CN116356174B - Aluminum-based composite material based on graphene and preparation method thereof - Google Patents

Aluminum-based composite material based on graphene and preparation method thereof Download PDF

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CN116356174B
CN116356174B CN202310352590.3A CN202310352590A CN116356174B CN 116356174 B CN116356174 B CN 116356174B CN 202310352590 A CN202310352590 A CN 202310352590A CN 116356174 B CN116356174 B CN 116356174B
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molybdenum disulfide
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CN116356174A (en
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李盾
王晓鍇
李健强
陈德安
吴葛亮
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Shanghai Jialang Industrial Nantong Intelligent Technology Co ltd
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    • C22C1/00Making non-ferrous alloys
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    • 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
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    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
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    • B22CASTING; POWDER METALLURGY
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    • B22F9/00Making metallic powder or suspensions thereof
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Abstract

The invention relates to the technical field of aluminum-based composite materials, in particular to a graphene-based aluminum-based composite material and a preparation method thereof. Step 1: according to mass fraction, mixing 92.2% -95.5% of pure aluminum powder, 3% -6% of aluminum-silicon alloy powder and 1.5% -1.8% of reinforcing agent by ball milling to obtain mixed powder; step 2: and (3) carrying out mould pressing, hot pressing, sintering, extrusion, induction heat treatment, stretching and aging treatment on the mixed powder in sequence to obtain the aluminum-based composite material. The beneficial effects are that: in the technical scheme, the aluminum-based composite material with excellent mechanical property and heat conducting property is prepared by optimizing the component proportion and adjusting the multistage process on the basis that the introduction amount of the reinforcing agent is more than 1%, so that the application range is widened.

Description

Aluminum-based composite material based on graphene and preparation method thereof
Technical Field
The invention relates to the technical field of aluminum-based composite materials, in particular to a graphene-based aluminum-based composite material and a preparation method thereof.
Background
The aluminum-based composite material is formed by processing and compounding a plurality of materials with different properties, has the advantages of light weight, small density, good plasticity, low thermal expansion coefficient, high specific strength and the like, and is widely applied to the fields of automobiles, aerospace, metal mirrors and the like. In the development of new energy automobiles, the aluminum-based composite material is generally applied to an engine bracket, and the aluminum-based composite material is required to have excellent mechanical properties and heat dissipation properties.
In the prior art, reinforcing agents such as ceramic fibers, silicon carbide, aluminum oxide and the like are generally introduced into the aluminum-based composite material for enhancing mechanical properties, but compared with graphene, the traditional reinforcing agents have the defects of relatively poor interfacial properties with aluminum powder and poor thermal conductivity. In the graphene reinforced aluminum matrix composite, when the introduction amount of the reinforcing agent is low, the thermal conductivity is low; when the introduction amount of the reinforcing agent is high, the graphene is uniformly dispersed in the aluminum matrix and reacts with the aluminum interface, so that segregation and agglomeration exist, and the performance is reduced and cracks are generated.
In summary, solving the problems, the preparation of the graphene-based aluminum-based composite material with excellent mechanical properties and thermal conductivity has important significance.
Disclosure of Invention
The invention aims to provide an aluminum-based composite material based on graphene and a preparation method thereof, so as to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme:
the preparation method of the graphene-based aluminum matrix composite material comprises the following steps:
step 1: according to mass fraction, mixing 92.2% -95.5% of pure aluminum powder, 3% -6% of aluminum-silicon alloy powder and 1.5% -1.8% of reinforcing agent by ball milling to obtain mixed powder;
step 2: and (3) carrying out mould pressing, hot pressing, sintering, extrusion, induction heat treatment, stretching and aging treatment on the mixed powder in sequence to obtain the aluminum-based composite material.
More optimally, the pure aluminum powder is A00 pure aluminum powder, and the grain diameter is 8-10 mu m; the aluminum-silicon alloy powder is AlSi10 aluminum-silicon alloy powder with the grain diameter of 5-8 mu m.
More optimally, the reinforcing agent is a mixture of graphene oxide and molybdenum disulfide, and the mass ratio of the graphene oxide to the molybdenum disulfide is (1.5-2): 1.
More preferably, in step 2, the induction heat treatment process is as follows: setting the temperature to 480-500 ℃, heating for 60 seconds, keeping for 60 seconds, and cooling for 10 seconds to perform treatment;
the stretching process is as follows: the temperature is set to 400-420 ℃, the preheating is carried out for 10-15 minutes, and then the stretching speed is set to 20-22 mm/min for stretching.
More preferably, in step 2, the molding process is: setting the pressure to 200-300 Mpa at room temperature, and pressing for 10-20 minutes;
the hot pressing process comprises the following steps: setting the temperature to 550-580 ℃, the pressure to 50-60 Mpa, and pressing for 5-8 minutes;
the sintering process is as follows: setting the temperature to 600-620 ℃, heating up the powder at a rate of 80-100 ℃/min, and sintering the powder for 5-8 minutes by vacuum plasma under the pressure of 30 Mpa;
the extrusion process is as follows: setting the temperature to 450-480 ℃, preheating for 30-40 minutes, then setting the extrusion ratio to be (20-25): 1, and extruding at the extrusion rate of 1-1.2 mm/s;
the aging treatment process comprises the following steps: setting the temperature to 160-180 ℃ and treating for 1-3 hours.
More preferably, in step 1, the grinding and mixing process is as follows: the inert gas atmosphere is ball-milled for 7 to 9 hours at a low speed of 80 to 120rpm and then ball-milled for 2 to 3 hours at a high speed of 280 to 320rpm according to the ball-to-material ratio of (15 to 16): 1.
Optimally, the aluminum-silicon alloy powder and the reinforcing agent are pre-compounded firstly and then mixed with pure aluminum powder to obtain mixed powder; the method specifically comprises the following steps:
step 1: (1) Weighing 93-96.25% of pure aluminum powder, 3-6% of aluminum-silicon alloy powder and 0.75-1.2% of reinforcing agent according to mass fraction, wherein the reinforcing agent comprises graphene oxide and molybdenum disulfide;
(2) Dispersing molybdenum disulfide in deionized water, adding L-cysteine, stirring for 1-4 hours, centrifugally separating, and drying to obtain modified molybdenum disulfide;
(3) Sequentially ultrasonically dispersing modified molybdenum disulfide and graphene oxide in deionized water to obtain a dispersion liquid; dropwise adding a magnesium chloride solution, uniformly stirring, adding aluminum-silicon alloy powder, performing ultrasonic dispersion, stirring, drying, and performing heat treatment at 380-400 ℃ for 1 hour to obtain a raw material A; and ball-milling and mixing the raw material A with pure aluminum powder to obtain mixed powder.
More optimally, in the modified molybdenum disulfide, the mass ratio of the molybdenum disulfide to the L-cysteine is (8-10): 1.
More preferably, the concentration of the dispersion is 0.2mg/mL; the volume ratio of the dispersion liquid to the magnesium chloride solution is 6:1, wherein the magnesium chloride solution is 0.5-0.6 mg/mL.
More optimally, the aluminum-based composite material prepared by the preparation method of the graphene-based aluminum-based composite material.
Compared with the prior art, the beneficial effects are as follows:
in the technical scheme, the aluminum-based composite material with excellent mechanical property and heat conducting property is prepared by optimizing the component proportion and adjusting the multistage process on the basis that the introduction amount of the reinforcing agent is more than 1%, so that the application range is widened.
(1) In the scheme, in the ball milling mixing process, a mixing process of long-time low speed and short-time high speed is adopted, so that the morphology damage of the reinforcing agent (graphene oxide and molybdenum disulfide) in the ball milling process is reduced. In a further scheme, the reinforcing agent is firstly mixed with the silicon-aluminum alloy powder, so that the dispersibility in an aluminum matrix is further improved, the ball milling damage is reduced, the interface reaction is inhibited, and the Al is inhibited 4 C 3 Thereby reducing brittleness and improving the mechanical property of the aluminum-based composite material.
(2) In the scheme, the reinforcing agent comprises graphene oxide and molybdenum disulfide, the single graphene oxide has limited improvement on mechanical properties, and molybdenum disulfide is introduced and is cooperatively dispersed in a matrix to generate dislocation blocking movement, so that the toughness is improved, and the subsequent stretching process is facilitated. In addition, the introduction of molybdenum disulfide can reduce the damage of impurities in the pure aluminum powder (unavoidable iron impurities exist in the pure aluminum powder), so that dislocation is reduced, and the graphene oxide and the molybdenum disulfide can cooperate to improve the performance of the aluminum-based composite material.
(3) In the scheme, the reinforcing agent is mixed with the silicon aluminum alloy powder by using magnesium chloride, so that the dispersibility is improved, and meanwhile, the heat conductivity and the mechanical property of the aluminum-based composite material are enhanced.
Wherein, as graphene oxide and molybdenum disulfide are nano particles, the graphene oxide and molybdenum disulfide are directly introduced into ball milling, and agglomeration can be caused; at the same time, the wettability is poorThe affinity with aluminum base is poor, the excessive introduction amount is easy to generate interface reaction with the aluminum base, and Al is generated 4 C 3 . Therefore, in the scheme, the silicon aluminum alloy powder with proper content is introduced, magnesium ions generated in magnesium chloride are used as bridges, the reinforcing agent is anchored on the surface of the aluminum silicon alloy powder through chemical bonds and electrostatic action, and then the affinity between the aluminum silicon alloy and the aluminum powder is utilized to be uniformly dispersed in the aluminum-based composite material. It should be noted that: the quality of cysteine of the modified molybdenum disulfide, the concentration of the reinforcing agent and the concentration of magnesium chloride are required to be set, because interaction exists between carboxyl and magnesium ions, if parameters such as the concentration of magnesium ions and the like are inappropriate, the interaction between magnesium and the reinforcing agent is stronger than the interaction between aluminum and graphene oxide, so that the dispersion of graphene is influenced, and the performance is reduced; and the magnesium is not introduced in an excessively high amount, otherwise the elongation is lowered, so that the performance is lowered.
(4) In the scheme, aluminum-silicon alloy powder is introduced, and because the melting temperature of the aluminum-silicon alloy powder is about 585 ℃ and the melting temperature of pure aluminum powder is about 650 ℃, the sintering temperature selected in the scheme is 600-620 ℃, and the process is equivalent to a semi-liquid metallurgical process, the flow among particles is enhanced by utilizing the aluminum-silicon alloy powder, so that the interface performance is improved, the pores are reduced, the boundary thermal resistance is reduced, and the thermal conductivity of the aluminum-based composite material is improved. On the other hand, due to the introduction of silicon element, the solid solution of carbon in aluminum is reduced, thereby suppressing Al 4 C 3 The generation of (3) improves the interface reaction; meanwhile, silicon and magnesium can form Mg with silicon in the heat induction treatment process 2 The Si reinforced phase improves the mechanical property of the aluminum-based composite material. It should be noted that: the silicon-aluminum alloy is not introduced in an excessive amount, and after the final aging treatment, silicon is precipitated in the aluminum crystal grains, resulting in a decrease in thermal conductivity.
(5) In the scheme, induction heat treatment and stretching processes are added, and the heat induction treatment can induce grain refinement and reduce pores; in the stretching process, the scheme is preheated at a lower temperature, and the shearing stress caused by plastic deformation is utilized, so that the separation and refinement of the reinforcing agent are further increased; the dispersibility and the interfacial effect of the reinforcing agent in the composite material are synergistically improved by the two steps, so that the reinforcing agent is effectively dispersed on the basis of higher content in the scheme, and the heat conductivity and the mechanical property of the aluminum-based composite material are improved.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the following examples, the pure aluminum powder was A00 pure aluminum powder with a particle size of 8 to 10. Mu.m; the aluminum-silicon alloy powder is AlSi10 aluminum-silicon alloy powder with the grain diameter of 5-8 mu m; the average granularity of the graphene oxide is 5 mu m, and the carboxyl content is 5-6%; the average particle size of molybdenum disulfide was 2 μm, all commercially available.
Example 1: a preparation method of an aluminum-based composite material based on graphene comprises the following steps:
step 1: (1) Weighing raw materials according to 93.4% of pure aluminum powder, 5% of aluminum-silicon alloy powder and 1.6% of reinforcing agent by mass, wherein the reinforcing agent is graphene oxide and molybdenum disulfide in a mass ratio of 1.5:1; (2) Ball-milling the raw materials at a ball-material ratio of 16:1 under an argon gas atmosphere at a low speed of 100rpm for 8 hours, and then ball-milling at a high speed of 300rpm for 2 hours to obtain mixed powder;
step 2: filling the mixed powder into a die, setting the pressure to 250Mpa at room temperature, and pressing for 15 minutes; hot-pressing at 560 deg.C under 60Mpa for 5 min; placing the powder into a vacuum plasma sintering furnace, setting the temperature to 610 ℃, the heating rate to 100 ℃/min, and the pressure to 30Mpa, and preserving the heat for 8 minutes; preheating the mixture for 30 minutes at the temperature of 460 ℃, and then setting the extrusion ratio to be 25:1, wherein the extrusion speed is 1 mm/s; then carrying out induction heat treatment at 500 ℃ for 60 seconds, 60 seconds for holding and 10 seconds for cooling; preheating the steel plate at 400 ℃ for 15 minutes, and setting the stretching rate to be 20mm/min for stretching; finally, aging the aluminum-based composite material for 2 hours at the temperature of 180 ℃ to obtain the aluminum-based composite material.
Example 2: a preparation method of an aluminum-based composite material based on graphene comprises the following steps:
step 1: (1) Weighing raw materials according to 93.4% of pure aluminum powder, 5% of aluminum-silicon alloy powder and 1.6% of reinforcing agent by mass, wherein the reinforcing agent is graphene oxide and molybdenum disulfide in a mass ratio of 1.5:1;
(2) Ultrasonically dispersing molybdenum disulfide in deionized water to obtain a dispersion liquid with the weight percent of 0.5, adding L-cysteine, stirring for 4 hours, centrifugally separating, and freeze-drying to obtain modified molybdenum disulfide; in the modified molybdenum disulfide, the mass ratio of the molybdenum disulfide to the L-cysteine is 10:1;
(3) Sequentially ultrasonically dispersing modified molybdenum disulfide and graphene oxide in deionized water to obtain a dispersion liquid with the concentration of 0.2mg/mL; dropwise adding 0.55mg/mL of magnesium chloride solution, uniformly stirring, adding aluminum-silicon alloy powder, performing ultrasonic dispersion, stirring, drying, and performing heat treatment at 400 ℃ for 1 hour in a nitrogen atmosphere to obtain a raw material A; the volume ratio of the dispersion liquid to the magnesium chloride solution is 6:1;
(4) Ball-milling the raw material A and pure aluminum powder at a ball-material ratio of 16:1 under the argon gas atmosphere at a low speed of 100rpm for 8 hours, and then ball-milling at a high speed of 300rpm for 2 hours to obtain mixed powder;
step 2: filling the mixed powder into a die, setting the pressure to 250Mpa at room temperature, and pressing for 15 minutes; hot-pressing at 560 deg.C under 60Mpa for 5 min; placing the powder into a vacuum plasma sintering furnace, setting the temperature to 610 ℃, the heating rate to 100 ℃/min, and the pressure to 30Mpa, and preserving the heat for 8 minutes; preheating the mixture for 30 minutes at the temperature of 460 ℃, and then setting the extrusion ratio to be 25:1, wherein the extrusion speed is 1 mm/s; then carrying out induction heat treatment at 500 ℃ for 60 seconds, 60 seconds for holding and 10 seconds for cooling; preheating the steel plate at 400 ℃ for 15 minutes, and setting the stretching rate to be 20mm/min for stretching; finally, aging the aluminum-based composite material for 2 hours at the temperature of 180 ℃ to obtain the aluminum-based composite material.
Example 3: a preparation method of an aluminum-based composite material based on graphene comprises the following steps:
step 1: (1) Weighing raw materials according to 92.2% of pure aluminum powder, 6% of aluminum-silicon alloy powder and 1.8% of reinforcing agent, wherein the reinforcing agent is graphene oxide and molybdenum disulfide in a mass ratio of 2:1;
(2) Ultrasonically dispersing molybdenum disulfide in deionized water to obtain a dispersion liquid with the weight percent of 0.5, adding L-cysteine, stirring for 4 hours, centrifugally separating, and freeze-drying to obtain modified molybdenum disulfide; in the modified molybdenum disulfide, the mass ratio of the molybdenum disulfide to the L-cysteine is 10:1;
(3) Sequentially ultrasonically dispersing modified molybdenum disulfide and graphene oxide in deionized water to obtain a dispersion liquid with the concentration of 0.2mg/mL; dropwise adding 0.6mg/mL of magnesium chloride solution, uniformly stirring, adding aluminum-silicon alloy powder, performing ultrasonic dispersion, stirring, drying, and performing heat treatment at 400 ℃ for 1 hour in a nitrogen atmosphere to obtain a raw material A; the volume ratio of the dispersion liquid to the magnesium chloride solution is 6:1;
(4) Ball-milling the raw material A and pure aluminum powder at a ball-material ratio of 16:1 under the argon gas atmosphere at a low speed of 100rpm for 8 hours, and then ball-milling at a high speed of 300rpm for 2 hours to obtain mixed powder;
step 2: filling the mixed powder into a die, setting the pressure to 250Mpa at room temperature, and pressing for 15 minutes; hot-pressing at 560 deg.C under 60Mpa for 5 min; placing the powder into a vacuum plasma sintering furnace, setting the temperature to 610 ℃, the heating rate to 100 ℃/min, and the pressure to 30Mpa, and preserving the heat for 8 minutes; preheating the mixture for 30 minutes at the temperature of 460 ℃, and then setting the extrusion ratio to be 25:1, wherein the extrusion speed is 1 mm/s; then carrying out induction heat treatment at 500 ℃ for 60 seconds, 60 seconds for holding and 10 seconds for cooling; preheating the steel plate at 400 ℃ for 15 minutes, and setting the stretching rate to be 20mm/min for stretching; finally, aging the aluminum-based composite material for 2 hours at the temperature of 180 ℃ to obtain the aluminum-based composite material.
Example 4: a preparation method of an aluminum-based composite material based on graphene comprises the following steps:
step 1: (1) Weighing raw materials according to the mass fraction of 95.5% of pure aluminum powder, 3% of aluminum-silicon alloy powder and 1.5% of reinforcing agent, wherein the reinforcing agent is graphene oxide and molybdenum disulfide with the mass ratio of 1.5:1;
(2) Ultrasonically dispersing molybdenum disulfide in deionized water to obtain a dispersion liquid with the weight percent of 0.5, adding L-cysteine, stirring for 4 hours, centrifugally separating, and freeze-drying to obtain modified molybdenum disulfide; in the modified molybdenum disulfide, the mass ratio of the molybdenum disulfide to the L-cysteine is 10:1;
(3) Sequentially ultrasonically dispersing modified molybdenum disulfide and graphene oxide in deionized water to obtain a dispersion liquid with the concentration of 0.2mg/mL; dropwise adding 0.5mg/mL of magnesium chloride solution, uniformly stirring, adding aluminum-silicon alloy powder, performing ultrasonic dispersion, stirring, drying, and performing heat treatment at 400 ℃ for 1 hour in a nitrogen atmosphere to obtain a raw material A; the volume ratio of the dispersion liquid to the magnesium chloride solution is 6:1;
(4) Ball-milling the raw material A and pure aluminum powder at a ball-material ratio of 16:1 under the argon gas atmosphere at a low speed of 100rpm for 8 hours, and then ball-milling at a high speed of 300rpm for 2 hours to obtain mixed powder;
step 2: filling the mixed powder into a die, setting the pressure to 250Mpa at room temperature, and pressing for 15 minutes; hot-pressing at 560 deg.C under 60Mpa for 5 min; placing the powder into a vacuum plasma sintering furnace, setting the temperature to 610 ℃, the heating rate to 100 ℃/min, and the pressure to 30Mpa, and preserving the heat for 8 minutes; preheating the mixture for 30 minutes at the temperature of 460 ℃, and then setting the extrusion ratio to be 25:1, wherein the extrusion speed is 1 mm/s; then carrying out induction heat treatment at 500 ℃ for 60 seconds, 60 seconds for holding and 10 seconds for cooling; preheating the steel plate at 400 ℃ for 15 minutes, and setting the stretching rate to be 20mm/min for stretching; finally, aging the aluminum-based composite material for 2 hours at the temperature of 180 ℃ to obtain the aluminum-based composite material.
Comparative example 1: molybdenum disulfide was not introduced, and the rest was the same as in example 2;
step 1: (1) Weighing raw materials according to 93.4% of pure aluminum powder, 5% of aluminum-silicon alloy powder and 1.6% of reinforcing agent, wherein the reinforcing agent is graphene oxide;
(2) Sequentially ultrasonically dispersing graphene oxide in deionized water to obtain a dispersion liquid with the concentration of 0.2mg/mL; dropwise adding 0.55mg/mL of magnesium chloride solution, uniformly stirring, adding aluminum-silicon alloy powder, performing ultrasonic dispersion, stirring, drying, and performing heat treatment at 400 ℃ for 1 hour in a nitrogen atmosphere to obtain a raw material A; the volume ratio of the dispersion liquid to the magnesium chloride solution is 6:1;
(3) Ball-milling the raw material A and pure aluminum powder at a ball-material ratio of 16:1 under the argon gas atmosphere at a low speed of 100rpm for 8 hours, and then ball-milling at a high speed of 300rpm for 2 hours to obtain mixed powder;
step 2: filling the mixed powder into a die, setting the pressure to 250Mpa at room temperature, and pressing for 15 minutes; hot-pressing at 560 deg.C under 60Mpa for 5 min; placing the powder into a vacuum plasma sintering furnace, setting the temperature to 610 ℃, the heating rate to 100 ℃/min, and the pressure to 30Mpa, and preserving the heat for 8 minutes; preheating the mixture for 30 minutes at the temperature of 460 ℃, and then setting the extrusion ratio to be 25:1, wherein the extrusion speed is 1 mm/s; then carrying out induction heat treatment at 500 ℃ for 60 seconds, 60 seconds for holding and 10 seconds for cooling; preheating the steel plate at 400 ℃ for 15 minutes, and setting the stretching rate to be 20mm/min for stretching; finally, aging the aluminum-based composite material for 2 hours at the temperature of 180 ℃ to obtain the aluminum-based composite material.
Comparative example 2: aluminum silicon alloy powder is not introduced, and the rest is the same as in the example 2;
step 1: (1) Weighing raw materials according to 98.4% of pure aluminum powder and 1.6% of reinforcing agent by mass, wherein the reinforcing agent is graphene oxide and molybdenum disulfide by mass ratio of 1.5:1;
(2) Ultrasonically dispersing molybdenum disulfide in deionized water to obtain a dispersion liquid with the weight percent of 0.5, adding L-cysteine, stirring for 4 hours, centrifugally separating, and freeze-drying to obtain modified molybdenum disulfide; in the modified molybdenum disulfide, the mass ratio of the molybdenum disulfide to the L-cysteine is 10:1;
(3) Sequentially ultrasonically dispersing modified molybdenum disulfide and graphene oxide in deionized water to obtain a dispersion liquid with the concentration of 0.2mg/mL; dropwise adding 0.55mg/mL of magnesium chloride solution, uniformly stirring, adding 5% of pure aluminum powder, performing ultrasonic dispersion, stirring, drying, and performing heat treatment at 400 ℃ for 1 hour in a nitrogen atmosphere to obtain a raw material A; the volume ratio of the dispersion liquid to the magnesium chloride solution is 6:1;
(4) Ball-milling the raw material A and the rest pure aluminum powder at a ball-material ratio of 16:1 under the argon atmosphere at a low speed of 100rpm for 8 hours, and then ball-milling at a high speed of 300rpm for 2 hours to obtain mixed powder;
step 2: filling the mixed powder into a die, setting the pressure to 250Mpa at room temperature, and pressing for 15 minutes; hot-pressing at 560 deg.C under 60Mpa for 5 min; placing the powder into a vacuum plasma sintering furnace, setting the temperature to 610 ℃, the heating rate to 100 ℃/min, and the pressure to 30Mpa, and preserving the heat for 8 minutes; preheating the mixture for 30 minutes at the temperature of 460 ℃, and then setting the extrusion ratio to be 25:1, wherein the extrusion speed is 1 mm/s; then carrying out induction heat treatment at 500 ℃ for 60 seconds, 60 seconds for holding and 10 seconds for cooling; preheating the steel plate at 400 ℃ for 15 minutes, and setting the stretching rate to be 20mm/min for stretching; finally, aging the aluminum-based composite material for 2 hours at the temperature of 180 ℃ to obtain the aluminum-based composite material.
Comparative example 3: 10% of aluminum-silicon alloy powder is introduced, and the rest is the same as in example 2;
step 1: (1) Weighing raw materials according to 88.4% of pure aluminum powder, 10% of aluminum-silicon alloy powder and 1.6% of reinforcing agent, wherein the reinforcing agent is graphene oxide and molybdenum disulfide in a mass ratio of 1.5:1;
(2) Ultrasonically dispersing molybdenum disulfide in deionized water to obtain a dispersion liquid with the weight percent of 0.5, adding L-cysteine, stirring for 4 hours, centrifugally separating, and freeze-drying to obtain modified molybdenum disulfide; in the modified molybdenum disulfide, the mass ratio of the molybdenum disulfide to the L-cysteine is 10:1;
(3) Sequentially ultrasonically dispersing modified molybdenum disulfide and graphene oxide in deionized water to obtain a dispersion liquid with the concentration of 0.2mg/mL; dropwise adding 0.55mg/mL of magnesium chloride solution, uniformly stirring, adding aluminum-silicon alloy powder, performing ultrasonic dispersion, stirring, drying, and performing heat treatment at 400 ℃ for 1 hour in a nitrogen atmosphere to obtain a raw material A; the volume ratio of the dispersion liquid to the magnesium chloride solution is 6:1.
(4) Ball-milling the raw material A and pure aluminum powder at a ball-material ratio of 16:1 under the argon gas atmosphere at a low speed of 100rpm for 8 hours, and then ball-milling at a high speed of 300rpm for 2 hours to obtain mixed powder;
step 2: filling the mixed powder into a die, setting the pressure to 250Mpa at room temperature, and pressing for 15 minutes; hot-pressing at 560 deg.C under 60Mpa for 5 min; placing the powder into a vacuum plasma sintering furnace, setting the temperature to 610 ℃, the heating rate to 100 ℃/min, and the pressure to 30Mpa, and preserving the heat for 8 minutes; preheating the mixture for 30 minutes at the temperature of 460 ℃, and then setting the extrusion ratio to be 25:1, wherein the extrusion speed is 1 mm/s; then carrying out induction heat treatment at 500 ℃ for 60 seconds, 60 seconds for holding and 10 seconds for cooling; preheating the steel plate at 400 ℃ for 15 minutes, and setting the stretching rate to be 20mm/min for stretching; finally, aging the aluminum-based composite material for 2 hours at the temperature of 180 ℃ to obtain the aluminum-based composite material.
Comparative example 4: the concentration of the magnesium chloride solution was increased to 1mg/mL, and the rest was the same as in example 2;
step 1: (1) Weighing raw materials according to 93.4% of pure aluminum powder, 5% of aluminum-silicon alloy powder and 1.6% of reinforcing agent by mass, wherein the reinforcing agent is graphene oxide and molybdenum disulfide in a mass ratio of 1.5:1;
(2) Ultrasonically dispersing molybdenum disulfide in deionized water to obtain a dispersion liquid with the weight percent of 0.5, adding L-cysteine, stirring for 4 hours, centrifugally separating, and freeze-drying to obtain modified molybdenum disulfide; in the modified molybdenum disulfide, the mass ratio of the molybdenum disulfide to the L-cysteine is 10:1;
(3) Sequentially ultrasonically dispersing modified molybdenum disulfide and graphene oxide in deionized water to obtain a dispersion liquid with the concentration of 0.2mg/mL; dropwise adding 1mg/mL of magnesium chloride solution, uniformly stirring, adding aluminum-silicon alloy powder, performing ultrasonic dispersion, stirring, drying, and performing heat treatment at 400 ℃ for 1 hour in a nitrogen atmosphere to obtain a raw material A; the volume ratio of the dispersion liquid to the magnesium chloride solution is 6:1.
(4) Ball-milling the raw material A and pure aluminum powder at a ball-material ratio of 16:1 under the argon gas atmosphere at a low speed of 100rpm for 8 hours, and then ball-milling at a high speed of 300rpm for 2 hours to obtain mixed powder;
step 2: filling the mixed powder into a die, setting the pressure to 250Mpa at room temperature, and pressing for 15 minutes; hot-pressing at 560 deg.C under 60Mpa for 5 min; placing the powder into a vacuum plasma sintering furnace, setting the temperature to 610 ℃, the heating rate to 100 ℃/min, and the pressure to 30Mpa, and preserving the heat for 8 minutes; preheating the mixture for 30 minutes at the temperature of 460 ℃, and then setting the extrusion ratio to be 25:1, wherein the extrusion speed is 1 mm/s; then carrying out induction heat treatment at 500 ℃ for 60 seconds, 60 seconds for holding and 10 seconds for cooling; preheating the steel plate at 400 ℃ for 15 minutes, and setting the stretching rate to be 20mm/min for stretching; finally, aging the aluminum-based composite material for 2 hours at the temperature of 180 ℃ to obtain the aluminum-based composite material.
Comparative example 5: induction heat treatment was not performed, and the rest was the same as in example 2;
step 1: (1) Weighing raw materials according to 93.4% of pure aluminum powder, 5% of aluminum-silicon alloy powder and 1.6% of reinforcing agent by mass, wherein the reinforcing agent is graphene oxide and molybdenum disulfide in a mass ratio of 1.5:1;
(2) Ultrasonically dispersing molybdenum disulfide in deionized water to obtain a dispersion liquid with the weight percent of 0.5, adding L-cysteine, stirring for 4 hours, centrifugally separating, and freeze-drying to obtain modified molybdenum disulfide; in the modified molybdenum disulfide, the mass ratio of the molybdenum disulfide to the L-cysteine is 10:1;
(3) Sequentially ultrasonically dispersing modified molybdenum disulfide and graphene oxide in deionized water to obtain a dispersion liquid with the concentration of 0.2mg/mL; dropwise adding 0.55mg/mL of magnesium chloride solution, uniformly stirring, adding aluminum-silicon alloy powder, performing ultrasonic dispersion, stirring, drying, and performing heat treatment at 400 ℃ for 1 hour in a nitrogen atmosphere to obtain a raw material A; the volume ratio of the dispersion liquid to the magnesium chloride solution is 6:1;
(4) Ball-milling the raw material A and pure aluminum powder at a ball-material ratio of 16:1 under the argon gas atmosphere at a low speed of 100rpm for 8 hours, and then ball-milling at a high speed of 300rpm for 2 hours to obtain mixed powder;
step 2: filling the mixed powder into a die, setting the pressure to 250Mpa at room temperature, and pressing for 15 minutes; hot-pressing at 560 deg.C under 60Mpa for 5 min; placing the powder into a vacuum plasma sintering furnace, setting the temperature to 610 ℃, the heating rate to 100 ℃/min, and the pressure to 30Mpa, and preserving the heat for 8 minutes; preheating the mixture for 30 minutes at the temperature of 460 ℃, and then setting the extrusion ratio to be 25:1, wherein the extrusion speed is 1 mm/s; preheating the steel plate at 400 ℃ for 15 minutes, and setting the stretching rate to be 20mm/min for stretching; finally, aging the aluminum-based composite material for 2 hours at the temperature of 180 ℃ to obtain the aluminum-based composite material.
Comparative example 6: the stretching treatment was not performed, and the rest was the same as in example 2;
step 1: (1) Weighing raw materials according to 93.4% of pure aluminum powder, 5% of aluminum-silicon alloy powder and 1.6% of reinforcing agent by mass, wherein the reinforcing agent is graphene oxide and molybdenum disulfide in a mass ratio of 1.5:1;
(2) Ultrasonically dispersing molybdenum disulfide in deionized water to obtain a dispersion liquid with the weight percent of 0.5, adding L-cysteine, stirring for 4 hours, centrifugally separating, and freeze-drying to obtain modified molybdenum disulfide; in the modified molybdenum disulfide, the mass ratio of the molybdenum disulfide to the L-cysteine is 10:1;
(3) Sequentially ultrasonically dispersing modified molybdenum disulfide and graphene oxide in deionized water to obtain a dispersion liquid with the concentration of 0.2mg/mL; dropwise adding 0.55mg/mL of magnesium chloride solution, uniformly stirring, adding aluminum-silicon alloy powder, performing ultrasonic dispersion, stirring, drying, and performing heat treatment at 400 ℃ for 1 hour in a nitrogen atmosphere to obtain a raw material A; the volume ratio of the dispersion liquid to the magnesium chloride solution is 6:1;
(4) Ball-milling the raw material A and pure aluminum powder at a ball-material ratio of 16:1 under the argon gas atmosphere at a low speed of 100rpm for 8 hours, and then ball-milling at a high speed of 300rpm for 2 hours to obtain mixed powder;
step 2: filling the mixed powder into a die, setting the pressure to 250Mpa at room temperature, and pressing for 15 minutes; hot-pressing at 560 deg.C under 60Mpa for 5 min; placing the powder into a vacuum plasma sintering furnace, setting the temperature to 610 ℃, the heating rate to 100 ℃/min, and the pressure to 30Mpa, and preserving the heat for 8 minutes; preheating the mixture for 30 minutes at the temperature of 460 ℃, and then setting the extrusion ratio to be 25:1, wherein the extrusion speed is 1 mm/s; then carrying out induction heat treatment at 500 ℃ for 60 seconds, 60 seconds for holding and 10 seconds for cooling; finally, aging the aluminum-based composite material for 2 hours at the temperature of 180 ℃ to obtain the aluminum-based composite material.
Performance test: and carrying out mechanical property test and heat conductivity coefficient test on the prepared aluminum-based composite material. Wherein 48X 10X 2mm is taken 3 The tensile strength was measured at a rate of 0.5mm/m using a universal tester according to the standard of GB/T228.1. The thermal conductivity of the test sample was measured at 20 ℃ using a laser thermal conductivity meter and a differential calorimeter scanner. The data obtained are shown below:
sample of Tensile strength Mpa Thermal conductivity W/(m.K)
Example 1 225 213
Example 2 278 227
Example 3 270 223
Example 4 275 220
Comparative example 1 233 218
Comparative example 2 201 209
Comparative example 3 256 215
Comparative example 4 234 203
Comparative example 5 251 193
Comparative example 6 243 190
From the data in the table above, it can be seen that: as can be seen from the data of examples 1 and examples 2 to 4, in the scheme, the dispersibility of the reinforcing agent can be improved by compounding the reinforcing agent with the silicon-aluminum alloy, so that the mechanical property is remarkably improved, and the heat conduction property is improved.
Comparison of the data of example 2 with the data of comparative examples 1-6 shows that: the mechanical property is improved by introducing molybdenum disulfide and graphene oxide. The introduction of the aluminum-silicon alloy can improve the mechanical property and the heat conduction property, and excessive introduction can lead silicon to precipitate and affect the property of the aluminum-based composite material. And the concentration of the magnesium chloride solution is increased, so that the dispersibility of the graphene oxide is reduced, and meanwhile, the performance is obviously reduced due to the increase of the introduced amount of magnesium. In comparative examples 5 and 6, the dispersibility and interfacial properties of graphene were reduced and the properties of the aluminum-based composite material were reduced to different extents due to the absence of induction heat treatment and stretching treatment.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (4)

1. A preparation method of an aluminum-based composite material based on graphene is characterized by comprising the following steps: the method comprises the following steps:
step 1: (1) Weighing 92.2-95.5% of pure aluminum powder, 3-6% of aluminum-silicon alloy powder and 1.5-1.8% of reinforcing agent according to mass fraction, wherein the reinforcing agent is graphene oxide and molybdenum disulfide with mass ratio of (1.5-2): 1;
(2) Dispersing molybdenum disulfide in deionized water, adding L-cysteine, stirring for 1-4 hours, centrifugally separating, and drying to obtain modified molybdenum disulfide;
(3) Sequentially ultrasonically dispersing modified molybdenum disulfide and graphene oxide in deionized water to obtain a dispersion liquid; dropwise adding a magnesium chloride solution, uniformly stirring, adding aluminum-silicon alloy powder, performing ultrasonic dispersion, stirring, drying, and performing heat treatment at 380-400 ℃ for 1 hour to obtain a raw material A; ball-milling and mixing the raw material A with pure aluminum powder to obtain mixed powder;
in the modified molybdenum disulfide, the mass ratio of the molybdenum disulfide to the L-cysteine is (8-10): 1; the concentration of the dispersion liquid is 0.2mg/mL; the volume ratio of the dispersion liquid to the magnesium chloride solution is 6:1, wherein the magnesium chloride solution is 0.5-0.6 mg/mL;
the ball milling mixing process comprises the following steps: ball milling is carried out for 7 to 9 hours at a low speed under 80 to 120rpm in an inert gas atmosphere according to the ball-to-material ratio of (15 to 16): 1, and then ball milling is carried out for 2 to 3 hours at a high speed under 280 to 320 rpm;
step 2: carrying out mould pressing, hot pressing, sintering, extrusion, induction heat treatment, stretching and aging treatment on the mixed powder in sequence to obtain an aluminum-based composite material;
the induction heat treatment process comprises the following steps: setting the temperature to 480-500 ℃, heating for 60 seconds, keeping for 60 seconds, and cooling for 10 seconds to perform treatment;
the stretching process is as follows: the temperature is set to 400-420 ℃, the preheating is carried out for 10-15 minutes, and then the stretching speed is set to 20-22 mm/min for stretching.
2. The method for preparing the graphene-based aluminum-based composite material according to claim 1, wherein the method comprises the following steps: the pure aluminum powder is A00 pure aluminum powder, and the grain diameter is 8-10 mu m; the aluminum-silicon alloy powder is AlSi10 aluminum-silicon alloy powder with the grain diameter of 5-8 mu m.
3. The method for preparing the graphene-based aluminum-based composite material according to claim 1, wherein the method comprises the following steps: in the step 2, the mould pressing process is as follows: setting the pressure to be 200-300 MPa at room temperature, and pressing for 10-20 minutes;
the hot pressing process comprises the following steps: setting the temperature to 550-580 ℃, the pressure to 50-60 MPa, and pressing for 5-8 minutes;
the sintering process is as follows: setting the temperature to 600-620 ℃, heating up the powder at a speed of 80-100 ℃/min, and sintering the powder for 5-8 minutes by vacuum plasma under the pressure of 30 MPa;
the extrusion process is as follows: setting the temperature to 450-480 ℃, preheating for 30-40 minutes, then setting the extrusion ratio to be (20-25): 1, and extruding at the extrusion rate of 1-1.2 mm/s;
the aging treatment process comprises the following steps: setting the temperature to 160-180 ℃ and treating for 1-3 hours.
4. The aluminum-based composite material prepared by the preparation method of the graphene-based aluminum-based composite material according to any one of claims 1 to 3.
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