CN112974842A - Nano multiphase reinforced aluminum matrix composite material and preparation method thereof - Google Patents

Nano multiphase reinforced aluminum matrix composite material and preparation method thereof Download PDF

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CN112974842A
CN112974842A CN202110162047.8A CN202110162047A CN112974842A CN 112974842 A CN112974842 A CN 112974842A CN 202110162047 A CN202110162047 A CN 202110162047A CN 112974842 A CN112974842 A CN 112974842A
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scandium
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CN112974842B (en
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席丽霞
丁凯
顾冬冬
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Nanjing University of Aeronautics and Astronautics
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24After-treatment of workpieces or articles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE 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
    • B33Y10/00Processes of additive manufacturing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE 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
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE 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
    • B33Y50/00Data acquisition or data processing for additive manufacturing
    • B33Y50/02Data acquisition or data processing for additive manufacturing for controlling or regulating additive manufacturing processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE 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
    • B33Y70/00Materials specially adapted for additive manufacturing
    • B33Y70/10Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
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    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C21/00Alloys based on aluminium
    • C22C21/02Alloys based on aluminium with silicon as the next major constituent
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24After-treatment of workpieces or articles
    • B22F2003/248Thermal after-treatment
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling

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Abstract

The invention disclosesThe nanometer multiphase reinforced aluminum-base composite material includes aluminum alloy base body and Al dispersed in the aluminum alloy base body3Sc nano reinforcing phase, Al3Zr nano reinforcing phase and Al4C3A nanoreinforcement phase; the aluminum alloy matrix is an aluminum-silicon-scandium-zirconium-manganese alloy, wherein the silicon content is 0.5-2.0 wt.%, the scandium content is 0.5-1.5 wt.%, the zirconium content is 0.2-1.0 wt.%, the manganese content is 0.4-1.0 wt.%, and the balance is aluminum. Mixing the aluminum alloy matrix powder and the multi-walled carbon nano-tubes, melting and solidifying the composite powder layer by adopting selective laser melting forming equipment, and finally carrying out aging treatment on the composite powder by using overheating treatment equipment at a specific temperature for a specific time to obtain the composite powder. When the multi-walled carbon nanotube/aluminum-silicon-scandium-zirconium-manganese alloy material is subjected to laser irradiation to be melted to form a molten pool, the larger multi-walled carbon nanotube part reacts with an aluminum substrate in situ to generate Al4C3The reinforcing phase, while the smaller ceramic phase is fully reacted.

Description

Nano multiphase reinforced aluminum matrix composite material and preparation method thereof
Technical Field
The invention belongs to the field of nano multiphase reinforced aluminum matrix composite materials, and particularly relates to a high-strength high-bearing nano multiphase reinforced aluminum matrix composite material and a preparation method thereof.
Background
The aluminum alloy has the characteristics of low density, high specific strength, good corrosion resistance, excellent electric and thermal conductivity and the like, and is widely applied in the fields of aerospace, automobiles, power electronics and the like. However, the limited mechanical properties (ultimate tensile strength < 400MPa and elongation < 6%) of aluminum alloy are difficult to meet the requirements of rapidly developed high and new technical fields such as aerospace, electronic packaging and automobile manufacturing. In order to overcome the defects, the strength and the modulus of the matrix are hopefully and synergistically improved by compounding the multiphase ceramic reinforcement with low density, high strength and high modulus in the aluminum alloy matrix. Among the numerous ceramic reinforcements, Carbon Nanotubes (CNTs) have very large aspect ratios (1000), low densities (1.7 g/cm)3) High tensile strength (110 GPa), high elastic modulus (1 TPa), and high thermal conductivity (3000W m)-1K-1) Good conductivity (2X 10. about.7S m-1) And the like, and becomes a more ideal reinforcing phase for preparing the aluminum matrix composite. However, when the content of the reinforcing phase is high, the viscosity of the liquid phase is increased, the fluidity is poor, the reinforcing phase cannot be uniformly distributed, the problems of poor interface bonding, cracking and the like are caused in the forming process, and the forming quality of parts is high due to the adoption of the single-phase ceramic reinforced aluminum-based composite material at presentAnd (4) poor.
From the viewpoint of processing technology, there are many methods for preparing single-phase ceramic reinforced aluminum matrix composite materials, such as fusion casting method, powder metallurgy, mechanical alloying method, etc., but due to the difference of components, crystal structure and physicochemical properties between ceramic phase and metal matrix, the defects of uneven distribution of ceramic reinforcement, difficult control of size and shape, poor interface bonding between ceramic reinforcement and matrix, etc. are easy to occur, resulting in poor comprehensive performance of the composite material. The selective laser melting technology is used as a novel laser additive manufacturing technology, based on the local forming principle of layered manufacturing and cumulative superposition, and based on a three-dimensional part model designed by a computer auxiliary, the high-energy laser heat source is utilized to selectively and rapidly melt/solidify, stack and form a metal powder layer in a channel-by-channel layer-by-layer mode, so that the direct and rapid forming of a metal component with a complex structure is realized. In the selective laser melting forming process, the action time of a laser heat source and a pre-laid powder layer is extremely short, so that the molten powder has a quite high cooling speed, favorable conditions are provided for grain refinement of the nano multi-phase reinforced aluminum-based composite material, powder particles are completely melted under the action of a high-energy laser beam, adjacent scanning tracks or interlayer metallurgical bonding is good, the forming quality of nano multi-phase reinforced aluminum-based composite material parts is improved, and the mechanical property of the material is improved. The selective laser melting technology breaks through the constraint of the traditional manufacturing process, accords with the design concept of near-net-shape forming, effectively shortens the research and development and manufacturing period of new products, improves the production efficiency, and can form parts with complex geometric shapes, so that the selective laser melting technology for preparing the nano multiphase reinforced aluminum-based composite material has great development potential.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to solve the technical problem of the prior art and provides a high-strength high-bearing nano multiphase reinforced aluminum matrix composite material and a preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a high-strength high-load-bearing nano multi-phase reinforced Al-base composite material contains Al alloyGold matrix and Al dispersed in aluminum alloy matrix3Sc nano reinforcing phase, Al3Zr nano reinforcing phase and Al4C3A nanoreinforcement phase;
the aluminum alloy matrix is an aluminum-silicon-scandium-zirconium-manganese alloy, wherein the silicon content is 0.5-2.0 wt.%, the scandium content is 0.5-1.5 wt.%, the zirconium content is 0.2-1.0 wt.%, the manganese content is 0.4-1.0 wt.%, and the balance is aluminum.
The invention further provides a preparation method of the high-strength high-bearing nano multiphase reinforced aluminum matrix composite, which comprises the following steps:
(1) taking aluminum alloy matrix powder and multi-walled carbon nanotubes, and carrying out ball milling and mixing uniformly under the protection of inert gas by a ball mill to obtain composite powder;
(2) establishing a three-dimensional entity geometric model of a target part by using Soildworks software, then carrying out layered slicing on the model by using Magics software, planning a laser scanning path, dispersing a three-dimensional entity into a series of two-dimensional data, storing and guiding the two-dimensional data into selective laser melting forming equipment;
(3) melting and solidifying the composite powder in the step (1) layer by layer through selective laser melting forming equipment according to the data imported in the step (2) to form a three-dimensional solid part;
(4) and (4) carrying out aging treatment on the three-dimensional solid part formed in the step (3) at a specific temperature for a specific time through heat treatment equipment to obtain the three-dimensional solid part.
Preferably, in the step (1), the particle size distribution range of the aluminum alloy matrix powder is 25-60 μm, the purity is more than 99.0%, and the powder flowability is 65-74 s/50 g.
Preferably, in the step (1), the multi-wall carbon nano has an outer diameter of 10-40nm and a length of 10-50 μm.
Preferably, in the step (1), the addition amount of the multi-walled carbon nanotubes accounts for 0.1-1.0 wt% of the total mass of the composite material.
Preferably, in the step (1), the ball mill adopts a QM series planetary ball mill, the ball-material ratio is 2:1, the ball milling speed is 150-300 rpm, and the ball milling time is 3-6 h. In order to prevent the over-high temperature in the ball milling tank and the damage of the MWCNTs fiber structure, the equipment operation mode is selected in a spaced mode during ball milling, and air cooling is suspended for 5min after the operation is carried out for 15 min. The ball milling process requires that it be conducted under inert gas shielding to prevent oxidation or contamination of the aluminum-based powder during the ball milling process.
Preferably, in the step (3), SLM-150 type selective laser melting equipment is used, and the equipment mainly comprises a YLR-500 type optical fiber laser, a laser forming chamber, an automatic powder laying system, a protective atmosphere device, a computer control circuit system and a cooling circulation system. Before forming, the aluminum alloy substrate subjected to sand blasting treatment is fixed on a selective laser melting forming equipment workbench and leveled, and then a forming cavity is sealed through a sealing device, vacuumized and introduced with inert gas protective atmosphere. A typical selective laser fusion forming process is as follows: (a) uniformly laying the powder to be processed on a forming substrate by a powder laying device, scanning the slice area layer by a laser beam according to a pre-designed scanning path, and rapidly melting/solidifying a powder layer so as to obtain a first two-dimensional plane of the part to be formed; (b) the computer control system enables the forming substrate to descend by one powder layer thickness, the piston of the powder supply cylinder ascends by one powder layer thickness, the powder laying device lays a layer of powder to be processed again, and the high-energy laser beam finishes scanning of the second layer of powder according to the slice information to obtain a second two-dimensional plane of the part to be formed; (c) and (c) repeating the step (b), and forming the powder to be processed layer by layer until the part to be formed is processed.
Preferably, the laser power adopted by the selective laser melting forming equipment is 250-400W, the laser scanning speed is 400-1000 mm/s, the scanning interval is 60 mu m, the powder spreading thickness is 30 mu m, a partitioned island-shaped scanning strategy is adopted, and the laser parameters are determined after process optimization.
Preferably, in the step (4), the aging temperature adopted by the heat treatment equipment is 300-375 ℃, and the heat preservation time is 3-6 h.
Al is regulated and controlled by heat treatment process and addition amount of multi-walled carbon nano-tubes4C3The in-situ generated content of the nano reinforcing phase improves the interface combination between the reinforcing phase and the matrix, improves the forming quality of the material, and promotes Al as a heterogeneous nucleation point3Sc、Al3Of Zr nano reinforcing phaseA large amount of the precipitate is precipitated, and finally the comprehensive mechanical property of the material is improved. Al having rhombohedral crystal structure4C3The nanometer reinforcing phase can be tightly combined with the aluminum matrix and has Al of a face-centered cubic crystal structure3Sc and Al3Zr and an aluminum matrix can form a good coherent interface relationship, and the heat treatment process can release residual stress generated by the difference of the thermal expansion coefficients of the reinforcing phase and the matrix. Therefore, the comprehensive mechanical property of the aluminum matrix composite material can be remarkably improved by the precipitation of the nano multiphase reinforced phase.
The above parameters are the optimal parameters, the aluminum matrix composite reinforcing phase can be reasonably selected and properly added according to the tissue and performance characteristics of the aluminum matrix composite, and the preparation method which is combined with the front-edge selective laser melting technology and the heat treatment process is adopted, so that the content, the morphology, the size and the distribution state of the ceramic reinforcing phase can be effectively adjusted, and the aluminum matrix composite with good forming quality and excellent comprehensive performance can be successfully prepared.
Has the advantages that:
1. when the multi-walled carbon nanotube/aluminum-silicon-scandium-zirconium-manganese alloy material is subjected to laser irradiation to be melted to form a molten pool, the larger multi-walled carbon nanotube part reacts with an aluminum substrate in situ to generate Al4C3The reinforcing phase, while the smaller ceramic phase is fully reacted. The addition of the multi-wall carbon nano-tube refines the grain size, so that part of columnar crystal tends to be equiaxial and the equiaxial area interval is increased. In the subsequent non-equilibrium solidification and rapid cooling processes, a large amount of Sc and Zr elements can be dissolved in the aluminum alloy in a solid solution mode, and after the subsequent heat treatment, the unreacted multi-walled carbon nano tubes are completely converted into high-strength Al4C3The nano reinforcing phase improves the interface combination between the reinforcing phase and the matrix, improves the forming quality of the material, and is used as a heterogeneous nucleation point to promote Al3Sc、Al3The Zr nanometer reinforcing phase is greatly separated out around the Zr nanometer reinforcing phase, and finally the comprehensive mechanical property of the aluminum matrix composite material is improved.
2 in the invention, aluminum-silicon-scandium-zirconium-manganese alloy powder and nano-scale multi-walled carbon nanotubes are used as raw materials, the powder is mixed and then placed in a QM series planetary ball mill for ball milling and powder mixing, and the ball milling process is adoptedThe obtained composite powder has the advantages of uniform distribution of ceramic reinforcing phase, good flow property, high laser absorption rate and suitability for selective laser melting forming, and the process is simple to operate and saves cost. The method for preparing the nano multiphase reinforced aluminum-based composite material by adopting the selective laser melting technology and the heat treatment process not only shortens the production period and improves the production efficiency of products, but also can form parts with complex geometric shapes almost without subsequent machining treatment. The cooling speed of the molten pool is extremely high and can reach 10 when the selective laser melting forming is carried out3~108K/s, effectively avoids the characteristics of nanoparticle agglomeration and grain coarsening in the traditional processing technology, and improves the mechanical property of the part.
3. The invention can adjust the laser energy density by changing the laser power and the laser scanning speed, along with the change of the laser energy input of the powder bed, the thermodynamic and dynamic characteristics of a molten pool formed by the action of the laser and the powder bed are also changed, and by reasonably selecting laser process parameters and adjusting the laser energy input, the generation of metallurgical defects such as spheroidization effect, pores and the like is reduced, and the high-forming-quality nano multiphase enhanced aluminum-silicon-scandium-zirconium-manganese composite material is obtained.
4. According to the invention, the precipitation and distribution of a multiphase nano reinforced phase in the nano multiphase reinforced aluminum-based composite material formed by the selective laser melting technology are regulated and controlled by changing aging process parameters (aging temperature and heat preservation time), the interface combination between the reinforced phase and a matrix is improved, and the high-strength high-bearing nano multiphase reinforced aluminum-silicon-scandium-zirconium-manganese composite material is obtained.
Drawings
The foregoing and/or other advantages of the invention will become further apparent from the following detailed description of the invention when taken in conjunction with the accompanying drawings.
Fig. 1 is an optical image of a multi-walled carbon nanotube/aluminum-silicon-scandium-zirconium-manganese composite specimen prepared in example 1.
Fig. 2 is a schematic view of the distribution of the multiphase ceramic in the multi-walled carbon nanotube/aluminum-silicon-scandium-zirconium-manganese composite sample prepared in example 1 and a TEM photograph of the interface thereof.
Fig. 3 is an optical image of a multi-walled carbon nanotube/aluminum-silicon-scandium-zirconium-manganese composite specimen prepared in example 2.
Fig. 4 is an optical image of a multi-walled carbon nanotube aluminum-silicon-scandium-zirconium-manganese composite specimen prepared in example 3.
Fig. 5 is an optical image of a multi-walled carbon nanotube/aluminum-silicon-scandium-zirconium-manganese composite sample prepared in comparative example 1.
Fig. 6 is an optical image of a multi-walled carbon nanotube aluminum-silicon-scandium-zirconium-manganese composite sample prepared in comparative example 3.
Detailed Description
The invention will be better understood from the following examples.
In the following examples, an aluminum-silicon-scandium-zirconium-manganese alloy powder was used having a silicon content of 1.3 wt.%, a scandium content of 0.66 wt.%, a zirconium content of 0.42 wt.%, a manganese content of 0.49 wt.%, and the balance being Al, an average particle diameter of 38.8 μm, a purity of more than 99.0%, and a powder flowability of 70s/50 g.
The average outer diameter of the used multi-walled carbon nanotube powder was 30nm and the average length was 30 μm.
Example 1
(1) 1.0 wt.% multi-walled carbon nanotube powder (accounting for the total mass of the composite material) is mixed with aluminum-silicon-scandium-zirconium-manganese alloy powder, and ball-milling powder mixing is carried out to prepare 1.0 wt.% multi-walled carbon nanotube/aluminum-silicon-scandium-zirconium-manganese composite powder. The ball milling and powder mixing operation is carried out in a QM series planetary ball mill, a ceramic tank is adopted in the process, and the ball milling media are ceramic grinding balls with the diameters of 6mm, 8mm and 10 mm. The ball milling process parameters are set as follows: the ball-material ratio is 2:1, the ball milling speed is 200rpm, and the ball milling time is 6 h. Meanwhile, in order to prevent the damage to the multi-walled carbon nanotube fiber structure caused by overhigh temperature in the ball milling tank, the operation mode of the equipment is selected in a spaced mode during ball milling, namely, the air cooling is suspended for 5min after the equipment operates for 15 min. The ball milling process requires that it be conducted under argon protection to prevent oxidation or contamination of the aluminum-based powder during the ball milling process.
(2) Target part modeling and slicing process
The method comprises the steps of establishing a three-dimensional solid geometric model of a target part in a computer by using Soildworks software, then carrying out layered slicing and scanning path planning on the three-dimensional solid model by using Magics software, dispersing the three-dimensional solid into a series of two-dimensional data, storing the data and guiding the data into selective laser melting forming equipment. Wherein the laser process parameters are set as follows: the laser power is 300W, the laser scanning speed is 600mm/s, the scanning interval is 60 mu m, the powder spreading thickness is 30 mu m, a subarea island-shaped scanning strategy is adopted, and the rotation angle of the laser scanning direction of the adjacent layer is 37 degrees.
(3) Selective laser fusion forming process
And (2) applying the multi-walled carbon nanotube/aluminum-silicon-scandium-zirconium-manganese composite powder prepared in the step (1) to selective laser melting forming. The system mainly comprises a YLR-500 type optical fiber laser, a laser forming chamber, an automatic powder laying system, a protective atmosphere device, a computer control circuit system and a cooling circulation system. Before forming, fixing the aluminum alloy substrate subjected to sand blasting treatment on a selective laser melting forming equipment workbench, leveling, sealing a forming cavity through a sealing device, vacuumizing, and introducing argon protective atmosphere (Ar purity is 99.999%, outlet pressure is 30mbar) to ensure O in a forming chamber2The content is less than 10 ppm. A typical selective laser fusion forming process is as follows: (a) the powder spreading device uniformly spreads the powder to be processed on the forming substrate, and the laser beam scans the slice area line by line according to a pre-designed scanning path to rapidly melt and solidify the powder layer, so that a first two-dimensional plane of the part is obtained; (b) the computer control system enables the forming substrate to descend by one powder layer thickness, conversely, enables the powder supply cylinder piston to ascend by one powder layer thickness, the powder laying device re-lays a layer of powder to be processed, and the laser beam completes scanning of a second powder layer according to the slicing information to obtain a second two-dimensional plane of the part; (c) and (c) repeating the step (b), and forming the powder to be processed layer by layer until the part is processed.
(4) And after cooling, taking the formed substrate out of the equipment, separating the part from the substrate by using a linear cutting process to obtain the three-dimensional solid part of the nano multiphase reinforced aluminum-based composite material, and performing aging treatment at the speed of 325 ℃/6h to finally obtain the high-strength high-bearing nano multiphase reinforced aluminum-based composite material sample.
According to standard metallographic specimenThe preparation method is used for grinding, polishing and corroding the nano multiphase reinforced aluminum matrix composite material block sample. The high-density nano multiphase reinforced aluminum-silicon-scandium-zirconium-manganese composite material sample prepared by the selective laser melting process and the heat treatment process has no crack generation, nano ceramic reinforced particles are uniformly distributed in a matrix, and an optical image of a microscopic structure of the nano ceramic reinforced particles is shown in figure 1. The sample prepared in example 1 was subjected to TEM analysis, see fig. 2. As can be seen from the figure, Al4C3The nanometer reinforcing phase is uniformly distributed in the matrix and tightly combined with the matrix, and a large amount of Al is precipitated around the nanometer reinforcing phase3Sc、Al3Zr nanoparticles, which indicates Al4C3Form stable interface structure in the aluminum alloy matrix, reduce interface stress concentration, improve forming quality, and promote Al as heterogeneous nucleation point3Sc、Al3The Zr nanometer reinforcing phase is greatly separated out around the Zr nanometer reinforcing phase, thereby playing the role of improving the comprehensive mechanical property of the material.
The obtained nano multiphase reinforced aluminum-silicon-scandium-zirconium-manganese composite material sample is subjected to room temperature tensile and nano hardness tests, the tensile strength and the elastic modulus of the nano multiphase reinforced aluminum-silicon-scandium-zirconium-manganese composite material sample can respectively reach 562MPa and 98GPa, and are respectively improved by 8.7% and 22.5% compared with aluminum alloy (the tensile strength and the elastic modulus of the aluminum alloy are 517MPa and 80GPa), and the nano multiphase reinforced aluminum-silicon-scandium-zirconium-manganese composite material sample has high strength and high bearing performance.
Example 2
(1) 0.5 wt.% multi-walled carbon nanotube powder (accounting for the total mass of the composite material) is mixed with aluminum-silicon-scandium-zirconium-manganese alloy powder, and ball-milling powder mixing is carried out to prepare 0.5 wt.% multi-walled carbon nanotube/aluminum-silicon-scandium-zirconium-manganese composite powder. The ball milling and powder mixing operation is carried out in a QM series planetary ball mill, a ceramic tank is adopted in the process, and the ball milling media are ceramic grinding balls with the diameters of 6mm, 8mm and 10 mm. The ball milling process parameters are set as follows: the ball-material ratio is 2:1, the ball milling speed is 250rpm, and the ball milling time is 5 h. Meanwhile, in order to prevent the damage to the multi-walled carbon nanotube fiber structure caused by overhigh temperature in the ball milling tank, the operation mode of the equipment is selected in a spaced mode during ball milling, namely, the air cooling is suspended for 5min after the equipment operates for 15 min. The ball milling process requires that it be conducted under argon protection to prevent oxidation or contamination of the aluminum-based powder during the ball milling process.
(2) Target part modeling and slicing process
The method comprises the steps of establishing a three-dimensional solid geometric model of a target part in a computer by using Soildworks software, then carrying out layered slicing and scanning path planning on the three-dimensional solid model by using Magics software, dispersing the three-dimensional solid into a series of two-dimensional data, storing the data and guiding the data into selective laser melting forming equipment. Wherein the laser process parameters are set as follows: the laser power is 350W, the laser scanning speed is 800mm/s, the scanning interval is 60 mu m, the powder spreading thickness is 30 mu m, a subarea island-shaped scanning strategy is adopted, and the rotation angle of the laser scanning direction of the adjacent layer is 37 degrees.
(3) Selective laser fusion forming process
And (2) applying the MWCNTs/aluminum-silicon-scandium-zirconium-manganese composite powder prepared in the step (1) to selective laser melting forming. The system mainly comprises a YLR-500 type optical fiber laser, a laser forming chamber, an automatic powder laying system, a protective atmosphere device, a computer control circuit system and a cooling circulation system. Before forming, fixing the aluminum alloy substrate subjected to sand blasting treatment on a selective laser melting forming equipment workbench, leveling, sealing a forming cavity through a sealing device, vacuumizing, and introducing argon protective atmosphere (Ar purity is 99.999%, outlet pressure is 30mbar) to ensure O in a forming chamber2The content is less than 10 ppm. A typical selective laser fusion forming process is as follows: (a) the powder spreading device uniformly spreads the powder to be processed on the forming substrate, and the laser beam scans the slice area line by line according to a pre-designed scanning path to rapidly melt and solidify the powder layer, so that a first two-dimensional plane of the part is obtained; (b) the computer control system enables the forming substrate to descend by one powder layer thickness, conversely, enables the powder supply cylinder piston to ascend by one powder layer thickness, the powder laying device re-lays a layer of powder to be processed, and the laser beam completes scanning of a second powder layer according to the slicing information to obtain a second two-dimensional plane of the part; (c) and (c) repeating the step (b), and forming the powder to be processed layer by layer until the part is processed.
(4) And after cooling, taking the formed substrate out of the equipment, separating the part from the substrate by using a linear cutting process to obtain the three-dimensional solid part of the nano multiphase reinforced aluminum matrix composite, and performing aging treatment at the temperature of 350 ℃/5h to finally obtain the high-strength high-bearing nano multiphase reinforced aluminum matrix composite sample.
And (3) grinding, polishing and corroding the nano multiphase reinforced aluminum matrix composite block sample according to a standard metallographic sample preparation method. The high-density nano multiphase reinforced aluminum-silicon-scandium-zirconium-manganese composite material sample prepared by the selective laser melting process and the heat treatment process has no crack generation, and Al4C3The nanometer reinforcing phase is uniformly distributed in the matrix, is tightly combined with the matrix, and is precipitated with Al3Sc、Al3The Zr nanoparticle content was slightly reduced and the optical image of the microstructure was shown in fig. 3.
The obtained nano multiphase reinforced aluminum-silicon-scandium-zirconium-manganese composite material sample is subjected to room temperature tensile and nano hardness tests, the tensile strength and the elastic modulus of the nano multiphase reinforced aluminum-silicon-scandium-zirconium-manganese composite material sample can respectively reach 545MPa and 94GPa, and are respectively improved by 5.4% and 17.5% compared with aluminum alloy (the tensile strength and the elastic modulus of the aluminum alloy are 517MPa and 80GPa), and the nano multiphase reinforced aluminum-silicon-scandium-zirconium-manganese composite material sample has high strength and high bearing performance.
Example 3
(1) 0.1 wt.% of multi-walled carbon nanotube fiber powder (accounting for the total mass of the composite material) is mixed with aluminum-silicon-scandium-zirconium-manganese alloy powder, and the mixture is subjected to ball milling to prepare 0.1 wt.% of multi-walled carbon nanotube/aluminum-silicon-scandium-zirconium-manganese composite powder. The ball milling and powder mixing operation is carried out in a QM series planetary ball mill, a ceramic tank is adopted in the process, and the ball milling media are ceramic grinding balls with the diameters of 6mm, 8mm and 10 mm. The ball milling process parameters are set as follows: the ball-material ratio is 2:1, the ball milling speed is 300rpm, and the ball milling time is 4 h. Meanwhile, in order to prevent the damage to the multi-walled carbon nanotube fiber structure caused by overhigh temperature in the ball milling tank, the operation mode of the equipment is selected in a spaced mode during ball milling, namely, the air cooling is suspended for 5min after the equipment operates for 15 min. The ball milling process requires that it be conducted under argon protection to prevent oxidation or contamination of the aluminum-based powder during the ball milling process.
(2) Target part modeling and slicing process
The method comprises the steps of establishing a three-dimensional solid geometric model of a target part in a computer by using Soildworks software, then carrying out layered slicing and scanning path planning on the three-dimensional solid model by using Magics software, dispersing the three-dimensional solid into a series of two-dimensional data, storing the data and guiding the data into selective laser melting forming equipment. Wherein the laser process parameters are set as follows: the laser power is 400W, the laser scanning speed is 1000mm/s, the scanning interval is 60 mu m, the powder spreading thickness is 30 mu m, a subarea island-shaped scanning strategy is adopted, and the rotation angle of the laser scanning direction of the adjacent layer is 37 degrees.
(3) Selective laser fusion forming process
And (2) applying the MWCNTs/aluminum-silicon-scandium-zirconium-manganese composite powder prepared in the step (1) to selective laser melting forming. The system mainly comprises a YLR-500 type optical fiber laser, a laser forming chamber, an automatic powder laying system, a protective atmosphere device, a computer control circuit system and a cooling circulation system. Before forming, fixing the aluminum alloy substrate subjected to sand blasting treatment on a selective laser melting forming equipment workbench, leveling, sealing a forming cavity through a sealing device, vacuumizing, and introducing argon protective atmosphere (Ar purity is 99.999%, outlet pressure is 30mbar) to ensure O in a forming chamber2The content is less than 10 ppm. A typical selective laser fusion forming process is as follows: (a) the powder spreading device uniformly spreads the powder to be processed on the forming substrate, and the laser beam scans the slice area line by line according to a pre-designed scanning path to rapidly melt and solidify the powder layer, so that a first two-dimensional plane of the part is obtained; (b) the computer control system enables the forming substrate to descend by one powder layer thickness, conversely, enables the powder supply cylinder piston to ascend by one powder layer thickness, the powder laying device re-lays a layer of powder to be processed, and the laser beam completes scanning of a second powder layer according to the slicing information to obtain a second two-dimensional plane of the part; (c) and (c) repeating the step (b), and forming the powder to be processed layer by layer until the part is processed.
(4) And after cooling, taking the formed substrate out of the equipment, separating the part from the substrate by using a linear cutting process to obtain the three-dimensional solid part of the multiphase ceramic reinforced aluminum matrix composite, and performing aging treatment at 375 ℃/4h subsequently to finally obtain the high-strength high-bearing nano multiphase reinforced aluminum matrix composite sample.
And (3) grinding, polishing and corroding the nano multiphase reinforced aluminum matrix composite block sample according to a standard metallographic sample preparation method. The high-density nano multiphase reinforced aluminum-silicon-scandium-zirconium-manganese composite material sample prepared by the selective laser melting process and the heat treatment process has no crack generation, and Al4C3The nanometer reinforcing phase is uniformly distributed in the matrix, is tightly combined with the matrix, and is precipitated with Al3Sc、Al3The Zr nanoparticle content was significantly reduced and the microscopic structure was imaged by optical lens OM, as shown in fig. 4.
The obtained nano multiphase reinforced aluminum-silicon-scandium-zirconium-manganese composite material sample is subjected to room temperature tensile and nano hardness tests, the tensile strength and the elastic modulus of the nano multiphase reinforced aluminum-silicon-scandium-zirconium-manganese composite material sample can reach 538MPa and 91GPa, are respectively improved by 4.1% and 13.8% compared with aluminum alloy (the tensile strength and the elastic modulus of the aluminum alloy are 517MPa and 80GPa), and the nano multiphase reinforced aluminum-silicon-scandium-zirconium-manganese composite material sample has high strength and high bearing performance.
Comparative example 1
The comparative example is the same as the example 1 except that in the step (1), the MWCNTs powder is not used as the reinforcing phase raw material to prepare the composite powder by the ball milling process, and 1.0 wt.% of Al is selected4C3The nano ceramic and the aluminum-silicon-scandium-zirconium-manganese powder are used as raw materials, composite powder is prepared by ball milling, selective laser melting forming is carried out, aging treatment is carried out at 325 ℃/6h, and the microstructure of the composite powder is shown in figure 5. As can be seen by comparing FIGS. 1 and 5, comparative example 1 directly added Al4C3Al in microstructure of nano multiphase reinforced aluminum-based composite material prepared from ceramic4C3The nano enhanced phase is unevenly distributed, the bonding force with the substrate interface is low, metallurgical defects such as pores and the like are generated in a laser forming sample, the forming quality of the aluminum matrix composite material is reduced, and Al precipitated around the aluminum matrix composite material3Sc、Al3The Zr nanometer reinforcing phase has less particles. Comparative example 1 direct addition of Al4C3The tensile strength and the elastic modulus of the nano multiphase reinforced aluminum-silicon-scandium-zirconium-manganese composite material sample prepared from the ceramic are 491MPa and 74GPa, compared with the tensile strength and the elastic modulus of the nano multiphase reinforced aluminum-based composite material prepared by the in-situ reaction in example 1The reduction is obvious.
Comparative example 2
The specific procedure of this comparative example is substantially the same as example 1, except that: in steps (2) and (3) of the comparative example, the MWCNTs/aluminum-silicon-scandium-zirconium-manganese composite powder prepared was formed by a hot isostatic pressing method. In the comparative example, the distribution of the nano ceramic particles in the formed multiphase reinforced aluminum-silicon-scandium-zirconium-manganese composite material sample is uneven, partial reaction occurs between the ceramic particles and the matrix, and the interface combination between the ceramic particles and the matrix is poor, so that the mechanical property of the sample is seriously reduced. The tensile strength and the elastic modulus of the formed sample are 307MPa and 67GPa, and are greatly reduced compared with the nano multiphase reinforced aluminum-based composite material in the example 1.
Comparative example 3
The specific procedure of this comparative example is substantially the same as example 1, except that: in the step (1) of the present comparative example, 5.0 wt.% of multi-walled carbon nanotubes (percentage of the total mass of the alloy material) were mixed with the aluminum-silicon-scandium-zirconium-manganese alloy powder, and the powder was ball-milled to prepare 5.0 wt.% of MWCNTs/aluminum-silicon-scandium-zirconium-manganese composite powder. In the comparative example, the high-content carbon nano tube is easy to agglomerate, a large number of metallurgical defects such as pores, cracks and the like are generated in a laser forming sample, and the forming quality of the aluminum matrix composite material is obviously reduced. Meanwhile, a large amount of agglomerated Al is generated in the subsequent heat treatment process4C3Poor interface bonding between the phase and the matrix and serving as a germination point of cracks, so that the formed sample is seriously deformed and cracked, the comprehensive mechanical property is greatly reduced, and an optical microscope OM image of a microscopic structure of the sample is shown in figure 6. Compared with the nano multiphase reinforced aluminum matrix composite material in the embodiment 1, the tensile strength and the elastic modulus are greatly reduced.
As can be seen from the example 1 and the comparative examples 1 to 3, the cracks of the nano multiphase reinforced aluminum matrix composite sample prepared by the selective laser melting technology and the heat treatment process are obviously reduced, the forming quality is obviously improved, the nano reinforced phase is uniformly dispersed, the tensile strength and the elastic modulus are maintained at higher levels, the nano multiphase reinforced aluminum matrix composite sample has high strength and high bearing performance, the mechanical property is optimized, and the tensile strength is higher than that of the aluminum alloyThe degree and the elastic modulus are respectively improved by 4.1 to 8.7 percent and 13.8 to 22.5 percent. The addition of the multi-wall carbon nano-tube refines the grain size, promotes a large amount of solid solution of Sc and Zr elements in the selective laser melting forming process, and the subsequent heat treatment process enables the multi-wall carbon nano-tube which is not completely reacted to be completely converted into strong-bearing Al4C3The nano reinforcing phase forms a tightly combined interface with the aluminum matrix and promotes the nano reinforcing phase Al to form a good coherent interface relation with the aluminum matrix3Sc and Al3Zr precipitated out in a large amount around it. Meanwhile, the strong bearing Al which is tightly combined with the matrix and uniformly dispersed4C3The nanometer reinforced phase effectively restrains the thermal expansion behavior of the matrix in the aging process and releases high residual stress generated by the difference of thermal expansion coefficients between the reinforced phase and the matrix. Therefore, the tensile strength and the elastic modulus of the nano multiphase reinforced aluminum matrix composite are obviously improved.
The present invention provides a method and a concept for a nano multiphase reinforced aluminum matrix composite and a method for preparing the same, and a plurality of methods and ways for implementing the technical scheme are provided, the above description is only a preferred embodiment of the present invention, it should be noted that, for those skilled in the art, a plurality of improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be regarded as the protection scope of the present invention. All the components not specified in the present embodiment can be realized by the prior art.

Claims (8)

1. The high-strength high-bearing nano multiphase reinforced aluminum-based composite material is characterized by comprising an aluminum alloy matrix and Al dispersed in the aluminum alloy matrix3Sc nano reinforcing phase, Al3Zr nano reinforcing phase and Al4C3A nanoreinforcement phase;
the aluminum alloy matrix is an aluminum-silicon-scandium-zirconium-manganese alloy, wherein the silicon content is 0.5-2.0 wt.%, the scandium content is 0.5-1.5 wt.%, the zirconium content is 0.2-1.0 wt.%, the manganese content is 0.4-1.0 wt.%, and the balance is aluminum.
2. The preparation method of the high-strength high-load-bearing nano multiphase reinforced aluminum-based composite material as claimed in claim 1, characterized by comprising the following steps:
(1) taking aluminum alloy matrix powder and multi-walled carbon nanotubes, and carrying out ball milling and mixing uniformly under the protection of inert gas by a ball mill to obtain composite powder;
(2) establishing a three-dimensional entity geometric model of a target part by using Soildworks software, then carrying out layered slicing on the model by using Magics software, planning a laser scanning path, dispersing a three-dimensional entity into a series of two-dimensional data, storing and guiding the two-dimensional data into selective laser melting forming equipment;
(3) melting and solidifying the composite powder in the step (1) layer by layer through selective laser melting forming equipment according to the data imported in the step (2) to form a three-dimensional solid part;
(4) and (4) carrying out aging treatment on the three-dimensional solid part formed in the step (3) at a specific temperature for a specific time through heat treatment equipment to obtain the three-dimensional solid part.
3. The preparation method of the high-strength high-load-bearing nano multi-phase reinforced aluminum-based composite material as claimed in claim 2, wherein in the step (1), the particle size distribution range of the aluminum alloy matrix powder is 25-60 μm, the purity is more than 99.0%, and the powder flowability is 65-74 s/50 g.
4. The method for preparing the high-strength high-load-bearing nano multiphase reinforced aluminum-based composite material as claimed in claim 2, wherein in the step (1), the multi-walled carbon nano has an outer diameter of 10-40nm and a length of 10-50 μm.
5. The preparation method of the high-strength high-load-bearing nano multiphase reinforced aluminum-based composite material as claimed in claim 2, wherein in the step (1), the addition amount of the multi-walled carbon nanotubes accounts for 0.1-1.0 wt% of the total mass of the composite material.
6. The preparation method of the high-strength high-load-bearing nano multiphase reinforced aluminum matrix composite material as claimed in claim 2, wherein in the step (1), the ball mill adopts a QM series planetary ball mill, the ball-to-material ratio is 2:1, the ball milling rotation speed is 150-300 rpm, and the ball milling time is 3-6 h.
7. The preparation method of the high-strength high-load-bearing nano multiphase reinforced aluminum-based composite material as claimed in claim 2, wherein in the step (3), the laser power adopted by the selective laser melting forming equipment is 250-400W, and the laser scanning speed is 400-1000 mm/s.
8. The preparation method of the high-strength high-load-bearing nano multi-phase reinforced aluminum-based composite material according to claim 2, wherein in the step (4), the aging temperature adopted by the heat treatment equipment is 300-375 ℃, and the heat preservation time is 3-6 hours.
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