CN110539002A - Method for enhancing mechanical property of aluminum matrix composite material by cooperation of multi-element multi-dimensional enhanced phase - Google Patents
Method for enhancing mechanical property of aluminum matrix composite material by cooperation of multi-element multi-dimensional enhanced phase Download PDFInfo
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- 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
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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- 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
- B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- 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
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C21/00—Alloys based on aluminium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
- B22F2003/208—Warm or hot extruding
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
- C22C2026/002—Carbon nanotubes
Abstract
The invention relates to a preparation method for the mechanical property of a multi-element multi-dimensional reinforced phase synergistic reinforced aluminum matrix composite, which comprises the following steps: in-situ synthesis of a graphene-loaded carbon nanotube and copper nanoparticle composite reinforcing phase: dissolving glucose as a carbon source, copper nitrate trihydrate as a copper source and sodium chloride as a template in deionized water together with the carboxylated carbon nanotubes, and uniformly dispersing to obtain a mixed solution; then, quickly freezing the mixed solution under the assistance of liquid nitrogen, and removing water by adopting a freeze drying technology to obtain composite powder; placing the obtained composite powder in a square boat, then placing the square boat in a constant-temperature area of a high-temperature tube furnace for chemical reaction, wherein the synthesis condition is that the reaction is carried out under hydrogen, the synthesis temperature is 700-800 ℃, and after the reaction is finished, rapidly cooling a sample to obtain mixed powder; washing the powder obtained after the reaction with deionized water and performing suction filtration to remove sodium chloride; and finally, carrying out vacuum drying on the obtained powder to obtain the composite reinforced phase of the graphene-loaded carbon nano tube and the copper nano particles. (2) And (3) molding and preparing the graphene-loaded carbon nanotube and copper nanoparticle synergistically enhanced aluminum matrix composite.
Description
Technical Field
The invention relates to a preparation method for improving the mechanical property of an aluminum-based composite material by utilizing a cold pressing-sintering forming mode, belonging to the field of powder metallurgy.
Background
Aluminum and aluminum alloys are widely used in aerospace, automotive and electronic applications due to their high thermal stability, low density, good ductility and toughness, excellent corrosion resistance, etc. However, the aluminum and aluminum alloy used by us at present generally have low strength and cannot meet many industrial requirements. Therefore, researchers have improved the mechanical properties of aluminum and aluminum alloys in a variety of ways. Among them, it is a very effective method to improve the mechanical strength by preparing the aluminum matrix composite.
Traditionally, aluminum-based composites have been prepared mainly by ceramic phase nanoparticles and fibers, such as alumina nanoparticles, boron nitride nanosheets, silicon carbide nanoparticles, titanium carbide whiskers, and the like. The preparation method mainly comprises powder metallurgy, stirring casting, pressure infiltration and the like. However, with the continuous improvement of the requirements of the scientific and technological development on the performance of the structural materials, the traditional reinforcing phases gradually expose the defects of low reinforcing efficiency, high density and poor ductility and toughness, so that the problem to be solved by searching a novel light reinforcing phase with high toughness and good comprehensive performance is urgently needed.
Carbon nanomaterials (mainly including carbon nanotubes and graphene) are novel nanomaterials that have received much attention in recent years. The carbon nano tube and the graphene have excellent performance, and the strength of the carbon nano tube and the graphene is more than 100 times that of steel; the Young modulus is 1100GPa, the thermal conductivity is about 6000J/(m.K.s), the carrier mobility can reach 2 x 105cm 2/(V.s), and the density is only 2.2g/cm 3. Therefore, under the condition of low mass fraction addition, the carbon nano tubes and the graphene can greatly improve the metal matrix, and meanwhile, the density of the carbon nano tubes and the graphene is smaller than that of the metal matrix, so that the density of the composite material is reduced while the mechanical property of the metal matrix is improved, and the requirements of light weight, high strength and the like of the existing composite material are met. The carbon nano tube and the graphene have super-strong mechanical properties far exceeding those of traditional ceramic phases, nano particles and other reinforcing phases, and can be produced in a large scale at present, so that the problems of low elongation and difficult plastic processing of the composite material are hopefully solved by using the carbon nano tube and the graphene to reinforce the metal matrix, and the production cost can be reduced while a good reinforcing effect is obtained. Therefore, the research on the carbon nano tube and graphene reinforced metal matrix composite material has very important significance. However, at present, the performance improvement obtained by adding carbon nanotubes or graphene as a single reinforcing phase to an aluminum matrix is very limited, so many researchers try to reinforce the aluminum matrix composite material by constructing a composite reinforcing phase of the carbon nanotubes and the graphene to achieve a better reinforcing effect. However, the carbon nano material is very easy to react with aluminum in the sintering or high-temperature smelting process to generate an aluminum carbide brittle phase, so that the plasticity of the composite material is reduced, and the problem brings difficulty for the carbon nano material to reinforce the aluminum-based composite material. Researchers find that the combination of graphene or carbon nanotubes and an aluminum matrix can be improved by coating or loading nano metal particles on the surface of graphene or carbon nanotubes, and the structural integrity of the carbon nanotubes and graphene can be ensured in the processing process. Therefore, the carbon nano tube and graphene composite reinforced phase is constructed and simultaneously the metal nano particles are loaded, so that the method has important significance for reinforcing the aluminum matrix composite and improving the aluminum matrix composite.
The graphene-loaded carbon nanotube and the copper nanoparticle are synthesized in situ by a salt template-assisted method. The carbon nano tube and the graphene form stable combination, and the copper nano particles enable the graphene to have high crystallinity through in-situ catalytic reaction and have higher combination strength between the graphene and the graphene, so that the composite reinforced phase with stable performance is prepared. And then, the composite reinforcing phase is uniformly distributed in the matrix in a speed-variable ball milling mode, and the structural integrity is protected. And then obtaining the rod-shaped composite material by cold-pressing sintering and hot extrusion molding. Experiments show that the mechanical property of the composite material is remarkably improved, and the composite material has better elongation.
Disclosure of Invention
The invention aims to provide a preparation method of a novel composite reinforcing phase for reinforcing an aluminum matrix composite, which mainly enables graphene to uniformly load carbon nanotubes and copper nanoparticles in an in-situ synthesis mode, and finally realizes the remarkable improvement of the mechanical property of the aluminum matrix composite. In order to achieve the above object, the present invention is achieved by the following technical solutions.
A method for enhancing the mechanical property of an aluminum matrix composite material by the cooperation of a multi-element multi-dimensional enhancing phase comprises the following steps:
(1) In-situ synthesis of a graphene-loaded carbon nanotube and copper nanoparticle composite reinforcing phase: dissolving glucose as a carbon source, copper nitrate trihydrate as a copper source and sodium chloride as a template in deionized water together with the carboxylated carbon nanotubes, and uniformly dispersing to obtain a mixed solution; then, quickly freezing the mixed solution under the assistance of liquid nitrogen, and removing water by adopting a freeze drying technology to obtain composite powder; placing the obtained composite powder in a square boat, then placing the square boat in a constant-temperature area of a high-temperature tube furnace for chemical reaction, wherein the synthesis condition is that the reaction is carried out under hydrogen, the synthesis temperature is 700-800 ℃, the heating rate is 5-10 ℃/min, and after the reaction is finished, the sample is rapidly cooled to obtain mixed powder; washing the powder obtained after the reaction with deionized water and performing suction filtration to remove sodium chloride; and finally, carrying out vacuum drying on the obtained powder to obtain the composite reinforced phase of the graphene-loaded carbon nano tube and the copper nano particles.
(2) Molding and preparing the graphene-loaded carbon nanotube and copper nanoparticle synergistically enhanced aluminum matrix composite material: filling the obtained composite reinforcing phase and aluminum powder into a ball milling tank, wherein the ball-material ratio is 10:1, and filling argon gas into the ball milling tank to be used as protective gas; carrying out variable speed ball milling on the composite reinforcing phase and the aluminum powder to ensure that the reinforcing phase is uniformly dispersed in the aluminum powder and the structure is not seriously damaged; and finally, performing cold press molding on the ball-milled powder at 500-600MPa, sintering at the temperature of 600-630 ℃, selecting argon as a protective atmosphere, and performing hot extrusion on the sintered block material at the temperature of 500-600 ℃ to obtain the graphene-loaded carbon nanotube and copper nanoparticle synergistically enhanced aluminum-based composite material.
Drawings
FIG. 1 is a scan, transmission, Raman and infrared test chart of carboxylated carbon nanotubes used in the preparation of the composite reinforcement phase of example 1. The figure shows that the diameter of the carbon nano tube is about 10-30nm, the carbon nano tube contains carboxyl functional groups and more defects, and the outer wall of the carbon nano tube contains a layer of amorphous carbon defects.
fig. 2 is a scanning and transmission diagram of the graphene-supported carbon nanotube and the copper nanoparticle prepared in example 1. From this figure, it can be clearly observed that the carbon nanotubes and the copper nanotubes are supported on the surface of the graphene and are tightly combined with the graphene.
FIG. 3(a) is a Raman spectrum of the composite reinforcing phase prepared in example 1 and a composite powder after ball milling with aluminum powder. It can be seen from the figure that the structure of the reinforcing phase can be effectively protected from being seriously damaged by the variable speed ball milling.
FIG. 3(b) is a scanned photograph of the powder after ball milling in example 1. From this figure it can be seen that the powder after the shift forms slightly cold-welded granules and no significant agglomeration is observed on the surface of the granules.
Fig. 4 is a stress-strain curve of the composite material prepared in example 1 of the present invention and the pure aluminum prepared in comparative example 1.
Detailed Description
The present invention is illustrated below with reference to specific examples, but the present invention is not limited thereto.
Example 1
(1) Firstly, 0.1g of carboxylated carbon nanotubes are placed in 30ml of deionized water and placed in a cell crusher for ultrasonic dispersion for 1h, meanwhile, 0.938g of glucose, 1.812g of copper nitrate and 36.59g of sodium chloride are placed in a beaker, 150ml of deionized water is added, the materials are placed in a magnetic stirrer for uniform mixing, after the carboxylated carbon nanotubes are uniformly dispersed in the water to form a suspension, a dropper is used for dropwise adding the suspension into the solution of the glucose, the copper nitrate and the sodium chloride to form a mixed solution, then the mixed solution is ultrasonically dispersed for 0.5h, then the mixed solution is rapidly frozen under the assistance of liquid nitrogen to prevent the carbon nanotubes from forming clusters, the mixed solution is placed in a refrigerator for freezing for 12h, and finally the mixed solution is dried in a freeze dryer for 24h to obtain powder.
(2) Pouring the composite powder obtained in the step (1) into a square boat, placing the square boat in a tube furnace for chemical synthesis, reacting in a hydrogen environment, wherein the synthesis temperature is 700-800 ℃, the heating rate is 5-10 ℃/min, and rapidly cooling a sample after the reaction is finished to obtain mixed powder. The powder obtained after the reaction was washed with deionized water and filtered with suction to remove sodium chloride. And finally, carrying out vacuum drying on the obtained powder to obtain the composite reinforced phase of the graphene-loaded carbon nano tube and the copper nano particles.
(3) and (3) performing ball milling and mixing on the composite reinforcing phase obtained in the step (2) and 20g of aluminum powder according to the mass fraction of 2.0 wt.%, wherein in the experiment, the particle size of the aluminum powder is 9-11 μm, stearic acid is used as a process control agent, the ball-to-material ratio is 10:1, and an argon gas is filled in a ball milling tank to be used as a protective gas. The mixed powder was first ball milled at 200 revolutions for 3h and then at 400 revolutions for 1.5 h. And (3) carrying out cold pressing on the ball-milled composite powder for 3min at the pressure of 500 and the pressure of 600MPa to obtain the block composite powder. And then sintering the block composite powder at the temperature of 600-550 ℃ for 1h in an argon environment, and performing hot extrusion on the obtained block composite material at the temperature of 500-550 ℃ to obtain the graphene-loaded carbon nanotube and copper nanoparticle synergistically enhanced aluminum-based composite material.
(4) And (4) cutting the extruded rod-shaped composite material obtained in the step (3) to obtain a tensile sample, and performing mechanical property test.
The tensile strength of the graphene-supported carbon nanotube and copper nanoparticle reinforced aluminum matrix composite material prepared in the example in the cold-pressed sintering-hot extrusion state is 340MPa, and the elongation is 15.4%, and the result is shown in the example 1 curve in fig. 4.
Comparative example 1
(1) Putting 20g of aluminum powder into a ball milling tank for ball milling, wherein the particle size of the aluminum powder is 9-11 mu m, stearic acid is used as a process control agent, the ball-to-material ratio is 10:1, and argon is used as protective gas. The aluminum powder was first ball milled at 200 revolutions for 3 hours followed by 1.5 hours at 400 revolutions. And (3) carrying out cold pressing on the ball-milled aluminum powder for 3min at the pressure of 500 and the pressure of 600MPa to obtain block aluminum powder. And then sintering the block aluminum powder at the temperature of 600-630 ℃ for 1h in an argon environment to obtain a sintered aluminum block. Then carrying out hot extrusion on the obtained sintered aluminum block at the temperature of 500-550 ℃ to obtain a rod-shaped pure aluminum material;
(2) And (2) cutting the extruded rod-shaped pure aluminum material obtained in the step (1) to obtain a tensile sample, and performing mechanical property test.
The tensile strength of the pure aluminum prepared by the comparative example in the cold-pressed sintering-hot-pressed state is 150MPa, the elongation is 21.6%, and the result is shown in the curve of the comparative example 1 in FIG. 4.
Claims (2)
1. a method for enhancing the mechanical property of an aluminum matrix composite material by the cooperation of a multi-element multi-dimensional enhancing phase comprises the following steps:
(1) In-situ synthesis of a graphene-loaded carbon nanotube and copper nanoparticle composite reinforcing phase: dissolving glucose as a carbon source, copper nitrate trihydrate as a copper source and sodium chloride as a template in deionized water together with the carboxylated carbon nanotubes, and uniformly dispersing to obtain a mixed solution; then, quickly freezing the mixed solution under the assistance of liquid nitrogen, and removing water by adopting a freeze drying technology to obtain composite powder; placing the obtained composite powder in a square boat, then placing the square boat in a constant-temperature area of a high-temperature tube furnace for chemical reaction, wherein the synthesis condition is that the reaction is carried out under hydrogen, the synthesis temperature is 700-800 ℃, the heating rate is 5-10 ℃/min, and after the reaction is finished, the sample is rapidly cooled to obtain mixed powder; washing the powder obtained after the reaction with deionized water and performing suction filtration to remove sodium chloride; and finally, carrying out vacuum drying on the obtained powder to obtain the composite reinforced phase of the graphene-loaded carbon nano tube and the copper nano particles.
(2) Molding and preparing the graphene-loaded carbon nanotube and copper nanoparticle synergistically enhanced aluminum matrix composite material: filling the obtained composite reinforcing phase and aluminum powder into a ball milling tank, wherein the ball-material ratio is 10:1, and filling argon gas into the ball milling tank to be used as protective gas; carrying out variable speed ball milling on the composite reinforcing phase and the aluminum powder to ensure that the reinforcing phase is uniformly dispersed in the aluminum powder and the structure is not seriously damaged; and finally, performing cold press molding on the ball-milled powder at 500-600MPa, sintering at the temperature of 600-630 ℃, selecting argon as a protective atmosphere, and performing hot extrusion on the sintered block material at the temperature of 500-600 ℃ to obtain the graphene-loaded carbon nanotube and copper nanoparticle synergistically enhanced aluminum-based composite material.
2. The method as claimed in claim 1, wherein the glucose, the copper nitrate and the sodium chloride are used according to a mass ratio of 1:1-3: 20-80.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2022127941A1 (en) * | 2020-12-18 | 2022-06-23 | 江苏大学 | Graphene- and in-situ nanoparticle-reinforced aluminum-based composite material and preparation method |
| CN114799156A (en) * | 2022-05-13 | 2022-07-29 | 深圳市金石三维打印科技有限公司 | Method for preparing carbon nano tube reinforced aluminum matrix composite material through metal 3D printing |
| CN115418522A (en) * | 2022-04-27 | 2022-12-02 | 合肥工业大学 | Porosity-controllable copper-based wide-temperature-range liquid-solid synergistic self-lubricating composite material and preparation method thereof |
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| US20190122783A1 (en) * | 2017-10-20 | 2019-04-25 | Yazaki Corporation | Aluminum based composite material, electric wire using the same, and manufacturing method of aluminum based composite material |
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Cited By (4)
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Application publication date: 20191206 |