbide ceramic biscuit |
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