CN115637346A - Al/SiC composite material and preparation method thereof - Google Patents
Al/SiC composite material and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 19
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- 238000000034 method Methods 0.000 claims abstract description 52
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- 238000005245 sintering Methods 0.000 claims abstract description 23
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- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 8
- 229920001568 phenolic resin Polymers 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 8
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000004952 Polyamide Substances 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
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- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 6
- 229920002647 polyamide Polymers 0.000 claims description 6
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- 229910000861 Mg alloy Inorganic materials 0.000 claims description 5
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- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical group C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 4
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
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- CAVCGVPGBKGDTG-UHFFFAOYSA-N alumanylidynemethyl(alumanylidynemethylalumanylidenemethylidene)alumane Chemical compound [Al]#C[Al]=C=[Al]C#[Al] CAVCGVPGBKGDTG-UHFFFAOYSA-N 0.000 description 1
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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Abstract
The invention relates to an Al/SiC composite material and a preparation method thereof. The preparation method comprises the following steps: carrying out high-temperature oxidation on SiC powder with different particle sizes to form SiO on the surface of the SiC powder 2 Oxidizing a film, and then ball-milling and mixing the oxidized film with a binder and a curing agent to obtain ceramic powder; the grain composition of the SiC powder raw material is as follows by mass ratio of 2-6 μm:8-15 μm:18-30 μm:40-60 μm = (0-30): (0 to 30): (0 to 50): (0 to 75); siO for controlling surface formation 2 Oxide film accounts for the total mass of SiC powder0-22.22 wt% of the total volume of the SiC powder, and accounts for 0-29.36 vol% of the total volume of the SiC powder; carrying out laser 3D printing by using the ceramic powder to obtain a silicon carbide molding biscuit; obtaining a SiC prefabricated body through a dewaxing process; and placing an aluminum ingot on the SiC prefabricated body, and sintering to obtain the Al/SiC composite material.
Description
Technical Field
The invention relates to an Al/SiC composite material and a preparation method thereof, in particular to a method for preparing the Al/SiC composite material by pressureless infiltration of aluminum (Al) by using a silicon carbide (SiC) preform, belonging to the technical field of ceramic composite material preparation.
Background
Compared with pure phase silicon carbide (SiC) ceramic, the composite material formed by the multiphase material can be subjected to component cutting design and advantage complementation, and the actual service performance of the material is improved. The SiC reinforced aluminum-based (also called aluminum-based silicon carbide Al/SiC) composite material integrates the respective advantages of SiC and Al, and is a category of metal-based composite materials which are researched more and have more successful industrial application. The composite material has the characteristics of light weight, high specific strength, high specific stiffness, high shear strength and low thermal expansion coefficient, and has good thermal stability, heat conductivity, electrical conductivity, abrasion resistance and wear resistance. Meanwhile, aluminum resources are abundant worldwide. Therefore, the SiC reinforced aluminum matrix composite has wide application value in the fields of national defense, aerospace, automobiles, electronics, sports and the like.
However, how to realize the complicated structure, large size and controllable molding of the Al/SiC composite member and widen the practical application range of the Al/SiC composite member becomes a core problem to be solved urgently. At present, the preparation technology of the Al/SiC composite material mainly comprises a powder metallurgy method, a spray deposition method, a stirring casting method, a pressure infiltration method, a non-pressure infiltration method and the like. Among them, the pressureless infiltration method is one of the most effective methods for producing a composite material having a high volume fraction of a reinforcing phase. The production process comprises the following steps: firstly, a matrix alloy ingot is placed above a prefabricated body, a controllable inert atmosphere is introduced, and the alloy is melted and infiltrated into the SiC prefabricated body by heating. The method can be used for preparing the composite material with the high volume fraction reinforced phase, and has the characteristics of simple process, low cost and near net shape.
The traditional preparation method of the SiC prefabricated body can be mainly subdivided into dry forming and wet forming. The dry forming is suitable for producing the prefabricated body with simple shape, and the near-net forming of a complex structure is difficult to realize; the wet forming can produce preforms with complex shapes, but has the defects of complex process and easy cracking of products. Laser 3D printing (also called selective laser sintering) is an efficient and precise forming means, a local area of layer-spread powder is precisely scanned by strictly controlling a laser beam motion track through a program, a laser is used for generating high-power energy, and deposited light spots are focused on a micro area. In the laser 3D printing process, powder softens and flows under the action of laser beams, and biscuit molding is realized through accurate stacking. The laser 3D printing and forming method has the remarkable advantages of strong structure designability, high material utilization rate, uniform and controllable microstructure, local selective repair and the like, and can completely meet the urgent need of precise manufacturing of complex-configuration Al/SiC composite materials.
Disclosure of Invention
Aiming at the problems, the invention aims to provide an Al/SiC composite material and a preparation method thereof, so as to solve the problem of precise manufacturing of the Al/SiC composite material with large size and complex configuration.
In a first aspect, the present invention provides a method for preparing an Al/SiC composite material, comprising:
carrying out high-temperature oxidation on SiC powder with different particle sizes to form SiO on the surface of the SiC powder 2 Oxidizing a film, and then ball-milling and mixing the oxidized film with a binder and a curing agent to obtain ceramic powder; the SiC powder is selected from at least 2 of four kinds of powder with the median diameter of 2-6 μm, 8-15 μm, 18-30 μm and 40-60 μm; the grain composition of the SiC powder raw material is as follows by mass ratio of 2-6 μm:8-15 μm:18-30 μm:40-60 μm = (0-30): (0 to 30)): (0 to 50): (0 to 75); siO for controlling surface formation 2 The oxide film accounts for 0-22.22 wt% of the total mass of the SiC powder and 0-29.36 vol% of the total volume of the SiC powder;
carrying out laser 3D printing by using the ceramic powder to obtain a silicon carbide molding biscuit; obtaining a SiC prefabricated body through a dewaxing process; and placing an aluminum ingot on the SiC prefabricated body, and sintering to obtain the Al/SiC composite material.
Preferably, the temperature of the high-temperature oxidation is 1000-1400 ℃, and the time is 2-6 h.
Preferably, the binder is selected from thermoplastic resin powder, the thermoplastic resin is preferably at least one of Phenolic Resin (PR), polyvinyl butyral (PVB), polyvinyl alcohol (PVA) or Polyamide (PA) powder, and the phenolic resin powder with the median diameter of 20 μm is more preferred; the curing agent is urotropine.
Preferably, the laser 3D printing process is: adding ceramic powder into Selective Laser Printing (SLP) forming equipment, and preheating to 50-80 ℃, preferably 60 ℃; then, calling a pre-designed CAD model, layering according to the layer thickness of 0.1-0.15 mm, controlling the scanning speed to be 7000-7500 mm/s, the laser power to be 40-50W, and the line spacing to be 0.08-0.5 mm, and carrying out laser 3D printing.
Preferably, the dewaxing process is negative pressure dewaxing; the parameters of the dewaxing process are as follows: heating to 500-600 ℃ at the heating rate of 1-3 ℃/min, and keeping the temperature for 0.2-1 h.
Preferably, the SiC preform has a porosity of 50 to 80% and a density of 0.8 to 1.1g/cm 3 (ii) a The three-point bending strength is 0.3-10 MPa; the average pore diameter is 0.5-50 μm.
Preferably, the aluminum ingot is selected from one of pure aluminum, aluminum-magnesium alloy or aluminum-silicon alloy; the quality of the aluminum ingot is controlled to be 1.5 to 5 times of the quality of the SiC prefabricated body.
Preferably, the sintering atmosphere is argon atmosphere; the sintering temperature is controlled to be 800-1550 ℃, and the heat preservation time is 0.5-4 h.
In a second aspect, the present invention provides an Al/SiC composite material obtained according to the above-described production method.
Advantageous effects
According to the invention, the silicon carbide raw material is subjected to high-temperature pre-oxidation treatment, so that an oxide film is generated on the surface of the silicon carbide raw material, the wettability of the powder and aluminum is improved, and the harmful interface reaction between the aluminum and the silicon carbide is reduced;
the laser 3D printing forming technology is utilized, personalized customization of parts and near-net forming of large complex components can be realized, and the laser 3D printing forming method has the remarkable advantages of strong designability of structure, high utilization rate of materials, uniform and controllable microstructure, local selective repair and the like; meanwhile, the subsequent pressureless infiltration process is combined to obtain the particle reinforced metal matrix composite material with uniform tissue, high density and high strength, so that the urgent requirement of precise manufacturing of the Al/SiC composite material with a complex configuration can be met, and the method has important significance in the fields of national defense, aerospace, automobiles, electronics, sports and the like.
Drawings
FIG. 1 is a cross-sectional micro-topography of a SiC preform prepared in example 1;
FIG. 2 is a fracture micro-topography of the Al/SiC composite prepared in example 1;
FIG. 3 is a fracture micro-topography of the Al/SiC composite material prepared in comparative example 1.
Detailed Description
The present invention is further illustrated by the following examples, which are to be construed as merely illustrative, and not a limitation of the present invention. The invention provides a preparation method of an Al/SiC composite material, which mainly comprises the following steps.
(1) And (3) preparing ceramic powder. Putting SiC powder with different grain diameters into a corundum crucible, and carrying out high-temperature oxidation in an oxygen atmosphere to form SiO on the surface of the SiC powder 2 An oxide film; forming SiO on the surface 2 And carrying out particle grading on the SiC raw material powder of the oxide film, adding the SiC raw material powder, the binder and the curing agent into a ball mill, and carrying out ball milling to obtain uniformly mixed ceramic powder.
In some embodiments, the SiC powder is selected from at least 2 of four powders with a median diameter of 2-6 μm (such as 5 μm), 8-15 μm (such as 10 μm), 18-30 μm (such as 20 μm), 40-60 μm (such as 50 μm); the grain composition of the SiC powder raw material can be that the mass ratio is 2-6 μm:8-15 μm:18-30 μm:40-60 μm = (0-30): (0 to 30): (0 to 50): (0 to 75); preferably, the particle composition may be in a mass ratio of 2-6 μm:18-30 μm:40-60 μm = (0-5): (25-50): (50 to 75), more preferably 5.
The high-temperature oxidation temperature can be 1000-1400 ℃, and the time can be 2-6 h. The temperature of the silicon oxide growth is 1000-1400 ℃, the length of the heat preservation time determines the thickness (or growth amount) of the silicon oxide growth, the longer the oxidation time is, the more the content of the generated silicon oxide is, but the longer the oxidation time is, the silicon oxide grown on the surface falls off, and the coverage of the oxide layer on the surface of the SiC powder is influenced.
In some embodiments, surface-formed SiO may be controlled 2 The oxide film accounts for 0-22.22 wt% of the total mass of the SiC powder and 0-29.36 vol% of the total volume of the SiC powder. SiO 2 2 The oxide film falls off due to too large volume ratio of the oxide film, namely too long oxidation time; siO 2 2 If the volume ratio of the oxide film is too small, that is, if the time for oxidation is too short, the amount of the oxide film formed is insufficient, and the wettability of the biscuit is affected.
The binder may be selected from thermoplastic resin powder, preferably at least one of Phenol Resin (PR), polyvinyl butyral (PVB), polyvinyl alcohol (PVA) or Polyamide (PA) powder, and more preferably phenol resin powder with a median diameter of 20 μm. In alternative embodiments, the amount of binder added may be controlled to provide SiO formation to the surface 2 The total volume of the oxide film SiC raw material powder is 15 to 35vol%, preferably 20 to 30vol%.
The working principle of the Selective Laser Printing (SLP) is as follows: irradiating laser on the printing powder, absorbing heat and melting the binder in the powder, filling pores by mutual flowing, and finally condensing and forming; then, the printing is manufactured layer by layer, and finally the required printing piece is obtained. In the printing process, the binding force among the silicon carbide powder containing the surface oxide layer is insufficient due to too low content of the binding agent, so that the final printed sample is dropped; too high a binder content leads to an increase in porosity after dewaxing of the subsequent green body (later cracking of the binder gives off gas to produce pores). Therefore, the subsequent blank can be well formed only by controlling the reasonable dosage of the binder.
The curing agent can be urotropin. In an alternative embodiment, the curing agent may be added in an amount controlled to 10wt% of the binder content. The curing agent content is too high, so that the curing speed is too high, the heating is out of control, and the product is cracked and even burnt; too little curing agent content can result in incomplete curing of the article.
The ball milling time can be 2-4 h, the rotating speed can be controlled to be 80-120 rpm, the mass ratio of the material balls can be controlled to be 1 (1.2-1.5), and the grinding balls can be silicon carbide balls.
(2) And preparing a SiC prefabricated body. Adding the uniformly mixed ceramic powder obtained in the step (1) into a laser 3D printer, setting printing parameters matched with a target printing material, and printing and molding according to a target model to obtain a silicon carbide molding biscuit; and obtaining the SiC prefabricated body through a dewaxing process.
In an alternative embodiment, the ceramic powder can be added into an SLP (selective laser printing) molding device and preheated to 50 to 80 ℃, preferably 60 ℃; then, calling a pre-designed CAD model, layering according to the layer thickness of 0.1-0.15 mm, controlling the scanning speed to be 7000-7500 mm/s, the laser power to be 40-50W and the line spacing to be 0.08-0.5 mm, and carrying out laser 3D printing to obtain the silicon carbide SLP forming biscuit.
In the laser printing and forming process, the irradiation energy of laser on the powder surface is in direct proportion to the laser power and in inverse proportion to the beam radius and the scanning speed. The ratio of the laser power to the laser spot area is the laser power density, which directly influences the sintering temperature, and the sintering temperature and the printing quality have decisive influence. On the premise that the beam radius and the spot area of the equipment are fixed, due to the fact that different binders are different in sintering temperature, the high precision, the low porosity, the high density and the like of a printed sample can be guaranteed by controlling appropriate printing parameters, and the comprehensive performance is excellent.
Wherein the dewaxing process can be negative pressure dewaxing; the dewaxing process parameters may be: heating to 500-600 ℃ at the heating rate of 1-3 ℃/min, and keeping the temperature for 0.2-1 h. Through the dewaxing process, the gas and the volatile components of the organic matters (such as the binder) in the printed matter can be released through pyrolysis, and through controlling the appropriate heating rate, dewaxing temperature and heat preservation time, the defects that the silicon carbide forming biscuit cannot crack and the like when the gas and the volatile components are released through pyrolysis of different organic matters can be ensured.
The porosity of the SiC preform is 50-80% and the density is 0.8-1.1 g/cm by adopting an Archimedes drainage method for testing 3 (ii) a The bending strength of the ceramic material is adopted for testing, and the three-point bending strength of the obtained SiC prefabricated body is 0.3-10 MPa; the average pore size distribution of the obtained SiC prefabricated body is concentrated between 0.5 and 50 mu m by mercury intrusion method test. The pores of the preform can be filled with liquid metal in the sintering process, and the full infiltration of different types of aluminum ingots can be ensured by controlling the porosity (50-80%) of the preform, so that the aluminum-based composite material with high silicon carbide volume fraction is finally obtained. Meanwhile, when high-temperature metal liquid is infiltrated, the prefabricated body can bear certain thermal stress, the prefabricated body can crack in the infiltration process due to too low strength, and the structural integrity in the aluminizing process and the successful preparation of the final composite material can be guaranteed by controlling certain bending strength of the prefabricated body. The pore channels in the preform are channels for the molten metal to flow through, the average pore diameter of the preform is controlled within a proper range, so that the preform can suck the liquid metal into the preform through capillary force, and the penetration of the liquid metal is promoted.
(3) And preparing the Al/SiC composite material. Placing the SiC preform obtained in the step (2) in a graphite crucible, and placing an aluminum ingot with a certain mass on the SiC preform; and sintering to obtain the Al/SiC composite material.
In an alternative embodiment, the aluminum ingot may be selected from one of pure aluminum, aluminum magnesium alloy, or aluminum silicon alloy. When the aluminum ingot is pure aluminum, a preform with lower porosity can be selected so as to improve the volume fraction of the silicon carbide; when the aluminum ingot is aluminum-silicon alloy, since silicon can react with carbon in the preform to produce silicon carbide, the preform with higher porosity can be selected to obtain aluminum silicon carbide with higher volume fraction of silicon carbide. Meanwhile, aluminum-magnesium alloy is selected as the aluminum ingot, and magnesium can react with silicon oxide to promote the reaction in the infiltration process, thereby being beneficial to sintering. The mass of the aluminum ingot can be controlled to be 1.5 to 5 times of that of the SiC prefabricated body.
The sintering atmosphere can be argon atmosphere; the sintering temperature can be controlled to be 800-1550 ℃, and the heat preservation time is 0.5-4 h. The sintering temperature is too high, so that aluminum can volatilize, and meanwhile, the aluminum and the silicon carbide are subjected to an erosion reaction to generate aluminum carbide and other impurity phases; the sintering temperature is too low, the viscosity of the molten metal is high, and the infiltration is influenced. Meanwhile, incomplete reaction can be caused by too short heat preservation time; too long a holding time will result in energy waste.
The Al/SiC composite material obtained by the preparation method provided by the invention comprises an Al phase and a SiC phase, wherein the Al phase comprises a pure aluminum phase or an aluminum-magnesium alloy phase or an aluminum-silicon alloy phase. The porosity of the Al/SiC composite material is 0-4%, and the density is less than 3.0g/cm 3 The bending strength is 200-300 MPa.
According to the invention, the silicon carbide powder is subjected to high-temperature pre-oxidation treatment to generate an oxide film on the surface of the silicon carbide powder, so that the wettability of the raw material powder and an aluminum ingot is improved, and the harmful interface reaction between aluminum and silicon carbide is reduced. In addition, compared with the traditional SiC preform forming method, powder metallurgy and other methods, the laser 3D printing technology is adopted, the computer CAD component model is used for slicing, layer-by-layer printing and forming, biscuit forming can be achieved through accurate powder laying and stacking without a mold and additional support, and meanwhile personalized customization and near net forming of large complex configurations can be achieved. The laser 3D printing and forming method has the remarkable advantages of strong structural designability, high material utilization rate, easiness in reliably manufacturing complex structural parts in situ, uniformity and controllability of microstructures, local selective repair and the like, realizes densification by combining a pressureless infiltration process, and can meet the urgent requirement of precise manufacturing of complex-configuration Al/SiC composite materials.
The present invention will be described in detail by way of examples. It should also be understood that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adjustments made by those skilled in the art in light of the above disclosure are within the scope of the present invention, and that the specific process parameters and the like described in the following examples are only examples of suitable ranges, i.e., those skilled in the art can select from the suitable ranges described herein, and are not intended to be limited to the specific values listed below.
Example 1
(1) And (3) preparing ceramic powder. 2688g of SiC powder with the median diameter of 50um and 1152g of SiC powder with the median diameter of 10um are respectively placed in different corundum crucibles and oxidized for 4 hours at 1200 ℃ in an oxygen atmosphere, so that SiO is formed on the surface of the SiC powder 2 Oxide film, siO formed on the surface 2 The oxide film accounts for 16.98wt% of the total mass of the SiC powder and accounts for 20.73vol% of the total volume of the SiC powder. Uniformly mixing oxidized SiC powder (4070.4 g in total), adding the mixed powder into a ball mill, adding 488g (25 vol%) of phenolic resin powder with a median diameter of 20um and 48.8g of urotropine into the ball mill, and carrying out ball milling for 2 hours at a rotating speed of 88 revolutions per minute, wherein the mass ratio of material balls is controlled to be 1.5, so as to obtain uniformly mixed ceramic powder.
(2) And preparing a SiC prefabricated body. And (2) adding the uniformly mixed ceramic powder obtained in the step (1) into a laser 3D printer, setting the preheating temperature to be 60 ℃, the layer thickness to be 0.1mm, the scanning speed to be 7260mm/s, the laser power to be 45W and the line spacing to be 0.08mm, and printing and forming according to a target model. And (4) carrying out negative pressure dewaxing at the temperature of 600 ℃ for 0.5h to obtain the SiC preform. The mass of the SiC preform was 2.23g. The porosity of the SiC preform is 67.01% and the density is 1.02g/cm by adopting an Archimedes drainage method for testing 3 (ii) a The average pore diameter of the obtained SiC preform was 5.97um by mercury intrusion test. The SiC preform obtained was processed into a bar having dimensions of 4 mm. Times.3 mm. Times.36 mm, and the three-point bending strength was measured, the strength being 3.77. + -. 0.37MPa.
(3) And preparing the Al/SiC composite material. And placing the obtained SiC preform in a graphite crucible, placing 4.46g of pure aluminum ingot on the SiC preform, sintering in a pressureless sintering furnace in the atmosphere of argon at the maximum sintering temperature of 1000 ℃, and preserving heat for 1h to prepare the Al/SiC composite material.
The porosity of the prepared Al/SiC composite material is 2.93 percent and the density is 2.64g/cm measured by an Archimedes drainage method 3 . The obtained Al/SiC composite material is processed into a test strip with the size of 4mm multiplied by 3mm multiplied by 36mm, and the three-point bending strength is tested, wherein the bending strength is 232.7 +/-4.7 MPa.
FIG. 1 is a sectional micro-topography of the SiC preform prepared in example 1. As can be seen from the figure, the preform exhibits a porous structure with connected channels (liquid phase infiltration passages), which facilitates the infiltration reaction.
FIG. 2 is a fracture micro-topography of the Al/SiC composite prepared in example 1. As can be seen from the figure, the silicon carbide phase and the aluminum phase are dispersed and distributed, and the fracture is mainly plastic fracture.
Example 2
(1) And (3) preparing ceramic powder. Refer to the preparation scheme in example 1.
(2) And preparing a SiC prefabricated body. And (2) adding the uniformly mixed ceramic powder obtained in the step (1) into a laser 3D printer, setting the preheating temperature to be 60 ℃, the layer thickness to be 0.1mm, the scanning speed to be 7260mm/s, the laser power to be 45W and the line spacing to be 0.08mm, and printing and forming according to a target model. And (4) carrying out heat preservation at 600 ℃ for 0.5h and negative pressure dewaxing to obtain the SiC preform. The mass of the SiC preform was 2.08g. The porosity of the SiC preform is 66.67 percent and the density is 1.03g/cm by adopting the Archimedes drainage method for testing 3 (ii) a The average pore diameter of the obtained SiC preform was 5.54um as measured by mercury intrusion method. The SiC preform obtained was processed into a test bar having dimensions of 4 mm. Times.3 mm. Times.36 mm, and the three-point bending strength was measured, the strength being 4.13. + -. 0.41MPa.
(3) And preparing the Al/SiC composite material. And placing the obtained SiC preform in a graphite crucible, placing 4.16g of aluminum magnesium 20 alloy ingot on the SiC preform, sintering in a pressureless sintering furnace in the atmosphere of argon at the maximum sintering temperature of 800 ℃, and preserving heat for 1h to prepare the Al/SiC composite material.
Measured by an Archimedes drainage method, the prepared Al/SiC composite material has the porosity of 1.47 percent and the density of 2.69g/cm 3 . The obtained Al/SiC composite material is processed into a product with the size of 4mmThe three-point bending strength of the test strip with the thickness of 3mm multiplied by 36mm is tested, and the bending strength is 227.4 +/-6.2 MPa.
Example 3
(1) And (3) preparing ceramic powder. Refer to the preparation scheme in example 1.
(2) And preparing a SiC prefabricated body. And (2) adding the uniformly mixed ceramic powder obtained in the step (1) into a laser 3D printer, setting the preheating temperature to be 60 ℃, the layer thickness to be 0.1mm, the scanning speed to be 7260mm/s, the laser power to be 45W and the line spacing to be 0.08mm, and printing and forming according to a target model. And (4) carrying out heat preservation at 600 ℃ for 0.5h and negative pressure dewaxing to obtain the SiC preform. The mass of the SiC preform was 2.14g. The porosity of the SiC preform is 66.93 percent and the density is 1.03g/cm by adopting the Archimedes drainage method for testing 3 (ii) a The average pore diameter of the obtained SiC preform was 5.61um as measured by mercury intrusion method. The SiC preform obtained was processed into a test bar having dimensions of 4mm × 3mm × 36mm, and the three-point bending strength was measured, the strength being 4.02 ± 0.28MPa.
(3) And preparing the Al/SiC composite material. And placing the obtained SiC prefabricated body in a graphite crucible, placing 4.28g of aluminum-silicon 12 alloy on the SiC prefabricated body, sintering in a pressureless sintering furnace in the atmosphere of argon at the maximum sintering temperature of 1500 ℃, and preserving heat for 1h to prepare the Al/SiC composite material.
The porosity of the prepared Al/SiC composite material is 1.22 percent and the density is 2.74g/cm measured by an Archimedes drainage method 3 . The obtained Al/SiC composite material is processed into a test strip with the size of 4mm multiplied by 3mm multiplied by 36mm, and the three-point bending strength is tested, wherein the bending strength is 214.2 +/-4.4 MPa.
Comparative example 1
Refer to the preparation scheme in example 1. The main differences are that: in the step (1), the SiC powder is oxidized for 8 hours at 1200 ℃. Because the oxidation time is too long, an oxide layer on the surface of the SiC is peeled off, the porosity of the obtained Al/SiC composite material is 6.8%, and the bending strength is only 89.7 +/-6.8 MPa.
FIG. 3 is a fracture micro-topography of the Al/SiC composite material prepared in comparative example 1. As can be seen, a large number of pores are present in the composite material, mainly due to the fact that the oxide layer is peeled off to expose the silicon carbide, and the wettability of the silicon carbide and the aluminum ingot is affected.
Comparative example 2
Refer to the preparation scheme in example 1. The main differences are that: in the step (1), the SiC powder is not subjected to oxidation treatment.
The preform formed by the SiC powder without the oxide layer is difficult to infiltrate Al, and finally the Al/SiC composite material meeting the performance requirements cannot be obtained.
While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention. Various modifications and alterations to this invention will become apparent to those skilled in the art upon reading the foregoing description. Accordingly, the scope of the invention should be limited only by the attached claims.
Claims (9)
1. A preparation method of an Al/SiC composite material is characterized by comprising the following steps:
carrying out high-temperature oxidation on SiC powder with different particle sizes to form SiO on the surface of the SiC powder 2 Oxidizing a film, and then ball-milling and mixing the oxidized film with a binder and a curing agent to obtain ceramic powder; the SiC powder is selected from at least 2 of four kinds of powder with the median diameter of 2-6 μm, 8-15 μm, 18-30 μm and 40-60 μm; the grain composition of the SiC powder raw material is as follows by mass ratio of 2-6 μm:8-15 μm:18-30 μm:40-60 μm = (0-30): (0 to 30): (0 to 50): (0 to 75); siO for controlling surface formation 2 The oxide film accounts for 0-22.22 wt% of the total mass of the SiC powder and 0-29.36 vol% of the total volume of the SiC powder;
carrying out laser 3D printing by using the ceramic powder to obtain a silicon carbide molding biscuit; obtaining a SiC prefabricated body through a dewaxing process; and placing an aluminum ingot on the SiC prefabricated body, and sintering to obtain the Al/SiC composite material.
2. The preparation method according to claim 1, wherein the high-temperature oxidation temperature is 1000-1400 ℃ and the time is 2-6 h.
3. The preparation method of claim 1 or 2, wherein the binder is selected from thermoplastic resin powder, the thermoplastic resin is preferably at least one of Phenolic Resin (PR), polyvinyl butyral (PVB), polyvinyl alcohol (PVA) or Polyamide (PA) powder, and is more preferably phenolic resin powder with a median diameter of 20 μm; the curing agent is urotropin.
4. The method for preparing according to any one of claims 1 to 3, wherein the laser 3D printing process is: adding ceramic powder into Selective Laser Printing (SLP) forming equipment, and preheating to 50-80 ℃, preferably 60 ℃; then, calling a pre-designed CAD model, layering according to the layer thickness of 0.1-0.15 mm, controlling the scanning speed to be 7000-7500 mm/s, the laser power to be 40-50W and the line spacing to be 0.08-0.5 mm, and carrying out laser 3D printing.
5. The production method according to any one of claims 1 to 4, wherein the dewaxing process is negative pressure dewaxing; the parameters of the dewaxing process are as follows: heating to 500-600 ℃ at the heating rate of 1-3 ℃/min, and keeping the temperature for 0.2-1 h.
6. The production method according to any one of claims 1 to 5, wherein the SiC preform has a porosity of 50 to 80% and a density of 0.8 to 1.1g/cm 3 (ii) a The three-point bending strength is 0.3-10 MPa; the average pore diameter is 0.5-50 μm.
7. The production method according to any one of claims 1 to 6, wherein the aluminum ingot is selected from one of pure aluminum, an aluminum-magnesium alloy, or an aluminum-silicon alloy; the quality of the aluminum ingot is controlled to be 1.5 to 5 times of the quality of the SiC prefabricated body.
8. The production method according to any one of claims 1 to 7, wherein the atmosphere for sintering is an argon atmosphere; the sintering temperature is controlled to be 800-1550 ℃, and the heat preservation time is 0.5-4 h.
9. An Al/SiC composite material obtained by the production method according to any one of claims 1 to 8.
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