CN111889686B - Method for reinforcing aluminium base composite material by high-strength silicon carbide particle and composite material thereof - Google Patents
Method for reinforcing aluminium base composite material by high-strength silicon carbide particle and composite material thereof Download PDFInfo
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Abstract
The invention discloses a method for preparing a high-strength silicon carbide particle reinforced aluminum matrix composite and the composite, which comprises the following steps: s1, uniformly ball-milling silicon carbide particles and aluminum powder with different particle sizes according to a certain mass ratio; s2, adding the adhesive, the milk wax and the aluminum dihydrogen phosphate, uniformly stirring and sieving for later use; s3, placing the sieved material into a mold, and demolding to obtain a silicon aluminum carbide pre-sintered body; and S4, sintering, crushing, ball-milling and shaping the pre-sintered body, and sieving to obtain silicon aluminum carbide particles. The invention obtains the high-strength silicon carbide reinforced aluminum composite material by modifying small-particle-size silicon carbide particles, then preparing a silicon aluminum carbide prefabricated model and finally infiltrating aluminum liquid in a differential pressure manner.
Description
Technical Field
The invention relates to the technical field of composite material preparation, in particular to a method for preparing a high-strength silicon carbide particle reinforced aluminum matrix composite material and the composite material.
Background
The silicon carbide aluminum composite material belongs to a ceramic reinforced metal matrix composite material, and takes aluminum alloy as a matrix and silicon carbide ceramic particles as a reinforcing phase. The composite material has the advantages of high specific stiffness, high thermal conductivity, low expansion coefficient, low density and the like, and is widely applied to the fields of aerospace, high-power electronic component heat dissipation packaging, optical devices, wear resistance and the like.
The existing high-volume silicon carbide aluminum composite material is obtained by adopting a pressure casting mode, namely, silicon carbide particles are firstly adopted to prepare a porous ceramic prefabricated model, then an aluminum alloy solution permeates into silicon carbide ceramic through pressure casting, the method has no problem for preparing the silicon carbide aluminum material with common strength, and is difficult to prepare the ultrahigh-strength composite material, especially when the size of the silicon carbide particles is less than 5 mu m, the silicon carbide particles in the sintering or heating process of the prepared ceramic prefabricated model can move or diffuse, reserved channels are extruded, and therefore the aluminum liquid can not permeate into the silicon carbide prefabricated model, or even if a small amount of silicon carbide particles permeate into the surface layer, the performance can not meet the requirements far.
When the size of silicon carbide particles is less than 5 mu m, the submicron or nanoscale silicon aluminum carbide is mostly realized by adopting a stirring casting method, however, the method is easy to generate particle agglomeration, the volume fraction of the prepared composite material is generally difficult to be more than 25%, and the strength and the performance in all aspects are not as good as those of a product prepared by a pressure casting method.
Disclosure of Invention
The invention aims to: aiming at the existing problems, the method for enhancing the aluminum matrix composite by the high-strength silicon carbide particles and the composite thereof are provided, the high-strength silicon carbide particle composite is obtained by modifying the small-particle size silicon carbide particles, then obtaining the silicon carbide aluminum prefabricated model, and finally infiltrating aluminum liquid by differential pressure, so that the problem that the high-volume small-particle size silicon carbide prefabricated model cannot infiltrate the aluminum liquid is solved, a new thought is provided for the preparation of the high-strength silicon carbide particle composite, and the defects of the existing pressure casting and stirring casting are overcome.
The technical scheme adopted by the invention is as follows: a method for reinforcing an aluminum matrix composite by high-strength silicon carbide particles is characterized by comprising the following steps:
s1, uniformly ball-milling silicon carbide particles with the particle sizes of 0.1-0.25 mu m, 0.3-0.5 mu m and 0.6-0.8 mu m and aluminum powder with the particle size of 5-10 mu m in an inert gas atmosphere according to a certain mass ratio;
s2, adding 0.5-3% of adhesive, 0.5-2% of emulsion wax and 0.3-1% of aluminum dihydrogen phosphate in mass ratio into the ball-milled materials, uniformly stirring and sieving for later use;
s3, placing the sieved material into a mold, maintaining the pressure for 5-60S under the pressure of 10-20MPa, and demolding to obtain a silicon aluminum carbide pre-sintered body;
s4, sintering the pre-sintered body in a vacuum weak reducing atmosphere sintering furnace to obtain a silicon aluminum carbide material with low aluminum content after sintering;
s5, crushing, ball-milling, shaping and sieving the silicon aluminum carbide composite material to obtain silicon aluminum carbide particles;
and S6, taking the silicon-aluminum carbide particles obtained in the step S5 as a raw material of the high-strength silicon carbide particle reinforced aluminum matrix composite.
In the invention, the mass ratio of silicon carbide particles with the particle diameters of 0.1-0.25 mu m, 0.3-0.5 mu m and 0.6-0.8 mu m to aluminum powder with the particle diameter of 5-10 mu m is respectively 5-25:10-35:30-75:5-10.
preferably, in S1, the silicon carbide particles have particle diameters of 0.25 μm,0.5 μm, and 0.8 μm, respectively.
In the invention, in S4, the sintering temperature is 500-800 ℃, and the sintering atmosphere is a mixed atmosphere of nitrogen and hydrogen.
In the invention, the adhesive is selected from one or more of polyvinyl alcohol, polyvinyl acetate, dextrin and paraffin, and is preferably polyvinyl alcohol.
The invention also comprises a preparation method of the high-strength silicon aluminum carbide composite material, which is characterized by comprising the following steps:
s5.1, selecting the silicon aluminum carbide particles prepared by the method for preparing the high-strength silicon carbide particle reinforced aluminum matrix composite, and selecting the silicon aluminum carbide particles with the particle sizes of 8-12 microns, 20-40 microns and 50-80 microns respectively;
s5.2, uniformly mixing silicon aluminum carbide particles with the particle sizes of 8-12 microns, 20-40 microns and 50-80 microns according to a certain mass ratio, then adding 0.5-3% of adhesive, 0.5-2% of emulsion wax and 0.5-5% of pore-forming agent by mass ratio, uniformly stirring and sieving for later use;
s5.3, putting the material prepared in the previous step into a die to prepare a pre-sintered body;
s5.4, sintering the pre-sintered body in a vacuum weak reducing atmosphere sintering furnace to obtain a silicon-aluminum carbide prefabricated model;
s5.5, placing the silicon aluminum carbide prefabricated model into a mold in a vacuum differential pressure casting furnace, and injecting aluminum alloy molten metal into pores of the silicon aluminum carbide prefabricated model by a vacuum differential pressure casting method to prepare a composite material;
and S5.6, after cooling, putting the composite material into a heat treatment furnace for annealing treatment, thus obtaining the high-strength aluminum-based silicon carbide composite material.
Further, the mass ratio of the silicon aluminum carbide particles with the particle diameters of 8-12 μm, 20-40 μm and 50-80 μm is 10-20:20-40:30-70.
preferably, silicon aluminum carbide particles with the particle diameters of 10 μm, 30 μm and 60 μm are mixed according to the mass ratio of 10-20:20-40:30-70, then adding adhesive, cream wax and pore-forming agent.
In the invention, the adhesive is selected from one or more of polyvinyl alcohol, polyvinyl acetate, dextrin and paraffin, and is preferably polyvinyl alcohol; the pore-forming agent is selected from one or more of starch, carbon powder and ammonium oxalate, and is preferably starch.
The invention also comprises a high-strength silicon aluminum carbide composite material, which is characterized by being prepared by the preparation method of the high-strength silicon aluminum carbide composite material according to any one of claims 5 to 9, wherein the bending strength of the high-strength silicon aluminum carbide composite material is not lower than 600MPa, and the air tightness of the high-strength silicon aluminum carbide composite material is less than 10 -10 Pa·m 3 /s。
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. according to the method for preparing the high-strength silicon carbide particle reinforced aluminum-based composite material and the composite material thereof, provided by the invention, small-particle-size silicon carbide particles are modified, then a silicon-aluminum carbide prefabricated model is obtained, and finally aluminum liquid is infiltrated by differential pressure to obtain the high-strength silicon-aluminum carbide composite material, so that the defects of easy agglomeration and difficult infiltration of submicron or nanoscale silicon carbide (the particle size is less than 1 mu m) are overcome, the problems of small-particle-size silicon carbide surface wettability and difficulty in pore reservation are solved, a new thought is provided for the preparation of the high-strength silicon-aluminum carbide composite material, and the defects of the existing pressure casting and stirring casting are overcome;
2. the preparation method can prepare the silicon aluminum carbide composite material with 50-70 percent of volume according to the proportion, and the silicon aluminum carbide composite material has excellent mechanical property, bending strength of more than 600MPa, good compactness and air tightness of less than 10 -10 Pa·m 3 And/s, meets the requirements of military industry, has low roughness after processing, and is beneficial to carrying out later surface treatment and related electroplating and chemical plating work.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
A preparation method of a high-strength silicon carbide reinforced aluminum composite material comprises the following steps:
s1, respectively mixing silicon carbide particles with the particle sizes of 0.1-0.25 mu m, 0.3-0.5 mu m and 0.6-0.8 mu m and aluminum powder with the particle size of 5-10 mu m according to the mass ratio of 5:10:75:10, ball milling uniformly under the protection of nitrogen atmosphere;
s2, adding 0.5% of polyvinyl alcohol solution, 2% of emulsion wax and 0.3% of aluminum dihydrogen phosphate solution in mass ratio into the ball-milled materials, uniformly stirring and sieving for later use;
s3, placing the sieved materials into a mold, maintaining the pressure for 5S under the pressure of 10MPa, and demolding to obtain a silicon aluminum carbide pre-sintered body;
s4, sintering the pre-sintered body in a vacuum weak reducing atmosphere sintering furnace, wherein the sintering temperature is 500 ℃, the sintering atmosphere is nitrogen and hydrogen, and after sintering is completed, the silicon aluminum carbide material with low aluminum content is obtained;
s5, crushing, ball-milling and shaping the low-aluminum-content silicon carbide aluminum composite material, sieving, and selecting silicon carbide aluminum particles with the particle sizes of 8-12 microns, 20-40 microns and 50-80 microns respectively;
s6, respectively mixing silicon aluminum carbide particles with the particle sizes of 8-12 microns, 20-40 microns and 50-80 microns according to the mass ratio of 10:20:70, then adding 3 percent of polyvinyl alcohol solution, 0.5 percent of milk wax and 0.5 percent of starch in mass ratio, stirring uniformly and sieving for later use;
s7, placing the material prepared in the previous step into a mold, maintaining the pressure for 5S under the pressure of 10MPa, and demolding to obtain a blank;
s8, sintering the presintered body in a vacuum weak reducing atmosphere sintering furnace at the temperature of 300 ℃ in the nitrogen and hydrogen atmosphere to obtain a silicon aluminum carbide prefabricated model after sintering;
s9, placing the silicon carbide aluminum prefabricated mold into a mold in a vacuum differential pressure casting furnace, and injecting aluminum alloy molten metal into pores of the silicon carbide aluminum prefabricated mold by a vacuum differential pressure casting method under the protection of inert atmosphere so as to complete interface compounding of ceramic particles and molten metal, wherein in the impregnation process, the temperature of the aluminum alloy solution is controlled to be 680 ℃, and the impregnation pressure is 0.1MPa;
and S10, after cooling, putting the composite material into a heat treatment furnace for annealing treatment to obtain the high-strength aluminum-based silicon carbide composite material.
Example 2
A preparation method of a high-strength silicon carbide reinforced aluminum composite material comprises the following steps:
s1, respectively mixing silicon carbide particles with the particle sizes of 0.25 mu m,0.5 mu m and 0.8 mu m and aluminum powder with the particle size of 5-10 mu m according to the mass ratio of 10:20:60:10, ball milling uniformly under the protection of nitrogen atmosphere;
s2, adding 3% of polyvinyl alcohol solution, 0.5% of emulsion wax and 1% of aluminum dihydrogen phosphate solution in mass ratio into the ball-milled materials, uniformly stirring and sieving for later use;
s3, placing the sieved material into a mold, maintaining the pressure for 60S under the pressure of 15MPa, and demolding to obtain a silicon aluminum carbide pre-sintered body;
s4, sintering the presintered body in a vacuum weak reducing atmosphere sintering furnace, wherein the sintering temperature is 800 ℃, the sintering atmosphere is nitrogen and hydrogen, and obtaining the silicon aluminum carbide material with low aluminum content after sintering;
s5, crushing, ball-milling and shaping the low-aluminum-content silicon carbide aluminum composite material, sieving, and selecting silicon carbide aluminum particles with the particle sizes of 10 microns, 30 microns and 60 microns respectively;
s6, respectively mixing 10-micron, 30-micron and 60-micron silicon aluminum carbide particles according to the mass ratio of 20:40:40, adding 3% of polyvinyl alcohol solution, 2% of milk wax and 5% of starch in mass ratio, stirring uniformly and sieving for later use;
s7, placing the material prepared in the previous step into a mold, maintaining the pressure for 120S under the pressure of 20MPa, and demolding to obtain a blank;
s8, sintering the presintered body in a vacuum weak reducing atmosphere sintering furnace at the sintering temperature of 500 ℃ in the sintering atmosphere of nitrogen and hydrogen to obtain a silicon aluminum carbide prefabricated model after sintering;
s9, placing the silicon carbide aluminum prefabricated mold into a mold in a vacuum differential pressure casting furnace, and injecting aluminum alloy molten metal into pores of the silicon carbide aluminum prefabricated mold by a vacuum differential pressure casting method under the protection of inert atmosphere so as to complete interface compounding of ceramic particles and molten metal, wherein in the impregnation process, the temperature of the aluminum alloy solution is controlled to be 750 ℃, and the impregnation pressure is 0.3MPa;
and S10, after cooling, putting the composite material into a heat treatment furnace for annealing treatment to obtain the high-strength aluminum-based silicon carbide composite material.
Example 3
A preparation method of a high-strength silicon carbide reinforced aluminum composite material comprises the following steps:
s1, respectively mixing silicon carbide particles with the particle sizes of 0.25 mu m,0.5 mu m and 0.8 mu m and aluminum powder with the particle size of 5-10 mu m according to the mass ratio of 10:12:70:8, ball milling uniformly under the protection of nitrogen atmosphere;
s2, adding a polyvinyl alcohol solution with the mass ratio of 2%, a milk wax with the mass ratio of 1% and an aluminum dihydrogen phosphate solution with the mass ratio of 1% into the ball-milled materials, uniformly stirring and sieving for later use;
s3, placing the sieved material into a mold, maintaining the pressure for 30S under the pressure of 20MPa, and demolding to obtain a silicon aluminum carbide pre-sintered body;
s4, sintering the pre-sintered body in a vacuum weak reducing atmosphere sintering furnace, wherein the sintering temperature is 700 ℃, the sintering atmosphere is nitrogen and hydrogen, and after sintering is completed, the silicon aluminum carbide material with low aluminum content is obtained;
s5, crushing, ball-milling and shaping the low-aluminum-content silicon carbide aluminum composite material, sieving, and selecting silicon carbide aluminum particles with the particle sizes of 10 microns, 30 microns and 60 microns respectively;
s6, respectively mixing 10-micron, 30-micron and 60-micron silicon aluminum carbide particles according to a mass ratio of 15:20:65, then adding a polyvinyl alcohol solution with the mass ratio of 2%, emulsion wax with the mass ratio of 1% and carbon powder with the mass ratio of 8%, stirring uniformly and sieving for later use;
s7, placing the material prepared in the previous step into a mold, maintaining the pressure for 80S under the pressure of 20MPa, and demolding to obtain a blank;
s8, sintering the presintered body in a vacuum weak reducing atmosphere sintering furnace at the sintering temperature of 600 ℃ in nitrogen and hydrogen, and obtaining a silicon aluminum carbide prefabricated model after sintering;
s9, placing the silicon carbide aluminum prefabricated mold into a mold in a vacuum differential pressure casting furnace, and injecting aluminum alloy molten metal into pores of the silicon carbide aluminum prefabricated mold by a vacuum differential pressure casting method under the protection of inert atmosphere so as to complete interface compounding of ceramic particles and molten metal, wherein in the impregnation process, the temperature of the aluminum alloy solution is controlled to be 720 ℃, and the impregnation pressure is 0.2MPa;
and S10, after cooling, putting the composite material into a heat treatment furnace for annealing treatment to obtain the high-strength aluminum-based silicon carbide composite material.
Example 4
A preparation method of a high-strength silicon carbide reinforced aluminum composite material comprises the following steps:
s1, respectively mixing silicon carbide particles with the particle sizes of 0.25 mu m,0.5 mu m and 0.8 mu m and aluminum powder with the particle size of 5-10 mu m according to the mass ratio of 6:14:65:15, ball milling uniformly under the protection of nitrogen atmosphere;
s2, adding 1.5% of polyvinyl alcohol solution, 1.5% of milk wax and 1.5% of aluminum dihydrogen phosphate solution in mass ratio into the ball-milled materials, uniformly stirring and sieving for later use;
s3, placing the sieved material into a mold, maintaining the pressure for 40S under the pressure of 18MPa, and demolding to obtain a silicon aluminum carbide pre-sintered body;
s4, sintering the presintered body in a vacuum weak reducing atmosphere sintering furnace, wherein the sintering temperature is 650 ℃, the sintering atmosphere is nitrogen and hydrogen, and obtaining the silicon aluminum carbide material with low aluminum content after sintering;
s5, crushing, ball-milling and shaping the low-aluminum-content silicon carbide aluminum composite material, sieving, and selecting silicon carbide aluminum particles with the particle sizes of 10 microns, 30 microns and 60 microns respectively;
s6, respectively mixing 10-micron, 30-micron and 60-micron silicon aluminum carbide particles according to the mass ratio of 12:28:60, adding a polyvinyl alcohol solution accounting for 2.5 percent of the mass ratio, emulsion wax accounting for 1.5 percent of the mass ratio and carbon powder accounting for 6 percent of the mass ratio, stirring uniformly and sieving for later use;
s7, placing the material prepared in the previous step into a mold, maintaining the pressure for 40S under the pressure of 18MPa, and demolding to obtain a blank;
s8, sintering the pre-sintered body in a vacuum weak reducing atmosphere sintering furnace, wherein the sintering temperature is 500 ℃, the sintering atmosphere is nitrogen and hydrogen, and the silicon-aluminum carbide prefabricated model is obtained after sintering is completed;
s9, placing the silicon carbide aluminum prefabricated mold into a mold in a vacuum differential pressure casting furnace, and injecting aluminum alloy molten metal into pores of the silicon carbide aluminum prefabricated mold by a vacuum differential pressure casting method under the protection of inert atmosphere so as to complete interface compounding of ceramic particles and molten metal, wherein in the impregnation process, the temperature of the aluminum alloy solution is controlled to be 700 ℃, and the impregnation pressure is 0.2MPa;
and S10, after cooling, putting the composite material into a heat treatment furnace for annealing treatment to obtain the high-strength aluminum-based silicon carbide composite material.
Example 5
The preparation of example 5 was essentially the same as in example 1, except that the temperature used during impregnation was 700 ℃ and the pressure was 0.3MPa.
Example 6
The preparation method of example 6 is substantially the same as that of example 1 except that the particle sizes selected at the step S5 of the preparation are 20 μm, 40 μm and 80 μm, respectively.
The high-strength silicon aluminum carbide composite material prepared by the embodiment has the advantages that the volume fraction of silicon carbide is 50-70%, the mechanical property is excellent, the bending strength can reach more than 600MPa, the compactness is good, and the air tightness is less than 10 -10 Pa·m 3 And/s, the requirement of high-precision industry is met, the roughness is low after processing, and the post-treatment surface treatment and the related electroplating and chemical plating work are facilitated.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (6)
1. The preparation method of the high-strength silicon aluminum carbide composite material is characterized by comprising the following steps of:
s1, respectively selecting silicon aluminum carbide particles with the particle sizes of 8-12 microns, 20-40 microns and 50-80 microns;
s2, mixing silicon aluminum carbide particles with the particle sizes of 8-12 microns, 20-40 microns and 50-80 microns according to the ratio of 10-20:20-40:30-70, then adding 0.5-3% of adhesive, 0.5-2% of emulsion wax and 0.5-5% of pore-forming agent, stirring uniformly and sieving for later use;
s3, placing the material prepared in the previous step into a mold to prepare a pre-sintered body;
s4, sintering the pre-sintered body in a vacuum weak reducing atmosphere sintering furnace to obtain a silicon-aluminum carbide prefabricated model;
s5, placing the silicon aluminum carbide prefabricated model into a mold in a vacuum differential pressure casting furnace, and injecting an aluminum alloy metal liquid into pores of the silicon aluminum carbide prefabricated model by a vacuum differential pressure casting method to prepare a composite material;
s6, after cooling, putting the composite material into a heat treatment furnace for annealing treatment to obtain a high-strength aluminum-based silicon carbide composite material;
the preparation method of the silicon-aluminum carbide particles comprises the following steps:
s1.1, respectively mixing silicon carbide particles with the particle sizes of 0.1-0.25 mu m, 0.3-0.5 mu m and 0.6-0.8 mu m and aluminum powder with the particle size of 5-10 mu m according to the weight ratio of 5-25:10-35:30-75:5-10, and ball-milling uniformly under the protection of inert gas atmosphere;
s1.2, adding 0.5-3% of adhesive, 0.5-2% of emulsion wax and 0.3-1% of aluminum dihydrogen phosphate into the ball-milled materials, uniformly stirring and sieving for later use;
s1.3, placing the sieved material into a mold, maintaining the pressure for 5-60S under the pressure of 10-20MPa, and demolding to obtain a silicon aluminum carbide pre-sintered body;
s1.4, sintering the presintered body in a vacuum weak reducing atmosphere sintering furnace to obtain a silicon aluminum carbide material with low aluminum content after sintering;
s1.5, crushing, ball-milling and shaping the silicon aluminum carbide composite material, and sieving to obtain silicon aluminum carbide particles.
2. The method of producing a high-strength silicon aluminum carbide composite material according to claim 1, wherein the silicon carbide particles have particle diameters of 0.25 μm,0.5 μm and 0.8 μm, respectively.
3. The method for preparing a high-strength silicon aluminum carbide composite material according to claim 1, wherein in S1.4, the sintering temperature is 500-800 ℃, and the sintering atmosphere is a mixed atmosphere of nitrogen and hydrogen.
4. The method of preparing the high strength silicon aluminum carbide composite material according to claim 1, wherein the binder is selected from one or more of polyvinyl alcohol, polyvinyl acetate, dextrin, paraffin; the pore-forming agent is selected from one or more of starch, carbon powder and ammonium oxalate.
5. The method for preparing a high-strength silicon aluminum carbide composite material according to claim 1, wherein the silicon aluminum carbide particles with the particle diameters of 10 μm, 30 μm and 60 μm are mixed in a mass ratio of 10-20:20-40:30-70, then adding adhesive, emulsion wax and pore-forming agent.
6. A high-strength silicon aluminum carbide composite material, characterized in that the high-strength silicon aluminum carbide composite material is prepared by the preparation method of the high-strength silicon aluminum carbide composite material as claimed in any one of claims 1 to 5, the bending strength of the high-strength silicon aluminum carbide composite material is not less than 600MPa, and the air tightness is less than 10 -10 Pa•m 3 /s。
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