CN108941547B - Preparation method of copper-doped graphene reinforced aluminum-based composite material - Google Patents
Preparation method of copper-doped graphene reinforced aluminum-based composite material Download PDFInfo
- Publication number
- CN108941547B CN108941547B CN201810846435.6A CN201810846435A CN108941547B CN 108941547 B CN108941547 B CN 108941547B CN 201810846435 A CN201810846435 A CN 201810846435A CN 108941547 B CN108941547 B CN 108941547B
- Authority
- CN
- China
- Prior art keywords
- copper
- aluminum
- graphene
- doped graphene
- composite material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 129
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 116
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 65
- 239000002131 composite material Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 29
- 238000003756 stirring Methods 0.000 claims abstract description 28
- 238000005245 sintering Methods 0.000 claims abstract description 23
- 238000007731 hot pressing Methods 0.000 claims abstract description 22
- 229910000365 copper sulfate Inorganic materials 0.000 claims abstract description 18
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 18
- 239000011159 matrix material Substances 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000006228 supernatant Substances 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- 230000008569 process Effects 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000003825 pressing Methods 0.000 claims description 7
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Inorganic materials [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 abstract description 19
- 229910001431 copper ion Inorganic materials 0.000 abstract description 15
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 238000005054 agglomeration Methods 0.000 abstract 1
- 230000002776 aggregation Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 34
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 18
- 229910052802 copper Inorganic materials 0.000 description 18
- 239000010949 copper Substances 0.000 description 18
- 235000019441 ethanol Nutrition 0.000 description 12
- 239000011248 coating agent Substances 0.000 description 11
- 238000000576 coating method Methods 0.000 description 11
- 239000000203 mixture Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 238000001878 scanning electron micrograph Methods 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 5
- 238000005266 casting Methods 0.000 description 4
- 238000004663 powder metallurgy Methods 0.000 description 4
- 230000002787 reinforcement Effects 0.000 description 4
- 238000009210 therapy by ultrasound Methods 0.000 description 4
- 229910000838 Al alloy Inorganic materials 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 239000012286 potassium permanganate Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- WPPDFTBPZNZZRP-UHFFFAOYSA-N aluminum copper Chemical compound [Al].[Cu] WPPDFTBPZNZZRP-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000005661 hydrophobic surface Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- -1 meanwhile Chemical compound 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011156 metal matrix composite Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
- C22C21/12—Alloys based on aluminium with copper as the next major constituent
Abstract
The invention relates to a preparation method of a copper-doped graphene reinforced aluminum matrix composite, which specifically comprises the following steps: (1) adding an ethanol solution into aluminum powder, adding a graphene oxide solution, adding a copper sulfate solution after stirring, standing until a supernatant is clear, filtering, washing and drying to obtain copper-doped graphene/aluminum composite powder; (2) and carrying out hot-pressing sintering on the obtained copper-doped graphene/aluminum composite powder. Compared with the prior art, the copper ions are coated on the surface of the aluminum powder, so that the agglomeration of graphene and the interface reaction between the graphene and aluminum are effectively avoided, and the microhardness of the copper-doped graphene reinforced aluminum-based composite material prepared by the method is improved by more than 110%.
Description
Technical Field
The invention relates to a preparation method of a composite material, in particular to a preparation method of a copper-doped graphene reinforced aluminum-based composite material.
Background
The aluminum-based composite material has stable performance and is widely applied to the fields of aerospace and high-end automobile manufacturing due to low density. Compared with the traditional reinforcement (ceramic particles, carbon fibers, carbon nanotubes and the like), the graphene has the advantages of low density, high mechanical property, good heat conductivity, low thermal expansion coefficient and the like, and is considered to be a very promising reinforcement from birth. The high-performance graphene reinforced aluminum-based composite material is successfully developed, so that the performance of the composite material can be improved, and the density of the composite material can be reduced.
In the preparation method of the graphene reinforced aluminum matrix composite material, methods such as a powder metallurgy method, a casting method and friction stir processing are mainly used. In the method, due to the characteristics of mature process, uniform tissue, near-net-shape forming and the like of the powder metallurgy method, attention is paid to the preparation of the graphene reinforced aluminum matrix composite. At present, powder metallurgy becomes an important method for preparing the graphene reinforced aluminum matrix composite.
Through the search of the prior art documents, Jingyue Wang et al (relationship with graphene nanosheets in aluminum matrix composites, script materials, 2012,66, 594-. Bartolucci et Al (Graphene-aluminum nanocomposites, Materials Science and engineering A,2011,528,7933-4C3The carbide of (2) reduces the mechanical property of the composite material. Therefore, in the process of preparing the graphene reinforced metal matrix composite material by the powder metallurgy method, the graphene reinforcement has uniform dispersibility and the key problem of avoiding the interface reaction between the graphene and aluminum to prepare the high-performance graphene reinforced aluminum matrix composite material is solved.
Chinese patent CN201710342605.2 discloses a modified graphene reinforced aluminum matrix composite material and a preparation method thereof, which specifically comprises the following steps: (1) adding graphene into absolute ethyl alcohol, uniformly dispersing, adding a cationic surfactant, performing ultrasonic treatment, and drying to obtain modified graphene; (2) melting pure aluminum, adding modified graphene when half of the pure aluminum is melted, and preserving heat; (3) adding copper, carbon, iron, silicon carbide and lanthanum oxide, keeping the temperature, stirring uniformly, refining, standing, and skimming dross to obtain an aluminum alloy melt; (4) and carrying out gravity casting on the aluminum alloy melt to obtain an aluminum alloy casting, and carrying out solid solution, cooling and aging treatment on the casting once to obtain the modified graphene reinforced aluminum matrix composite. The preparation method has a complex process, and the mechanical property of the composite material is reduced due to the fact that the graphene and the aluminum have interface reaction in the process.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a copper-doped graphene reinforced aluminum-based composite material.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of a copper-doped graphene reinforced aluminum matrix composite material specifically comprises the following steps:
(1) adding an ethanol solution into aluminum powder, adding an ultrasonic-treated graphene oxide solution, stirring, adding a copper sulfate solution, stirring, standing until a supernatant is clear, filtering, washing and drying to obtain copper-doped graphene/aluminum composite powder;
(2) and carrying out hot-pressing sintering on the obtained copper-doped graphene/aluminum composite powder.
Preferably, in the step (1), the graphene oxide solution is prepared by a Hummers method.
Preferably, in the step (1), the Hummers method comprises the following specific steps: mixing high-purity graphite and NaNO3Is added to H2SO4Adding KMnO into the solution under stirring gradually4After stirring uniformly for 1H, 200ml of water are added, stirring is carried out at 100 ℃ for 1H, and then H is added2O2And HCl solution, and centrifugally separating the graphene oxides with different sizes.
Preferably, the mass ratio of the aluminum powder, the graphene and the copper sulfate added in the step (1) is 100 (0.3-1.0) to (5-15).
More preferably, the mass ratio of the aluminum powder, the graphene oxide and the copper sulfate added in the step (1) is 100:0.3: 10.
Preferably, in step (1): the ratio of water to alcohol in the ethanol solution is 1:7-1: 8.
More preferably, in step (1): the ratio of water to alcohol in the ethanol solution is 1: 7.
Preferably, in step (1): the ratio of the added aluminum powder to the ethanol solution is 10g to 80 mL.
Preferably, the hot-pressing sintering in the step (2) is performed in two steps, wherein the first step is cold-pressing treatment, and the second step is hot-pressing sintering.
More preferably, the process conditions of the cold pressing treatment are as follows: the load was 6t and the temperature was room temperature.
More preferably, the process conditions of the hot-pressing sintering are as follows: the load is 5-10t, the temperature is 580 ℃, and the treatment time is 3-4 h.
More preferably, the temperature rise process of the hot-pressing sintering is as follows: the temperature is increased to 580 ℃ for 1 hour, and the temperature is kept at 580 ℃ for 3 hours.
In step (2): copper ions are coated on the surface of the aluminum powder, meanwhile, graphene oxide is partially reduced and is adsorbed on the surface of the aluminum powder, and finally, the graphene/copper/aluminum multilayer coating structure powder is formed through cleaning and drying.
Aluminum powder with a hydrophobic surface did not react with graphene oxide in the suspension before copper sulfate was added to the solution. After the copper sulfate solution is added, copper ions and functional oxygen groups (including epoxy groups, carbonyl groups and carboxyl groups) of the graphene oxide are chemically or electrostatically combined on one hand, and aluminum powder and the copper ions are subjected to a displacement reaction on the other hand, so that the graphene oxide sheets are adsorbed to the surfaces of the aluminum powder, and in the chemical reaction process, metal serves as a reducing agent to promote the reduction reaction of the graphene oxide. And preparing the graphene/copper/aluminum multilayer coating structure powder by a wet method. On the other hand, the addition of copper ions enables the formation of an aluminum-copper alloy during sintering to further improve performance. The graphene oxide is used as a reinforcement to improve the performance of the aluminum-based composite material, and the copper sulfate solution provides copper ions. The ethanol solution inhibits the hydrolysis of the aluminum powder.
Copper sulfate is added into the solution of aluminum powder and alcohol, then graphene oxide solution is added, and after repeated tests, copper ions are brought out in the final alcohol cleaning process. But not copper doping. Firstly adding graphene oxide and then adding a copper sulfate solution to obtain 1% Cu2+，3％Cu2+，5％Cu2+The hardness values of the graphene/aluminum composite material are 33, 50, 71 and 68 respectively. At 3% Cu2+The hardness of the composite material reaches a maximum. In addition, if the proportion of water is too high, the particulate aluminum powder is severely hydrolyzed to become aluminum hydroxide. Copper sulfate if addedSaturation occurs when the copper ions are in excess, and the excess copper ions cannot be completely adsorbed.
Compared with the prior art, the preparation method of the copper-doped graphene reinforced aluminum-based composite material can be used for preparing powder with a graphene/copper/aluminum multilayer coating structure, effectively avoids uneven dispersion of graphene and interface reaction between aluminum and graphene, and is beneficial to improvement of mechanical properties of the graphene reinforced aluminum-based composite material.
Drawings
FIG. 1 is a scanning electron micrograph of graphene oxide sheets as a starting material in example 1;
FIG. 2 is a scanning electron micrograph of the aluminum powder prepared in example 1;
FIG. 3 is a scanning electron micrograph of the graphene/copper/aluminum composite powder in example 1;
FIG. 4 shows the elemental analysis results of the graphene/copper/aluminum composite split EDS in example 1;
figure 5 is the vickers hardness results for the pure aluminum and copper doped graphene reinforced aluminum matrix composites of example 1.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
Example 1
(1) Preparation of graphene oxide
The preparation method of the graphene oxide comprises the following steps: 5g of high-purity graphite and 2.5g of NaNO were mixed3Is added to H2SO4To the solution, stirring was carried out uniformly, followed by gradual addition of KMnO4Stirring for 1 hr, adding 200ml water, stirring at 100 deg.C for 1 hr, adding H2O2And a HCl solution. And then centrifugally separating the graphene oxide with different sizes to obtain a graphene oxide solution with basically consistent size. A scanning electron micrograph of the graphene oxide sheet obtained by the preparation is shown in fig. 1.
(2) Preparation of graphene/copper/aluminum multilayer coating structure powder
Dissolving 0.03g of graphene oxide in 10mL of water to prepare a graphene oxide solution, performing ultrasonic treatment, adding the graphene oxide solution into a mixed solution of 10g of aluminum powder and 80mL of ethanol, stirring the mixture for 3-5 min by using a glass rod, adding a copper sulfate solution, stirring the mixture, standing the mixture until a supernatant is clear, cleaning and drying, wherein the volume ratio of the copper sulfate to the aluminum powder is 1: 10. In the process, copper ions are coated on the surface of the aluminum powder, and the graphene oxide is partially reduced to form reduced graphene oxide. The scanning electron microscope photo of the raw material aluminum powder is shown in fig. 2, the micro-morphology of the composite powder is shown in fig. 3, and the EDS element distribution result is shown in fig. 4. The coating of graphene on the surface of the aluminum powder can be obviously observed in the SEM image of FIG. 3, and the EDS analysis of FIG. 4 shows that the surface of the aluminum powder contains copper and carbon, further proving that copper ions can be used as a binding bridge to promote the adsorption of the aluminum powder and graphene oxide.
(3) Hot-pressing sintering of copper-doped graphene reinforced aluminum-based composite material and microhardness test of composite material
Putting the prepared graphene/copper/aluminum multilayer coating structure powder into a hot-pressing sintering mold, cold pressing at room temperature under the load of 6t, then adopting hot-pressing sintering, and setting hot-pressing sintering parameters: the loading load is 5-10t, the temperature is raised for 1h at 580 ℃ in the first stage under the protection of argon, and the temperature is maintained for 3h at 580 ℃ in the second stage, so that the copper-doped graphene reinforced aluminum-based material is obtained.
And (3) carrying out microhardness test on the graphene reinforced aluminum matrix composite material with or without copper doping, wherein the load is 100N, and the load holding time is 10 s. 3 sets of samples were prepared for each material and 16 points were tested, and the average was taken and the results are shown in FIG. 5.
Test results show that the graphene/copper/aluminum multilayer coating structure powder prepared by the method can be prepared into a copper-doped graphene reinforced aluminum matrix composite material with excellent performance. The microhardness test result shows that compared with a material without copper ions, the hardness of the copper-doped graphene reinforced aluminum-based composite material is improved from 33 to 71, and the copper-doped graphene reinforced aluminum-based composite material (0.3 wt% of graphene content and 3 wt% of copper content) is improved by 110% compared with the graphene reinforced aluminum-based composite material without copper ions (0.3 wt% of graphene content). The method can be used for preparing the high-performance copper-doped graphene reinforced aluminum matrix composite.
Example 2
(1) Preparation of graphene oxide
The preparation method of the graphene oxide comprises the following steps: 5g of high-purity graphite and 2.5g of NaNO were mixed3Is added to H2SO4To the solution, stirring was carried out uniformly, followed by gradual addition of KMnO4Stirring for 1 hr, adding 200ml water, stirring at 100 deg.C for 1 hr, adding H2O2And a HCl solution. And then centrifugally separating the graphene oxide with different sizes to obtain a graphene oxide solution with basically consistent size. A scanning electron micrograph of the graphene oxide sheet obtained by the preparation is shown in fig. 1.
(2) Preparation of graphene/copper/aluminum multilayer coating structure powder
Dissolving 0.08g of graphene oxide in 10mL of water to prepare a graphene oxide solution, adding the graphene oxide solution into a mixed solution of 10g of aluminum powder and 80mL of ethanol after ultrasonic treatment, stirring the mixture for 3-5 min by using a glass rod, then adding a copper sulfate solution, stirring the mixture, standing the mixture until a supernatant is clear, cleaning and drying, wherein the volume ratio of the copper sulfate to the aluminum powder is 1: 8. In the process, copper ions are coated on the surface of the aluminum powder, and the graphene oxide is partially reduced to form reduced graphene oxide.
(3) Hot-pressing sintering of copper-doped graphene reinforced aluminum-based composite material and microhardness test of composite material
Putting the prepared graphene/copper/aluminum multilayer coating structure powder into a hot-pressing sintering mold, cold pressing at room temperature under the load of 6t, then adopting hot-pressing sintering, and setting hot-pressing sintering parameters: the loading load is 5-10t, the temperature is raised for 1h at 580 ℃ in the first stage under the protection of argon, and the temperature is maintained for 3h at 580 ℃ in the second stage, so that the copper-doped graphene reinforced aluminum-based material is obtained.
Example 3
(1) Preparation of graphene oxide
The preparation method of the graphene oxide comprises the following steps: 5g of high-purity graphite and 2.5g of NaNO were mixed3Is added to H2SO4To the solution, stirring was carried out uniformly, followed by gradual addition of KMnO4Stirring for 1 hr, adding 200ml water, stirring at 100 deg.C for 1 hr, adding H2O2And a HCl solution. And then centrifugally separating the graphene oxide with different sizes to obtain a graphene oxide solution with basically consistent size. A scanning electron micrograph of the graphene oxide sheet obtained by the preparation is shown in fig. 1.
(2) Preparation of graphene/copper/aluminum multilayer coating structure powder
Dissolving 0.1g of graphene oxide in 10mL of water to prepare a graphene oxide solution, performing ultrasonic treatment, adding the graphene oxide solution into a mixed solution of 10g of aluminum powder and 80mL of ethanol, stirring the mixture for 3-5 min by using a glass rod, adding a copper sulfate solution, stirring the mixture, standing the mixture until a supernatant is clear, cleaning and drying, wherein the volume ratio of the copper sulfate to the aluminum powder is 1: 7. In the process, copper ions are coated on the surface of the aluminum powder, and the graphene oxide is partially reduced to form reduced graphene oxide.
(3) Hot-pressing sintering of copper-doped graphene reinforced aluminum-based composite material and microhardness test of composite material
Putting the prepared graphene/copper/aluminum multilayer coating structure powder into a hot-pressing sintering mold, cold pressing at room temperature under the load of 6t, then adopting hot-pressing sintering, and setting hot-pressing sintering parameters: the loading load is 5-10t, the temperature is raised for 1h at 580 ℃ in the first stage under the protection of argon, and the temperature is maintained for 3h at 580 ℃ in the second stage, so that the copper-doped graphene reinforced aluminum-based material is obtained.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (6)
1. The preparation method of the copper-doped graphene reinforced aluminum matrix composite is characterized by comprising the following steps:
(1) adding an ethanol solution into aluminum powder, adding an ultrasonic-treated graphene oxide solution, stirring, adding a copper sulfate solution, stirring, standing until a supernatant is clear, filtering, washing and drying to obtain copper-doped graphene/aluminum composite powder;
(2) carrying out hot-pressing sintering on the obtained copper-doped graphene/aluminum composite powder;
the mass ratio of the aluminum powder, the graphene and the copper sulfate added in the step (1) is 100 (0.3-1.0) to 5-15;
in the step (1): the volume ratio of water to alcohol in the ethanol solution is 1:7-1: 8;
in the step (1): the ratio of the added aluminum powder to the ethanol solution is 10g to 80 mL.
2. The method for preparing the copper-doped graphene reinforced aluminum-based composite material according to claim 1, wherein in the step (1), the graphene oxide solution is prepared by a modified Hummers method.
3. The preparation method of the copper-doped graphene reinforced aluminum matrix composite material according to claim 2, wherein the modified Hummers method comprises the following specific steps: mixing high-purity graphite and NaNO3Is added to H2SO4Adding KMnO into the solution under stirring gradually4After stirring uniformly for 1H, 200ml of water are added, stirring is carried out at 100 ℃ for 1H, and then H is added2O2And HCl solution, and centrifugally separating the graphene oxides with different sizes.
4. The preparation method of the copper-doped graphene reinforced aluminum-based composite material according to claim 1, wherein the hot-pressing sintering in the step (2) is carried out in two steps, wherein the first step is cold-pressing treatment, and the second step is hot-pressing sintering.
5. The preparation method of the copper-doped graphene reinforced aluminum matrix composite material according to claim 4, wherein the cold pressing treatment is carried out under the following process conditions: the load was 6t and the temperature was room temperature.
6. The preparation method of the copper-doped graphene reinforced aluminum matrix composite material according to claim 4, wherein the hot-pressing sintering process conditions are as follows: the load is 5-10t, the temperature is 580 ℃, and the treatment time is 3-4 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810846435.6A CN108941547B (en) | 2018-07-27 | 2018-07-27 | Preparation method of copper-doped graphene reinforced aluminum-based composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810846435.6A CN108941547B (en) | 2018-07-27 | 2018-07-27 | Preparation method of copper-doped graphene reinforced aluminum-based composite material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108941547A CN108941547A (en) | 2018-12-07 |
| CN108941547B true CN108941547B (en) | 2020-09-04 |
Family
ID=64466177
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810846435.6A Active CN108941547B (en) | 2018-07-27 | 2018-07-27 | Preparation method of copper-doped graphene reinforced aluminum-based composite material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108941547B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110408808A (en) * | 2019-08-28 | 2019-11-05 | 徐州宇帆机电科技有限公司 | A method of graphene-aluminum matrix composite is prepared based on aluminium powder in-situ reducing and microwave hot-press sintering |
| CN110788346B (en) * | 2019-10-11 | 2022-06-21 | 陕西科技大学 | Semi-metal structure tungsten ditelluride/redox graphene compound and preparation method of copper-doped compound powder thereof |
| CN112111665B (en) * | 2020-08-17 | 2021-09-10 | 丽水正阳电力建设有限公司 | Method for preparing carbon modified aluminum alloy composite material by vacuum pressure infiltration method |
| CN113745642A (en) * | 2021-08-09 | 2021-12-03 | 信阳师范学院 | Preparation method of shell structure aluminum-based material and application of shell structure aluminum-based material in lithium ion battery |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006103798A1 (en) * | 2005-03-29 | 2006-10-05 | Hitachi Metals, Ltd. | High-heat-conduction composite with graphite grain dispersed and process for producing the same |
| CN105624445A (en) * | 2016-01-06 | 2016-06-01 | 昆明理工大学 | Preparation method of graphene-reinforced copper-based composite |
| CN106521220A (en) * | 2016-10-11 | 2017-03-22 | 常州大学 | Novel graphene Al-Cu intermediate alloy preparation method |
| CN106566942A (en) * | 2016-10-24 | 2017-04-19 | 上海理工大学 | A method of preparing a high-performance graphene reinforced aluminium-based composite material |
| CN107299257A (en) * | 2017-05-16 | 2017-10-27 | 苏州莱特复合材料有限公司 | A kind of modified graphene reinforced aluminum matrix composites and preparation method thereof |
| CN108251671A (en) * | 2018-01-08 | 2018-07-06 | 北京科技大学 | A kind of preparation method for adulterating graphene oxide enhancing ODS copper |
-
2018
- 2018-07-27 CN CN201810846435.6A patent/CN108941547B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006103798A1 (en) * | 2005-03-29 | 2006-10-05 | Hitachi Metals, Ltd. | High-heat-conduction composite with graphite grain dispersed and process for producing the same |
| CN101151384A (en) * | 2005-03-29 | 2008-03-26 | 日立金属株式会社 | High-heat-conduction composite with graphite grain dispersed and process for producing the same |
| CN105624445A (en) * | 2016-01-06 | 2016-06-01 | 昆明理工大学 | Preparation method of graphene-reinforced copper-based composite |
| CN106521220A (en) * | 2016-10-11 | 2017-03-22 | 常州大学 | Novel graphene Al-Cu intermediate alloy preparation method |
| CN106566942A (en) * | 2016-10-24 | 2017-04-19 | 上海理工大学 | A method of preparing a high-performance graphene reinforced aluminium-based composite material |
| CN107299257A (en) * | 2017-05-16 | 2017-10-27 | 苏州莱特复合材料有限公司 | A kind of modified graphene reinforced aluminum matrix composites and preparation method thereof |
| CN108251671A (en) * | 2018-01-08 | 2018-07-06 | 北京科技大学 | A kind of preparation method for adulterating graphene oxide enhancing ODS copper |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108941547A (en) | 2018-12-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108941547B (en) | Preparation method of copper-doped graphene reinforced aluminum-based composite material | |
| CN107353017B (en) | Graphene-coated aluminum oxide ceramic powder and preparation method and application thereof | |
| JP6490253B2 (en) | Method for preparing graphene / silver composite material | |
| CN110331325B (en) | Nano-alumina reinforced copper-based composite material and preparation method thereof | |
| Wu et al. | Graphene oxide/Al composites with enhanced mechanical properties fabricated by simple electrostatic interaction and powder metallurgy | |
| CN108889959B (en) | rGO/Cu composite material and preparation method thereof | |
| KR102193589B1 (en) | Method for manufacturing aluminium-graphene composites having enhanced thermal conductivity | |
| CN111408714B (en) | Preparation method of graphene reinforced copper-based composite material with dual-scale structure and in-situ growth | |
| CN108559861A (en) | A method of preparing graphene reinforced aluminum matrix composites | |
| CN113355548B (en) | Atmosphere control powder metallurgy preparation method of graphene reinforced aluminum matrix composite | |
| CN112853142B (en) | Graphene-modified metal composite material | |
| CN106566942B (en) | A kind of method for preparing High-performance graphene reinforced aluminum matrix composites | |
| CN112008087A (en) | Method for improving comprehensive performance of carbon nano material reinforced nickel-based high-temperature alloy | |
| CN111549246A (en) | Preparation method of high-toughness graphene/ZK 61 magnesium alloy composite material | |
| CN110295298B (en) | Preparation method of graphene-aluminum composite material | |
| CN111534236A (en) | Graphite-doped high-temperature-resistant heat-conducting phosphate adhesive and preparation method thereof | |
| CN114164355B (en) | Graphene reinforced metal composite material and preparation method and application thereof | |
| JP2552679B2 (en) | Method for manufacturing high hardness composite copper alloy | |
| CN111321314B (en) | Preparation method of graphene reinforced aluminum matrix composite with strong interface bonding strength | |
| Qian et al. | Effect of potential difference between nano-Al2O3 whisker and Mg matrix on the dispersion of Mg composites | |
| RU2811355C1 (en) | Method for producing composite material based on copper powder | |
| CN110603111A (en) | Hexagonal boron nitride nanosheet/metal nano composite powder and preparation method thereof | |
| CN113667858B (en) | Preparation method of spinel-coated nano-alumina reinforced aluminum-based composite material in situ | |
| CN112899588B (en) | Enhanced composite aluminum-based material and preparation method thereof | |
| CN114959344A (en) | High-strength Ti 3 C 2 T x Magnesium alloy ZK61 and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20240108 Address after: No. 143 Houtou, Xiban Village, Guanxun Town, Zhangpu County, Zhangzhou City, Fujian Province, 363200 Patentee after: Weng Senqi Address before: 200093 No. 516, military road, Shanghai, Yangpu District Patentee before: University of Shanghai for Science and Technology |
|
| TR01 | Transfer of patent right |