CN114525434A - SiC-induced multiphase reinforced aluminum matrix composite material and preparation method thereof - Google Patents
SiC-induced multiphase reinforced aluminum matrix composite material and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C21/00—Alloys based on aluminium
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- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/20—Direct sintering or melting
- B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B33Y70/00—Materials specially adapted for additive manufacturing
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- C22C1/00—Making non-ferrous alloys
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- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
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Abstract
The invention belongs to the technical field of additive manufacturing, and relates to a SiC-induced multiphase reinforced aluminum matrix composite material and a preparation method thereof. The preparation method comprises the step of carrying out preoxidation treatment on the surface of SiC particles to form SiO2The oxide layer improves the interface wettability between SiC and Al matrix, delays the reaction between SiC particles and the Al matrix, and SiO is formed at high temperature2Will react preferentially with the matrix to form only a small amount of Al2O3Particles of SiThe C particles are substantially retained. In the local high temperature area, the reaction can occur, SiC particles at the local high temperature area can be completely consumed, and Al is generated4SiC4A hard ceramic phase. The multiphase reinforced aluminum matrix composite with uniform nano-particle dispersion, high density, fine crystal grains and excellent mechanical property is successfully prepared by a method combining pre-oxidation, pre-dispersion and selective laser melting, and the problem of poor plasticity and toughness of the printed SiC reinforced aluminum matrix composite is effectively solved.
Description
Technical Field
The invention belongs to the technical field of additive manufacturing, relates to an aluminum matrix composite, and particularly relates to a SiC-induced multiphase reinforced aluminum matrix composite and a preparation method thereof.
Background
With the rapid development of modern science and technology, light-weight and high-strength Aluminum-based composite materials (AMCs) show wide application prospects in the fields of aerospace, automobile light weight and the like, and therefore, people attract extensive attention and research. For example, the prior art has been developed by adding some reinforcing phases (such as SiC, CNTs, TiC, TiB) with excellent properties2、Al2O3AlN, etc.) is favorable for realizing the improvement of the comprehensive mechanical property of the pure aluminum/aluminum alloy. Among them, SiC particles are considered to be an ideal reinforcing phase for preparing AMCs because of their advantages of low density, high hardness (about 25 GPa), high elastic modulus (about 410 GPa), stable chemical properties, and low cost. However, in the conventional processes (such as the stir casting method, the melt infiltration method, the particle metallurgy method, etc.) for preparing AMCs, it is inevitable that particles of the reinforcing phase are difficult to uniformly disperse, wettability between the matrix and the reinforcing particles is poor, and boundaries are poorSurface bonding is weak and Al is easily generated4C3Brittleness, etc., making it difficult to effectively exert the reinforcing effect of SiC in AMCs. Meanwhile, due to the limitation of the die and the processing method, the application of SiC enhanced AMCs in parts with complex shapes is obviously restricted.
Selective Laser Melting (SLM) is a new process for integrally forming complex-shaped, high-performance AMCs due to its extremely high melting/solidification rate (about 10) during the forming process3~106DEG C/s) is beneficial to realizing the uniform dispersion of the reinforcing phase and refining grains, and the method has unique advantages for preparing AMCs with excellent performance and complex structure. Therefore, the preparation of the composite particles with uniformly distributed nano particles and suitable for the laser melting of the particle bed is still the key to obtain the aluminum-based composite material with refined grains and excellent performance.
However, in the process of preparing the composite material by adopting the external addition method, how to uniformly disperse the nano particles with larger specific surface energy on the matrix particles is a great problem which is always puzzled for researchers. Meanwhile, the contact angle between SiC and Al liquid is larger than 90 degrees below 1173K, the SiC and the Al liquid are not wetted, and a gas layer is attached to the surface when the SiC is added, so that the difficulty of compounding the SiC and the Al matrix in the forming process is increased, the compatibility between an enhanced phase and the matrix is poor, a formed sample contains more pores, and the density is not high. In addition, at a relatively low forming temperature (940-4C3(s) +3Si forms a brittle phase Al which is easily hydrolyzed4C3. The factors can cause the plasticity and toughness of the AMCs to be remarkably reduced, and the material performance is difficult to meet the application requirement.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a SiC-induced multiphase reinforced aluminum matrix composite and a preparation method thereof, and the multiphase reinforced aluminum matrix composite with uniformly dispersed nano particles, high density, fine crystal grains and excellent mechanical property is prepared by using a method combining pre-oxidation, pre-dispersion and selective laser melting.
In order to achieve the purpose, the invention provides the following technical scheme:
on one hand, the invention provides a SiC-induced multiphase reinforced aluminum-based composite material, raw material powder consists of nano SiC powder and AlSi10Mg powder, and a reinforced phase comprises additional nano SiC particles and Al generated by in-situ reaction2O3、Al4SiC4And (3) granules.
Further, the mass percent of the nano SiC powder in the raw material powder is 2-10%, and the mass percent of the AlSi10Mg powder is 90-98%; the grain size of the nano SiC powder is 40-100 nm, the grain size of the AlSi10Mg powder is 45-106 mu m, and the grain size of an Al matrix in the multiphase reinforced aluminum matrix composite material is 400-600 nm.
On the other hand, the invention provides a preparation method of the SiC-induced multiphase reinforced aluminum-based composite material, namely, pre-dispersing the pre-oxidized nano SiC particles to obtain SiCOXSuspending the solution, and mixing the SiCOXBall milling and mixing the suspension and AlSi10Mg particles to obtain SiCOXthe/AlSi 10Mg composite powder is finally prepared into the multiphase reinforced aluminum-based composite material through a selective laser melting forming process.
Further, the preparation method specifically comprises the following steps:
1) uniformly spreading the nano SiC particles, placing the nano SiC particles in a heat treatment furnace, carrying out pre-oxidation treatment in an air atmosphere, keeping the pre-oxidation temperature at 800-1200 ℃, and cooling the nano SiC particles to room temperature along with the furnace after heat preservation for 2-6 hours;
2) pre-oxidized nano SiCOXAdding the particles and a dispersing agent into an absolute ethyl alcohol solution, and obtaining SiC by mechanical stirring and ultrasonic dispersionOXSuspending liquid; the mass of the dispersing agent is nano SiCOXThe mass of the particles is 0.5% -20%;
3) mixing AlSi10Mg particles with the SiCOXAdding the suspension into a ball milling tank together for planetary ball milling dispersion;
4) screening the composite particles obtained by ball milling and dispersing in the step 3), and preparing the multiphase reinforced aluminum matrix composite material by a selective laser melting forming process.
Further, before the nano SiC particles are subjected to pre-oxidation treatment in the step 1), the nano SiC particles are firstly placed in an organic solvent for ultrasonic cleaning for 0.5-1 h, then are cleaned twice by distilled water, and are dried at the temperature of 60-80 ℃.
Further, the pre-oxidation treatment in the step 1) adopts a sectional heating process: firstly, heating to 300 ℃ at a heating rate of 5-15 ℃/min, and keeping the temperature for 15-60 min; and then heating to 600 ℃ at the heating rate of 5-15 ℃/min, preserving the heat for 15-60 min, and then heating to the pre-oxidation temperature and preserving the heat for 2-6 h.
Further, the rotating speed of mechanical stirring in the step 2) is 50-150 r/min, and the time of mechanical stirring and ultrasonic dispersion is 0.5-1 h.
Further, the ball milling tank in the step 3) adopts argon protection in the ball milling process, and the ball-to-material ratio is (1-2): 1, the ball milling speed is 50-150 r/min, and the ball milling time is 2-6 h.
Further, the screening in the step 4) specifically comprises:
drying the particles subjected to ball milling dispersion in the step 3) in a vacuum drying oven at the drying temperature of 80 ℃ for 6-12 h;
followed by sieving with a 150 mesh sieve.
Further, the selected area laser melting forming process in the step 4) is carried out in an argon atmosphere, and the argon pressure is not higher than 10 bar; the parameters of the selective laser melting forming process are as follows: the scanning speed is 800-1600 mm/s, and the laser power is 280-350W.
Compared with the prior art, the technical scheme provided by the invention has the following beneficial effects: the multiphase reinforced aluminum matrix composite material with uniform nano-particle dispersion, high density, fine crystal grains and excellent mechanical property is prepared by a method combining pre-oxidation, pre-dispersion and selective laser melting. SiO is formed after the surface of the nano SiC particles is subjected to pre-oxidation treatment2On one hand, the oxide layer effectively improves the interface wettability between SiC and Al matrix, and obviously improves the density of the composite material; on the other hand, the SiO2The oxide layer significantly delays the reaction between the SiC particles and the Al matrix, which preferentially reacts with the matrix at high temperatures: al + SiO2→Al2O3+ Si, since the higher Si content in the Al-Si alloy inhibits the forward progress of this reaction, only a small amount of Al is formed2O3Particles, SiC particles are substantially retained. In the local region of excessive temperature (>1670K) Then the reaction will take place: 4Al (l) +4SiC(s) → Al4SiC4(s) +3Si, complete consumption of SiC particles at the site, Al formation4SiC4A hard ceramic phase. Reaction product (Al) generated by in situ reaction2O3And Al4SiC4) The SiC reinforced aluminum matrix composite material can be used as a new reinforced phase and the original reinforced phase SiC to be pinned at a crystal boundary together, the effect of blocking dislocation movement is effectively achieved, the obtained composite material is guaranteed to have good strong plasticity proportion, the mechanical property of the composite material is remarkably improved, and the problem that the printed SiC reinforced aluminum matrix composite material is poor in plasticity and toughness is effectively solved.
In addition, SiO can be regulated and controlled by changing pre-oxidation and selective laser melting forming parameters2The thickness and the in-situ reaction degree of the layer effectively realize the controllable preparation of the multiphase reinforced aluminum-based composite material with uniformly dispersed nano particles, and the method has the advantages of low cost, good controllability, simple operation and the like.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description, serve to explain the principles of the invention.
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without inventive exercise.
FIG. 1 is a schematic flow chart of a method for preparing a SiC-induced multiphase reinforced aluminum matrix composite material according to the present invention;
FIG. 2 is a graph of the relationship between pre-oxidation temperature and time according to the present invention;
FIG. 3 is a graph showing changes of wetting angles theta of SiC particles with an Al matrix before and after pre-oxidation treatment;
FIG. 4 is a TEM bright field image of a SiC-induced multiphase reinforced aluminum matrix composite provided by the present invention;
FIG. 5 is a schematic structural diagram of a SiC-induced multiphase reinforced aluminum matrix composite provided by the invention.
Detailed Description
Reference will now be made in detail to the exemplary embodiments, examples of which are illustrated in the accompanying drawings. When the following description refers to the accompanying drawings, like numbers in different drawings represent the same or similar elements unless otherwise indicated. The embodiments described in the following exemplary embodiments do not represent all embodiments consistent with the present invention. Rather, they are merely examples of products, methods consistent with certain aspects of the invention, as detailed in the appended claims.
Referring to fig. 1, the invention provides a preparation method of a multiphase reinforced aluminum matrix composite, which is implemented according to the following steps:
weighing raw materials, and cleaning nano SiC particles;
weighing nano SiC and AlSi10Mg powder raw materials in corresponding weight according to mass percentage, placing the SiC powder in an acetone solution for ultrasonic cleaning for 0.5-1 h to remove surface stains and gas adsorption, then cleaning twice with distilled water, and drying at 60-80 ℃.
The mass percentage of the nano SiC powder is 2-10%, the mass ratio of the AlSi10Mg powder is 90-98%, and the sum of the mass percentages of the powder raw materials is 100%. The grain size of the nano SiC powder is 40-100 nm, the grain size of the AlSi10Mg powder is 45-106 microns, and the grain size of an Al matrix in the prepared composite material is 400-600 nm.
Secondly, carrying out pre-oxidation treatment on the nano SiC powder;
flatly spreading the cleaned nano SiC powder in a quartz crucible, placing the quartz crucible in a heat treatment furnace, and carrying out pre-oxidation treatment in an air atmosphere; in order to prevent the SiC powder from agglomerating at high temperature, the pre-oxidation treatment adopts a sectional type heating process: firstly, heating to 300 ℃ at a heating rate of 5-15 ℃, and preserving heat for 15-60 min; then heating to 60 ℃ at a heating rate of 5-15 ℃/minKeeping the temperature at 0 ℃ for 15-60 min, then heating to a preset oxidation temperature (800-1200 ℃), keeping the temperature for 2-6 h, and cooling to room temperature along with the furnace; the pre-oxidation heating process is shown in FIG. 2, and the SiO obtained after the pre-oxidation treatment2The theoretical thickness of the layer is 2-15 nm.
Step three, to SiCOXPerforming pre-dispersion treatment on the powder;
pre-oxidized nano SiCOXAdding the powder and polyvinylpyrrolidone (PVP) into 500ml of absolute ethyl alcohol solution, and obtaining SiC by mechanical stirring and ultrasonic dispersionOXThe suspension liquid, wherein the mechanical stirring rotating speed is 50-150 r/min, and the mass of the dispersing agent with the mechanical stirring and ultrasonic dispersion time of 0.5-1 h is nano SiCOX0.5-20% of the powder mass.
Step four, preparing SiCOXa/AlSi 10Mg composite powder;
mixing AlSi10Mg powder with the above SiCOXAdding the turbid liquid into a ball milling tank filled with zirconia grinding balls together, and carrying out low-energy planetary ball milling; argon is adopted for protection in the ball milling process, and the ball material ratio is (1-2): 1, the ball milling speed is 50-150 rpm, the ball milling time is 2-6 h, and the ball milling process stops for 10min every 25min of positive rotation and then reverses for 25min so as to prevent the powder from overheating.
Step five, preparing SiCOXa/AlSi 10Mg composite;
drying the ball-milled and dispersed particles in a vacuum drying oven at the drying temperature of 80 ℃ for 6-12 h, and then screening by using a 150-mesh screen to obtain SiC which is uniformly dispersed and suitable for powder bed laser meltingOXa/AlSi 10Mg composite powder; then, at SLM 280HLPerforming selective laser melting forming on equipment, performing sand blasting treatment on the surface of a substrate before forming, preheating to 150 ℃, wherein the oxygen content in a forming cavity is not higher than 100ppm, and the whole process adopts argon protection, and the argon pressure is not higher than 10 bar; the adopted selective laser melting process parameters are as follows: the thickness of the powder spreading layer is 30 mu m, the distance between scanning lines is 80 mu m, the scanning speed is 800-1600 mm/s, and the laser power is 280-350W.
The SiC-induced multi-phase reinforced aluminum matrix composite with uniformly dispersed nano particles can be prepared by the stepsA material. As can be seen from FIG. 3, the wettability of the interface between the reinforcing phase and the matrix is significantly improved, and the formed sample has a dense tissue (see FIG. 4), and the density of the formed sample can reach up to 99.7%. As can be seen from the microstructure diagram (fig. 5), the added SiC nanoparticles and the reaction in situ: al + SiO2→Al2O3+Si、4Al(l)+4SiC(s)→Al4SiC4New reinforcing phase (Al) formed by(s) +3Si2O3、Al4SiC4) The crystal grains are uniformly distributed on the crystal boundary, so that the effects of pinning the crystal boundary and blocking dislocation motion can be effectively achieved, and the size of the matrix crystal grains in the composite material is about 400-600 nm. Due to the synergistic effect of fine crystal strengthening and dislocation strengthening, compared with a printed SiC reinforced aluminum matrix composite, the composite has better tensile property and elongation at break.
In addition, the invention also provides a SiC-induced multiphase reinforced aluminum matrix composite material prepared by applying the preparation method, wherein the reinforcing phase of the aluminum matrix composite material is prepared by adding SiC particles and Al generated by in-situ reaction2O3、Al4SiC4And (4) particle composition.
Wherein, the specific components of the AlSi10Mg powder raw material are shown in the following table 1:
TABLE 1 AlSi10Mg powder chemistry (wt.%)
In order to make those skilled in the art better understand the technical solutions of the present invention, the present invention is further described in detail below with reference to the accompanying drawings and examples.
Example 1
The embodiment provides a preparation method of a SiC-induced multiphase reinforced aluminum matrix composite material with uniformly dispersed nano particles, which specifically comprises the following steps:
step one, weighing 2% of nano SiC powder and 98% of AlSi10Mg powder as raw materials according to mass percentage, then placing the SiC powder in an acetone solution for ultrasonic cleaning for 0.5h to remove surface stains and gas adsorption, then cleaning twice with distilled water, and drying at 80 ℃.
And step two, spreading the cleaned SiC powder in a quartz crucible, placing the quartz crucible in a heat treatment furnace, and carrying out pre-oxidation treatment in an air atmosphere. In order to prevent the SiC powder from agglomerating at high temperature, the pre-oxidation treatment adopts a sectional type heating process: firstly, heating to 300 ℃ at a heating rate of 5-15 ℃ and preserving heat for 15 min; heating to 600 ℃ at the heating rate of 5-15 ℃/min, preserving heat for 15min, then heating to the preset oxidation temperature of 800 ℃, preserving heat for 2h, and cooling to room temperature along with the furnace; the heating process of pre-oxidation is shown in FIG. 2, and the SiO obtained after pre-oxidation2The theoretical thickness of the layer is 2 nm.
Step three, pre-oxidized nano SiCOXAdding the powder and 0.5% of polyvinylpyrrolidone (PVP) by mass into 500ml of absolute ethyl alcohol solution, and performing mechanical stirring and ultrasonic dispersion to obtain a SiC suspension, wherein the mechanical stirring speed is 50r/min, and the mechanical stirring and ultrasonic dispersion time is 0.5 h.
Adding AlSi10Mg powder and the SiC suspension into a ball milling tank filled with zirconia grinding balls together, and carrying out low-energy planetary ball milling; argon is adopted for protection in the ball milling process, the ball material ratio is 1:1, the ball milling rotation speed is 50r/min, the ball milling time is 2 hours, and the ball milling process stops 15min for every 25min of positive rotation and then reverses 25min to prevent powder overheating.
Step five, drying the composite powder subjected to ball milling dispersion in the step four in a vacuum drying oven at the drying temperature of 80 ℃ for 6 hours, screening by using a 150-mesh screen, and then performing selective laser melting forming under the following parameters: the layer thickness of the powder coating is 30 μm, the scanning line spacing is 80 μm, the scanning speed is 800mm/s, and the laser power is 280W. The SiC-induced multiphase reinforced aluminum matrix composite (I) with uniformly dispersed nano particles is obtained through the steps.
Example 2
The embodiment provides a preparation method of a SiC-induced multiphase reinforced aluminum matrix composite material with uniformly dispersed nano particles, which specifically comprises the following steps:
weighing 6% of nano SiC and 94% of AlSi10Mg powder raw materials according to mass percentage, then placing the SiC powder in an acetone solution for ultrasonic cleaning for 0.8h to remove surface stains and gas adsorption, then cleaning twice with distilled water, and drying at 60 ℃.
And step two, spreading the cleaned SiC powder in a quartz crucible, placing the quartz crucible in a heat treatment furnace, and carrying out pre-oxidation treatment in an air atmosphere. In order to prevent the SiC powder from agglomerating at high temperature, a sectional heating process is adopted: firstly, heating to 300 ℃ at a heating rate of 5-15 ℃ and preserving heat for 45 min; heating to 600 ℃ at the heating rate of 5-15 ℃/min, preserving heat for 45min, then heating to the preset oxidation temperature of 1000 ℃, preserving heat for 4h, and cooling to room temperature along with the furnace; the heating process of pre-oxidation is shown in FIG. 2, and the SiO obtained after pre-oxidation2The theoretical thickness of the layer is 9 nm.
Step three, pre-oxidized nano SiCOXAdding the powder and 0.5% of polyvinylpyrrolidone (PVP) by mass into 500ml of absolute ethyl alcohol solution, and performing mechanical stirring and ultrasonic dispersion to obtain a SiC suspension, wherein the mechanical stirring speed is 100r/min, and the stirring and ultrasonic dispersion time is 0.8 h.
Adding AlSi10Mg powder and the SiC suspension into a ball milling tank filled with zirconia grinding balls together, and carrying out low-energy planetary ball milling; argon is adopted for protection in the ball milling process, the ball material ratio is 1.5:1, the ball milling rotation speed is 100r/min, the ball milling time is 4h, and the ball milling process stops 15min for every 25min of positive rotation and then reverses for 25min so as to prevent powder overheating.
Step five, drying the composite powder subjected to ball milling dispersion in the step four in a vacuum drying oven at the drying temperature of 80 ℃ for 10 hours, screening by using a 150-mesh screen, and then performing selective laser melting forming under the following parameters: the thickness of the powder spreading layer is 30 μm, the distance between scanning lines is 80 μm, the scanning speed is 1200mm/s, and the laser power is 320W. The SiC-induced multiphase reinforced aluminum matrix composite (II) with uniformly dispersed nano particles is obtained through the steps.
Example 3
The embodiment provides a preparation method of a SiC-induced multiphase reinforced aluminum matrix composite material with uniformly dispersed nano particles, which specifically comprises the following steps:
step one, weighing 10% of nano SiC and 90% of AlSi10Mg powder raw materials according to mass percentage, then placing the SiC powder in an acetone solution for ultrasonic cleaning for 1h to remove surface stains and gas adsorption, then cleaning twice with distilled water, and drying at 70 ℃.
And 2, flatly paving the cleaned SiC powder in a quartz crucible, placing the quartz crucible in a heat treatment furnace, and performing pre-oxidation treatment in an air atmosphere. In order to prevent the SiC powder from agglomerating at high temperature, a sectional heating process is adopted: firstly, heating to 300 ℃ at a heating rate of 5-15 ℃ and preserving heat for 60 min; heating to 600 ℃ at the heating rate of 5-15 ℃/min, preserving heat for 60min, then heating to the preset oxidation temperature of 1200 ℃, preserving heat for 6h, and cooling to room temperature along with the furnace; the heating process of pre-oxidation is shown in FIG. 2, and the SiO obtained after pre-oxidation2The theoretical thickness of the layer is 15 nm.
Step three, pre-oxidized nano SiCOXAdding the powder and polyvinylpyrrolidone (PVP) with the mass of 1% of the powder into 500ml of absolute ethanol solution, and performing mechanical stirring and ultrasonic dispersion by using an ultrasonic stirrer to obtain a SiC suspension, wherein the mechanical stirring speed is 150r/min, and the stirring and ultrasonic dispersion time is 1 h.
Step four, adding the AlSi10Mg powder and the SiC suspension obtained in the step three into a ball milling tank filled with zirconia grinding balls, and carrying out low-energy planetary ball milling; argon is adopted for protection in the ball milling process, the ball material ratio is 2:1, the ball milling rotation speed is 150rpm, the ball milling time is 6 hours, and the ball milling process stops 15 minutes every 25 minutes of forward rotation and then reverses 25 minutes to prevent powder overheating.
Step five, drying the composite powder subjected to ball milling dispersion in the step four in a vacuum drying oven at the drying temperature of 80 ℃ for 12 hours, then screening by using a 150-mesh screen, and then performing selective laser melting forming under the following parameters: the thickness of the powder spreading layer is 30 μm, the distance between scanning lines is 80 μm, the scanning speed is 1600mm/s, and the laser power is 350W. The SiC-induced multi-phase reinforced aluminum matrix composite (III) with uniformly dispersed nano particles is obtained through the steps.
Comparative example
The comparative example provides a non-pre-oxidized SiC reinforced aluminum matrix composite prepared by a direct dispersion method, and the other preparation processes are the same as the preparation parameters provided in the embodiment 2 of the invention, and the specific preparation process is as follows:
weighing 6% of nano SiC and 94% of AlSi10Mg powder raw materials according to mass percentage.
Adding the powder raw materials and zirconia grinding balls into a ball-milling tank together for planetary ball milling; in the ball milling process, absolute ethyl alcohol is used as a process control agent, argon is used for protection, the ball-material ratio is 1.5:1, the ball milling rotation speed is 100rpm, and the ball milling time is 4 hours; during the ball milling process, the rotation is stopped for 15min and then reversed for 25min every 25min to prevent the powder from overheating.
Drying the particles subjected to ball milling dispersion in a vacuum drying oven at the drying temperature of 80 ℃ for 10h, and then screening by using a 150-mesh screen; then, selective laser melting forming is carried out under the following parameters: and the thickness of the powder layer is 30 microns, the distance between scanning lines is 80 microns, the scanning speed is 1200mm/s, and the laser power is 320W, so that the non-pre-oxidized SiC reinforced aluminum matrix composite (IV) in the comparative example is obtained.
TABLE 2 mechanical properties of the aluminum matrix composites prepared in examples 1-3 and comparative examples
Tensile property tests are carried out on the aluminum-based composite materials prepared in the embodiments 1 to 3 and the aluminum-based composite material prepared in the comparative example under the same conditions, and as shown in table 2, the mechanical properties of the aluminum-based composite materials prepared in the embodiments 1 to 3 are obviously improved compared with the comparative example. Comparing example 2 with comparative example, the yield strength, tensile strength and elongation at break of the aluminum matrix composite material obtained in example 2 are respectively improved by about 8.64%, 7.42% and 112.82% compared with the composite material obtained in the comparative example.
Therefore, the invention successfully prepares the multiphase reinforced aluminum matrix composite material with uniform nano-particle dispersion, high density, fine crystal grains and excellent mechanical property by combining the pre-oxidation, pre-dispersion and selective laser melting, effectively solves the problem of poor plasticity and toughness of the printed SiC reinforced aluminum matrix composite material, realizes the controllable preparation of the aluminum matrix composite material with excellent performance, and provides reliable theoretical reference and technical support for practical application of the aluminum matrix composite material.
The foregoing are merely exemplary embodiments of the present invention, which enable those skilled in the art to understand or practice the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention.
It will be understood that the invention is not limited to what has been described above and that various modifications and changes can be made without departing from the scope thereof. The scope of the invention is limited only by the appended claims.
Claims (10)
1. The SiC-induced multiphase reinforced aluminum-based composite material is characterized in that raw material powder consists of nano SiC powder and AlSi10Mg powder, and a reinforcing phase comprises additional nano SiC particles and Al generated by in-situ reaction2O3、Al4SiC4And (3) granules.
2. The SiC-induced multiphase reinforced aluminum matrix composite material as claimed in claim 1, wherein the mass percentage of the nano SiC powder in the raw material powder is 2-10%, and the mass percentage of the AlSi10Mg powder is 90-98%; the grain size of the nano SiC powder is 40-100 nm, the grain size of the AlSi10Mg powder is 45-106 mu m, and the grain size of an Al matrix in the multiphase reinforced aluminum matrix composite material is 400-600 nm.
3. A method for preparing SiC-induced multiphase reinforced aluminum-based composite material is characterized in that pre-oxidized nano SiC is firstly subjected toOXPre-dispersing the particles to obtain SiCOXSuspending the solution, and mixing the SiCOXBall milling and mixing the suspension and AlSi10Mg particles to obtain SiCOXthe/AlSi 10Mg composite powder is finally melted into the alloy by selective laserThe multiphase reinforced aluminum matrix composite material is prepared by a shape forming process.
4. The method for preparing the SiC-induced multiphase reinforced aluminum matrix composite as claimed in claim 3, which comprises the following steps:
1) uniformly spreading the nano SiC particles, placing the nano SiC particles in a heat treatment furnace, carrying out pre-oxidation treatment in an air atmosphere, keeping the pre-oxidation temperature at 800-1200 ℃, and cooling the nano SiC particles to room temperature along with the furnace after heat preservation for 2-6 hours;
2) pre-oxidized nano SiCOXAdding the particles and a dispersing agent into an absolute ethyl alcohol solution, and obtaining SiC by mechanical stirring and ultrasonic dispersionOXSuspending liquid; the mass of the dispersing agent is nano SiCOXThe mass of the particles is 0.5% -20%;
3) mixing AlSi10Mg particles with the SiCOXAdding the suspension into a ball milling tank together for planetary ball milling dispersion;
4) screening the composite particles obtained by ball milling and dispersing in the step 3), and preparing the multiphase reinforced aluminum matrix composite material by a selective laser melting forming process.
5. The method for preparing the SiC-induced multiphase reinforced aluminum matrix composite material according to claim 4, wherein before the pre-oxidation treatment of the SiC nanoparticles in the step 1), the SiC nanoparticles are firstly placed in an organic solvent for ultrasonic cleaning for 0.5-1 h, then are cleaned twice by distilled water, and are dried at the temperature of 60-80 ℃.
6. The method for preparing the SiC-induced multiphase reinforced aluminum matrix composite material according to claim 4, wherein the pre-oxidation treatment in the step 1) adopts a sectional heating process: firstly, heating to 300 ℃ at a heating rate of 5-15 ℃/min, and keeping the temperature for 15-60 min; and then heating to 600 ℃ at the heating rate of 5-15 ℃/min, preserving the heat for 15-60 min, and then heating to the pre-oxidation temperature and preserving the heat for 2-6 h.
7. The preparation method of the SiC-induced multiphase reinforced aluminum matrix composite material according to claim 4, wherein the rotation speed of the mechanical stirring in the step 2) is 50-150 r/min, and the time of the mechanical stirring and the ultrasonic dispersion is 0.5-1 h.
8. The preparation method of the SiC-induced multiphase reinforced aluminum matrix composite material according to claim 4, wherein the ball milling tank in the step 3) is protected by argon in the ball milling process, and the ball-to-material ratio is (1-2): 1, the ball milling speed is 50-150 r/min, and the ball milling time is 2-6 h.
9. The method for preparing the SiC-induced multiphase reinforced aluminum matrix composite material according to claim 4, wherein the screening in the step 4) is specifically as follows:
drying the particles subjected to ball milling dispersion in the step 3) in a vacuum drying oven at the drying temperature of 80 ℃ for 6-12 h;
followed by sieving with a 150 mesh sieve.
10. The method for preparing the SiC-induced multiphase reinforced aluminum matrix composite according to claim 4, wherein the selective laser melting forming process in the step 4) is carried out in an argon atmosphere, and the argon pressure is not higher than 10 bar; the parameters of the selective laser melting forming process are as follows: the scanning speed is 800-1600 mm/s, and the laser power is 280-350W.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114990415A (en) * | 2022-06-15 | 2022-09-02 | 中国重汽集团济南动力有限公司 | Nano biphase reinforced aluminum-based composite material and 3D printing forming method thereof |
Citations (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08269591A (en) * | 1995-03-31 | 1996-10-15 | Toyo Alum Kk | Aluminum alloy powder molding partially containing ceramic particles and its production |
| KR19990069044A (en) * | 1998-02-04 | 1999-09-06 | 박호군 | SIC / (2XXX AL + SI) composite material for reaction solidification and its manufacturing method |
| WO2010128687A1 (en) * | 2009-05-08 | 2010-11-11 | Fujifilm Corporation | Aluminum base material, metal substrate having insulating layer employing the aluminum base material, semiconductor element, and solar battery |
| CN102864361A (en) * | 2012-08-17 | 2013-01-09 | 河南科技大学 | SiC enhanced aluminum-based composite material for spacecraft and preparation method thereof |
| CN103045914A (en) * | 2012-12-06 | 2013-04-17 | 南京航空航天大学 | Preparation method of nano silicon carbide reinforced aluminum-based composite material |
| CN105039793A (en) * | 2015-07-17 | 2015-11-11 | 三峡大学 | Nano-featured enhanced aluminum-based composite and preparing method thereof |
| CN107460376A (en) * | 2017-07-31 | 2017-12-12 | 华中科技大学 | A kind of hybrid reinforced aluminum-matrix composite material and preparation method thereof |
| CN108284226A (en) * | 2018-04-04 | 2018-07-17 | 鑫精合激光科技发展（北京）有限公司 | A kind of electronic package shell 3D printing increasing material manufacturing method |
| CN108640663A (en) * | 2018-08-15 | 2018-10-12 | 辽宁科技大学 | A kind of graphene/carbon SiClx enhancing alumina matrix composite and preparation method thereof |
| CN108950284A (en) * | 2018-07-24 | 2018-12-07 | 国家电网公司 | A kind of low creep aluminium alloy and preparation method thereof |
| CN109207804A (en) * | 2018-11-23 | 2019-01-15 | 湘潭金波新材料科技有限公司 | The preparation method of high-performance aluminium alloy |
| CN109852849A (en) * | 2017-11-30 | 2019-06-07 | 沈阳东青科技有限公司 | A kind of nano SiC granule enhancing aluminum-magnesium composite material |
| CN110170653A (en) * | 2019-05-29 | 2019-08-27 | 西安工业大学 | One kind is from feeding SiCp/AlSi composite material and preparation method |
| CN111235417A (en) * | 2020-01-15 | 2020-06-05 | 华南理工大学 | High-performance aluminum-based composite material based on selective laser melting and forming and preparation method thereof |
| WO2021000618A1 (en) * | 2019-07-01 | 2021-01-07 | 上海交通大学 | Aluminum alloy powder for laser additive manufacturing, and use thereof |
| CN113134625A (en) * | 2021-03-31 | 2021-07-20 | 中国商用飞机有限责任公司北京民用飞机技术研究中心 | Method for melting and forming high-strength aluminum-based composite material part in selective laser area |
-
2022
- 2022-04-22 CN CN202210428198.8A patent/CN114525434A/en active Pending
Patent Citations (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08269591A (en) * | 1995-03-31 | 1996-10-15 | Toyo Alum Kk | Aluminum alloy powder molding partially containing ceramic particles and its production |
| KR19990069044A (en) * | 1998-02-04 | 1999-09-06 | 박호군 | SIC / (2XXX AL + SI) composite material for reaction solidification and its manufacturing method |
| WO2010128687A1 (en) * | 2009-05-08 | 2010-11-11 | Fujifilm Corporation | Aluminum base material, metal substrate having insulating layer employing the aluminum base material, semiconductor element, and solar battery |
| CN102864361A (en) * | 2012-08-17 | 2013-01-09 | 河南科技大学 | SiC enhanced aluminum-based composite material for spacecraft and preparation method thereof |
| CN103045914A (en) * | 2012-12-06 | 2013-04-17 | 南京航空航天大学 | Preparation method of nano silicon carbide reinforced aluminum-based composite material |
| CN105039793A (en) * | 2015-07-17 | 2015-11-11 | 三峡大学 | Nano-featured enhanced aluminum-based composite and preparing method thereof |
| CN107460376A (en) * | 2017-07-31 | 2017-12-12 | 华中科技大学 | A kind of hybrid reinforced aluminum-matrix composite material and preparation method thereof |
| CN109852849A (en) * | 2017-11-30 | 2019-06-07 | 沈阳东青科技有限公司 | A kind of nano SiC granule enhancing aluminum-magnesium composite material |
| CN108284226A (en) * | 2018-04-04 | 2018-07-17 | 鑫精合激光科技发展（北京）有限公司 | A kind of electronic package shell 3D printing increasing material manufacturing method |
| CN108950284A (en) * | 2018-07-24 | 2018-12-07 | 国家电网公司 | A kind of low creep aluminium alloy and preparation method thereof |
| CN108640663A (en) * | 2018-08-15 | 2018-10-12 | 辽宁科技大学 | A kind of graphene/carbon SiClx enhancing alumina matrix composite and preparation method thereof |
| CN109207804A (en) * | 2018-11-23 | 2019-01-15 | 湘潭金波新材料科技有限公司 | The preparation method of high-performance aluminium alloy |
| CN110170653A (en) * | 2019-05-29 | 2019-08-27 | 西安工业大学 | One kind is from feeding SiCp/AlSi composite material and preparation method |
| WO2021000618A1 (en) * | 2019-07-01 | 2021-01-07 | 上海交通大学 | Aluminum alloy powder for laser additive manufacturing, and use thereof |
| CN111235417A (en) * | 2020-01-15 | 2020-06-05 | 华南理工大学 | High-performance aluminum-based composite material based on selective laser melting and forming and preparation method thereof |
| CN113134625A (en) * | 2021-03-31 | 2021-07-20 | 中国商用飞机有限责任公司北京民用飞机技术研究中心 | Method for melting and forming high-strength aluminum-based composite material part in selective laser area |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114990415A (en) * | 2022-06-15 | 2022-09-02 | 中国重汽集团济南动力有限公司 | Nano biphase reinforced aluminum-based composite material and 3D printing forming method thereof |
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