CN110129606B - Preparation method of directionally arranged carbon nanotube reinforced aluminum-based composite wire - Google Patents
Preparation method of directionally arranged carbon nanotube reinforced aluminum-based composite wire Download PDFInfo
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- 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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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
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- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
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- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
- C22C2026/002—Carbon nanotubes
Abstract
The invention discloses a preparation method of a directional arrangement carbon nano tube reinforced aluminum-based composite wire, belonging to the technical field of composite material preparation. The method comprises the steps of uniformly mixing the carbon nano tube and pure aluminum powder, and extruding by using continuous extrusion equipment to obtain a carbon nano tube reinforced aluminum matrix composite round rod; then, repeatedly extruding the obtained composite round rod for a plurality of times; then, drawing the repeatedly extruded composite round rod for a plurality of times to obtain a carbon nano tube reinforced aluminum matrix composite wire rod with a circular cross section; and finally, annealing the drawn wire to obtain a finished wire. The invention makes the carbon nano tube uniformly and directionally arranged in the aluminum-based composite material through a series of processes of mixed powder preparation, continuous extrusion, drawing, annealing and the like, and finally prepares the carbon nano tube reinforced aluminum-based composite wire with good mechanical, electric and thermal conductivity.
Description
Technical Field
The invention relates to a preparation method of a Carbon Nano Tube (CNTs) reinforced aluminum-based composite wire rod in oriented arrangement, belonging to the technical field of composite material preparation.
Background
With the improvement of power transmission technology and the development of power transmission lines, more and more large-span power transmission lines need to use wires which can transmit large current and bear large tension. Aluminum conductors have shown increasing superiority in this respect, and are widely used in long-distance, large-span, and ultra-high voltage power transmission. The aluminum has a face-centered cubic structure, has good shaping and is easy to process; the conductivity of the aluminum is good, and the conductivity is about 60 percent of that of the annealed copper; a layer of compact aluminum oxide film can be formed on the surface of the aluminum, so that the aluminum oxide film is prevented from being oxidized continuously, and the aluminum oxide film has good oxidation resistance and corrosion resistance; in addition, aluminum is light and cheaper than copper. Therefore, aluminum wire is considered as the most promising alternative material for copper wire. At present, the existing aluminum alloy conductor material has low matching property of mechanical property and electrical property, so that the development of an aluminum conductor cable with high strength and good conductivity is urgently needed.
The carbon nano tube reinforced aluminum-based composite material is expected to obtain excellent comprehensive performance of light weight, high strength and high conductivity, and the preparation method mainly comprises a powder metallurgy method, a casting method, an infiltration method, an in-situ synthesis method and the like. Different preparation methods have different damages to the carbon nano tube structure, different reaction degrees of the carbon nano tube and the matrix aluminum, and different dispersion degrees and distribution conditions of the carbon nano tube in the matrix. For example, in the casting method, since the density difference between the carbon nanotube and the aluminum matrix is large and the interface is not wet, the carbon nanotube is difficult to be uniformly dispersed in the matrix, and in addition, a high temperature interface reaction may occur during the preparation process to generate a large amount of aluminum carbide (Al)4C3) Embrittlement adversely reduces the material properties. The traditional powder metallurgy method can uniformly disperse the carbon nano-tube into the aluminum matrix, but the method has the defects of discontinuous production, limited wire length, complex preparation process and the like, and the production efficiency and the large-scale use of the composite material are influenced. Other innovative methods such as a stirring friction method, an in-situ growth composite method, a spraying method, a molecular-level blending method and the like can also disperse the carbon nanotubes into the aluminum matrix, but the methods are still basically in a laboratory exploration stage, and the processes are complicated and difficult to be applied in a large scale. It should be noted that the existing method for preparing carbon nanotube reinforced aluminum matrix composite material can not realize the directional arrangement of carbon nanotubes basically, and can not fully exert the excellent mechanical, electrical and thermal performance advantages of carbon nanotubes, and the reinforcing efficiency is greatly reduced. In order to further improve the strengthening efficiency in the carbon nano tube and the comprehensive performance of the composite material, reduce the process flow and the costLow production cost, and promotion of large-scale production and application, and further innovation of a preparation method of the carbon nano tube reinforced aluminum matrix composite material is needed.
Disclosure of Invention
The invention aims to provide a preparation method of a directional arrangement carbon nano tube reinforced aluminum-based composite wire; the method combines the processes of powder metallurgy, continuous extrusion, drawing, annealing and the like to realize the directional arrangement of the carbon nano tubes in the aluminum matrix, and specifically comprises the following steps:
(1) preparing mixed powder of carbon nano tube and pure aluminum powder by adopting a mechanical ball milling method for later use.
(2) Continuously extruding the mixed powder of the carbon nano tube and the pure aluminum obtained in the step (1) to obtain the productφ8-12 mm carbon nano tube reinforced pure aluminum round rod.
(3) Carrying out continuous repeated extrusion on the carbon nano tube reinforced pure aluminum round rod obtained in the step (2) for 1-5 times to obtain the carbon nano tube reinforced pure aluminum round rodφ4-8 mm composite round rod, and further uniformly dispersing and directionally arranging the carbon nano tubes.
(4) Performing multi-pass drawing on the round rod obtained in the step (3) by adopting a drawing machine to obtain the round rodφ1-3 mm composite wire, further promoting the uniform dispersion and directional arrangement of the carbon nano tube.
(5) And (4) annealing the wire rod obtained in the step (4) to obtain the directionally arranged carbon nano tube reinforced aluminum matrix composite wire rod.
Preferably, the average diameter of the pure aluminum powder is 10-40 μm, and the diameter and the length of the carbon nanotube are 10-30nm and 5-30 μm respectively.
Preferably, the mass percent of the carbon nano tube in the mixed powder of the carbon nano tube and the pure aluminum is 1-3 wt%.
Preferably, in the step (1) of the invention, the two powders are uniformly mixed by a ball milling mode, the ball-to-material ratio in the ball milling process is 10:1, the rotating speed is 100-.
Preferably, in step (2) of the present invention, the mixed powder is added at a rate of 50 to 100 g/min.
Preferably, in steps (2) and (3) of the present invention (heat is generated by friction between the powder and the tool surface during continuous extrusion without external heating), the rotation speed of the extrusion wheel is 5-20 r/min.
Preferably, in the step (4) of the present invention, the drawing speed is 3 to 12 m/min.
Preferably, in the step (5) of the present invention, the annealing temperature of the composite wire is 150-.
The principle of the invention is as follows: the extrusion die cavity is positioned at the side of the extrusion wheel, and the uniformly mixed powder obtained at the early stage enters the extrusion die cavity under the driving of the rotation of the extrusion wheel; under the action of friction force of the extrusion wheel groove, the pressure of the die cavity is increased, the temperature of the powder is raised, and the mixed powder is gradually extruded out of the die to form a composite round rod; during this extrusion process, the CNTs clusters are further broken up and gradually tend to align with the flow of the metal; through multiple times of continuous extrusion, the diameter of the composite round rod is gradually reduced, the density of the composite round rod is gradually increased, and the arrangement of the CNTs in the composite round rod is more consistent. Drawing the continuously extruded composite round rod for multiple times, and further reducing the diameter to form composite wires with different diameters; during the drawing process, the CNTs clusters in the composite material are further dispersed and further arranged in an oriented manner along the drawing direction, and the CNTs are possibly distributed in an end-to-end manner, so that the carbon nano wires are approximately distributed in the aluminum matrix. CNTs as a one-dimensional nano material has a plurality of excellent properties such as light weight, high strength, good electric conductivity and thermal conductivity and the like. The CNTs in the oriented arrangement can improve the electric conduction and heat conduction capability of the composite material to the maximum extent, and can improve the strength of the composite material through load transfer. In addition, the grains in the aluminum matrix are also elongated in the drawing direction during continuous extrusion and drawing, and may form a filament texture, which contributes to the improvement of the strength, electrical and thermal conductivity of the composite material in the drawing direction. Through the final annealing treatment, the point defects and the internal stress generated in the preparation process of the composite material can be eliminated, and the electric conductivity and the heat conductivity of the composite material can be further improved. Therefore, the carbon nano tube reinforced aluminum matrix composite material prepared by the process of the invention is expected to have excellent performances of high strength and high conductivity.
The invention has the beneficial effects that:
(1) the invention organically combines the processes of powder metallurgy, continuous extrusion, drawing, annealing and the like, can ensure that the CNTs are directionally arranged in the aluminum matrix, has good tissue uniformity, and is expected to obtain the CNTs reinforced aluminum matrix composite wire with high strength, good electric conductivity and thermal conductivity.
(2) The method has the advantages of simple process, high production efficiency, energy conservation, consumption reduction and low cost. The CNTs are uniformly dispersed in an aluminum alloy matrix by adopting low-speed ball milling, so that the structural damage degree is small; the mixed powder is directly processed into the composite round rod by adopting continuous extrusion, so that the processes of powder compacting, sintering and secondary heating in the traditional process are reduced; the friction heat generation of the mixed powder and the surface of the extrusion wheel groove can ensure that the temperature of a deformation zone reaches more than 400 ℃ and the extrusion force reaches 1000MPa under the condition of no need of external heating, thereby realizing the high-density preparation of the CNTS reinforced aluminum matrix composite.
Drawings
FIG. 1 is a flow chart of a preparation process
FIG. 2 is a schematic view of a preparation process
FIG. 3 is a schematic view of a continuous extrusion apparatus
FIG. 4 is a transmission electron microscope image of the carbon nanotube-reinforced aluminum matrix composite aligned in an orientation.
FIG. 5 is a schematic structural diagram of an aluminum matrix composite reinforced with aligned carbon nanotubes.
In fig. 3: 1-an extrusion wheel; 2-a boot seat; 3-a feed inlet; 4-a stop block; and 5-extruding the die.
Detailed Description
The present invention is described in further detail below with reference to examples and drawings, but the scope of the present invention is not limited thereto, and other methods of mixing powders, preparing metal matrix composites with aligned carbon nanotubes or subsequent deformation are within the scope of the present invention.
The continuous extrusion equipment used in embodiments 1 to 3 of the present invention is shown in fig. 3, and includes an extrusion wheel 1, a shoe base 2, a feed inlet 3, a stopper 4, and an extrusion die 5, where the feed inlet 3 faces a wheel groove of the extrusion wheel 1, and mixed powder is driven by rotation of the extrusion wheel to enter a die cavity of the extrusion die 5, and the mixed powder is gradually extruded out of the extrusion die 5 under the blocking action of the stopper 4 to form a composite round bar.
Example 1
A preparation method of a directional arrangement carbon nano tube reinforced aluminum-based composite wire specifically comprises the following steps:
(1) 30g of carbon nanotubes (diameter about 10 nm, length about 5 μm) and 2970g of pure aluminum powder (average diameter about 10 μm, purity 99.99%) were weighed in an argon atmosphere glove box and charged into a stainless steel ball mill jar; wherein the mass percent of the carbon nano tube is 1wt%, and the ball-to-material ratio is 10: 1; ball milling is carried out for 6 hours at a rotating speed of 100r/min, and the uniform mixed powder of pure aluminum and the carbon nano tube is obtained.
(2) Adding the mixed powder of the carbon nano tube and the pure aluminum obtained in the step (1) into a continuous extrusion device at the speed of 50 g/min for extrusion for 1 pass to obtain the productφThe carbon nano tube reinforced pure aluminum round rod with the diameter of 8 mm, and the rotating speed of the extrusion wheel is 5 r/min.
(3) Carrying out 1-pass repeated continuous extrusion on the carbon nano tube reinforced pure aluminum round rod obtained in the step (2) at the rotating speed of an extrusion wheel of 5r/min to obtain the carbon nano tube reinforced pure aluminum round rodφ7 mm composite round bar.
(4) Placing the composite round rod obtained in the step (3) on a drawing machine to carry out drawing for 5 times at a speed of 3m/min to obtain the composite round rodφ3 mm of composite wire.
(5) Annealing the composite wire obtained in the step (4) for 3 hours at the temperature of 150 ℃ to obtainφ3 mm of directionally arranged carbon nano tube reinforced aluminum-based composite wire; in the composite wire, CNTs tend to be directionally arranged along the extrusion and drawing directions, as shown in FIG. 5, and part of CNTs form a continuous arrangement mode of end-to-end lap joint; in addition, the crystal grains of the pure aluminum matrix are also elongated along the extrusion and drawing directions, which are beneficial to improving the strength, the electric conductivity and the thermal conductivity of the composite material.
Example 2
A preparation method of a directional arrangement carbon nano tube reinforced aluminum-based composite wire specifically comprises the following steps:
(1) 30g of carbon nanotubes (diameter about 20 nm, length about 15 μm) and 1470g of pure aluminum powder (average diameter about 25 μm, purity 99.99%) were weighed in an argon atmosphere glove box and charged into a stainless steel ball mill jar; wherein the mass percent of the carbon nano tube is 2 wt%, and the ball-to-material ratio is 10: 1; ball milling is carried out for 4 hours at a rotating speed of 200r/min, and the uniform mixed powder of pure aluminum and the carbon nano tube is obtained.
(2) Adding the mixed powder of the carbon nano tube and the pure aluminum obtained in the step (1) into continuous extrusion equipment at the speed of 75 g/min for extrusion for 1 pass to obtain the productφThe carbon nano tube reinforced pure aluminum round rod with the diameter of 10 mm, and the rotating speed of the extrusion wheel is 10 r/min.
(3) Carrying out 3-pass repeated continuous extrusion on the carbon nano tube reinforced pure aluminum round rod obtained in the step (2) at the rotating speed of an extrusion wheel of 10r/min to obtain the carbon nano tube reinforced pure aluminum round rodφ6 mm composite round bar.
(4) Placing the composite round rod obtained in the step (3) on a drawing machine to carry out drawing for 5 times at a speed of 9 m/min to obtain the composite round rodφ2 mm composite wire.
(5) Annealing the composite wire obtained in the step (4) at 200 ℃ for 2h to obtainφ2 mm of directionally arranged carbon nano tube reinforced aluminum-based composite wire. In the composite wire, CNTs tend to be directionally arranged along the extrusion and drawing directions, as shown in FIG. 5, and part of CNTs form a continuous arrangement mode of end-to-end lap joint; in addition, the crystal grains of the pure aluminum matrix are also elongated along the extrusion and drawing directions, which are beneficial to improving the strength, the electric conductivity and the thermal conductivity of the composite material.
Example 3
A preparation method of a directional arrangement carbon nano tube reinforced aluminum-based composite wire specifically comprises the following steps:
(1) 30g of carbon nanotubes (diameter about 30nm and length about 30 μm) and 970g of pure aluminum powder (average diameter about 40 μm and purity 99.99%) are weighed in an argon environment glove box and filled in a stainless steel ball milling tank; wherein the mass percent of the carbon nano tube is 3wt%, and the ball-to-material ratio is 10: 1; ball milling is carried out for 2h at the rotating speed of 300r/min, and the uniform mixed powder of pure aluminum and the carbon nano tube is obtained.
(2) Adding the mixed powder of the carbon nano tube and the pure aluminum obtained in the step (1) into a continuous extrusion device at the speed of 100g/min for extrusion for 1 pass to obtain the productφThe 12 mm carbon nano tube reinforced pure aluminum round rod has the rotating speed of the extrusion wheel of 20 r/min.
(3) Carrying out 5-time repeated continuous extrusion on the carbon nano tube reinforced pure aluminum round rod obtained in the step (2) at the rotating speed of an extrusion wheel of 20r/min to obtain the carbon nano tube reinforced pure aluminum round rodφ4 mm composite round bar.
(4) Placing the composite round rod obtained in the step (3) on a drawing machine to carry out drawing for 4 times at the speed of 12m/min to obtain the composite round rodφ1mm of composite wire.
(5) Annealing the composite wire obtained in the step (4) for 1 h at 250 ℃ to obtainφ1mm of directionally arranged carbon nano tube reinforced aluminum-based composite wire. In the composite wire, CNTs tend to be directionally arranged along the extrusion and drawing directions, as shown in FIG. 5, and part of CNTs form a continuous arrangement mode of end-to-end lap joint; in addition, the crystal grains of the pure aluminum matrix are also elongated along the extrusion and drawing directions, which are beneficial to improving the strength, the electric conductivity and the thermal conductivity of the composite material.
FIG. 4 is a transmission electron microscope image of the carbon nanotube-reinforced aluminum matrix composite aligned in example 3, from which it can be seen that: CNTs are distributed in aluminum matrix grain boundaries and tend to be directionally arranged along the extrusion and drawing directions, aluminum matrix grains are also elongated along the extrusion and drawing directions, and similar structures exist in the embodiment 1 and the embodiment 2.
Claims (8)
1. A preparation method of a directional arrangement carbon nano tube reinforced aluminum-based composite wire is characterized by comprising the following steps:
(1) preparing mixed powder of carbon nano tube and pure aluminum powder by adopting a mechanical ball milling method for later use;
(2) continuously extruding the mixed powder of the carbon nano tube and the pure aluminum obtained in the step (1) to obtain the productφ8-12 mm carbon nanotube reinforced pure aluminum round rod;
(3) carrying out continuous repeated extrusion on the carbon nano tube reinforced pure aluminum round rod obtained in the step (2) for 1-5 times to obtain the carbon nano tube reinforced pure aluminum round rodφ4-8 mm composite round rod, and further uniformly dispersing and directionally arranging the carbon nano tubes;
(4) drawing the round bar obtained in the step (3) by a drawing machineDrawing in multiple passes to obtainφ1-3 mm composite wires, further promoting the uniform dispersion and directional arrangement of the carbon nanotubes;
(5) and (4) annealing the wire rod obtained in the step (4) to obtain the directionally arranged carbon nano tube reinforced aluminum matrix composite wire rod.
2. The method for preparing the aligned carbon nanotube-reinforced aluminum-based composite wire according to claim 1, wherein: the average diameter of the pure aluminum powder is 10-40 μm, and the diameter and the length of the carbon nano tube are 10-30nm and 5-30 μm respectively.
3. The method for preparing the aligned carbon nanotube-reinforced aluminum-based composite wire according to claim 1, wherein: the mass percent of the carbon nano tube in the mixed powder of the carbon nano tube and the pure aluminum is 1-3 wt%.
4. The method for preparing the aligned carbon nanotube-reinforced aluminum-based composite wire according to claim 1, wherein: the two kinds of powder are uniformly mixed by a mechanical ball milling method in the step (1), the ball-material ratio in the ball milling process is 10:1, the rotating speed is 100-.
5. The method for preparing the aligned carbon nanotube-reinforced aluminum-based composite wire according to claim 1, wherein: in the step (2), the adding speed of the mixed powder is 50-100 g/min.
6. The method for preparing the aligned carbon nanotube-reinforced aluminum-based composite wire according to claim 1, wherein: the speed of the extrusion wheel in the steps (2) and (3) is 5-20 r/min.
7. The method for preparing the aligned carbon nanotube-reinforced aluminum-based composite wire according to claim 1, wherein: in the step (4), the drawing speed is 3-12 m/min.
8. The method for preparing the aligned carbon nanotube-reinforced aluminum-based composite wire according to claim 1, wherein: in the step (5), the annealing temperature of the composite wire is 150-250 ℃, and the annealing time is 1-3 h.
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