CN108326311B - Continuous extrusion preparation method of graphene aluminum alloy wire - Google Patents

Continuous extrusion preparation method of graphene aluminum alloy wire Download PDF

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CN108326311B
CN108326311B CN201711423075.0A CN201711423075A CN108326311B CN 108326311 B CN108326311 B CN 108326311B CN 201711423075 A CN201711423075 A CN 201711423075A CN 108326311 B CN108326311 B CN 108326311B
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graphene
extrusion
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powder
aluminum alloy
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CN108326311A (en
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马冰
卢科伟
王杰丰
王成军
钟小勇
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Xinjiang Xijin Graphene Technology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/20Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/22Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F5/00Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • B22F5/12Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of wires
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/0408Light metal alloys
    • C22C1/0416Aluminium-based alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/05Mixtures of metal powder with non-metallic powder
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium
    • C22C21/06Alloys based on aluminium with magnesium as the next major constituent
    • C22C21/08Alloys based on aluminium with magnesium as the next major constituent with silicon
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10Processes characterised by the sequence of their steps

Abstract

The invention provides a continuous extrusion preparation method of a graphene aluminum alloy wire. The alloy composite material prepared by the technical scheme provided by the invention has both the strength of the alloy and the conductivity of pure aluminum; the structure uniformity is good, and the performance stability is good; the material utilization rate is high and can generally reach 95 percent; the temperature is raised by utilizing the heat generated by friction, heating is not needed, and energy is saved; the working procedures are less, the production efficiency is high, and the product yield is high; the continuous production of the product can be realized without interval time; is suitable for mass production and small-batch multi-variety production; the product has good performance, high dimensional accuracy and good smoothness.

Description

Continuous extrusion preparation method of graphene aluminum alloy wire
Technical Field
The invention relates to a preparation method of a composite material, in particular to a continuous extrusion preparation method of a graphene aluminum alloy wire.
Background
With the improvement of power transmission and transformation technology and the development of power transmission and transformation lines, more and more large spans need to use wires which can not only transmit large current, but also bear large tension. Aluminum alloy conductors show the advantages in this respect, and have exclusive advantages in long-distance, large-span and ultrahigh-voltage transmission. At present, the materials of the aluminum alloy wire comprise pure aluminum and aluminum-magnesium-silicon alloy, but the mechanical property and the electrical property of the pure aluminum and the aluminum-magnesium-silicon alloy are low in matching performance. Pure aluminum has good conductivity but low strength; due to the addition of alloy elements such as Mg, Si and the like in the aluminum-magnesium-silicon alloy, the strength of the material is improved, and the conductivity is reduced. In recent years, as the suspension span of overhead transmission lines becomes larger, higher requirements are made on the performance of aluminum conductor cables. Therefore, it is necessary to develop a new aluminum conductor cable with high strength and good conductivity.
Graphene is a two-dimensional nanomaterial composed of carbon atoms, and is in a single-layer sheet structure (with a thickness of only a few nanometers). Due to the unique two-dimensional honeycomb crystal structure and extremely high bond strength, graphene is the hardest nano material with the highest specific strength in the world, and the strength of the graphene reaches 130GPa, the Young modulus is about 1100GPa, and the breaking strength is about 125 GPa. More importantly, graphene is also the material with the lowest resistivity in the world (the resistivity is only about 10n Ω · m), and the conductivity reaches 200% IACS. Therefore, the graphene/aluminum composite material is prepared by utilizing the high strength and good conductivity of the graphene and compounding the graphene/aluminum composite material with pure aluminum or aluminum composite material, and is expected to be used for improving the strength and conductivity of the aluminum cable, so that the mechanical property and the electrical property of the aluminum conductor are better matched, and the urgent requirements of overhead power transmission lines on novel aluminum conductor cables with high strength and good conductivity are met.
The preparation method of the graphene aluminum wire comprises a melt casting method and a powder metallurgy method. By adopting the traditional melting casting method, due to the large density difference and the non-wetting interface, the graphene is difficult to be uniformly dispersed in the aluminum liquid, and in addition, the graphene and the aluminum liquid are likely to have high-temperature interface reaction in the material preparation process to generate Al4C3Brittle phases, deteriorating material properties. One disadvantage of the conventional powder metallurgy method is that the discontinuity of production, the limited length of the wire, and a series of auxiliary operations such as separating and pressing the blank and filling the blank between the front and rear blank extrusionAnd the production efficiency of the aluminum wire is influenced. Therefore, in order to realize the engineering application of the graphene aluminum conductor and adapt to the large-scale production of aluminum conductor cable products, the existing process level needs to be broken through, and a batch production process which is low in cost and can realize continuous production is created.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention organically combines the traditional powder metallurgy method and the continuous extrusion method, provides a continuous extrusion method for preparing the graphene alloy composite material, and creatively realizes the continuous production of the graphene alloy composite wire. The graphene/aluminum mixed powder is used as a blank, so that friction heating between the powder and the surface of a tool is obvious during continuous extrusion, and the friction force between the powder and the tool is skillfully utilized. Therefore, the temperature of the deformation zone can be increased by 400-500 ℃ without external heating of the graphene alloy powder, and the pressure reaches 1000MPa, so that the high-density low-porosity preparation of the graphene aluminum conductor is realized.
The purpose of the invention is realized by adopting the following technical scheme:
a continuous extrusion preparation method of a graphene aluminum alloy wire comprises the following steps:
(1) weighing graphene and alloy powder of-200-400 meshes;
(2) carrying out ultrasonic dispersion on graphene in an alcohol solution for 0.5-1.0 h to obtain a graphene and alcohol mixed solution;
(3) adding alloy powder into the graphene and alcohol mixed solution in batches, mixing for 1-2 hours at the rotating speed of 100-500 r/min and the temperature of 40-60 ℃ to obtain semi-solid pasty graphene and alloy mixed powder;
(4) carrying out vacuum degassing and continuous extrusion on the mixed powder of graphene and alloy;
the alloy comprises the following components in percentage by mass: 0.1% of Cu; 4.0-4.9% of Mg; si, 0.4%; 0.15 percent of Ti; 0.4 percent of Fe; 0.25 percent of Zn; 0.40-1.0% of Mn; 0.05-0.25% of Cr; the balance of Al;
the continuous extrusion equipment comprises an extrusion module and a powder degassing module; the extrusion module comprises an extrusion wheel 1 and an arc shoe base 2 which is positioned at the tail end of a feed inlet 3 and is matched with the cross section of one side of the extrusion wheel 1, wherein the feed inlet 3 is arranged above the extrusion wheel 1, a powder heating and degassing device is arranged between the extrusion wheel 1 and the feed inlet 3, the arc length is smaller than that of a semicircle of the extrusion wheel 1, and an extrusion die 5 and a stop block 4 are sequentially arranged between the tail ends of contact parts of the extrusion wheel 1 and the shoe base 2 along an arc.
According to the first preferable scheme of the continuous extrusion preparation method of the graphene aluminum alloy wire, in the step (1), graphene accounts for 0.5-1.0% of the total mass of the composite material.
In the second preferable scheme of the continuous extrusion preparation method of the graphene aluminum alloy wire, in the step (2), an ultrasonic cell crushing instrument is adopted for ultrasonic dispersion, and 60-70% of graphene with less than 10 layers is obtained.
A third preferred scheme of the continuous extrusion preparation method of the graphene aluminum alloy wire is that in the step (3), alloy powder is added at a speed of 100-150 g/10 min.
A fourth preferred scheme of the continuous extrusion preparation method of the graphene aluminum alloy wire is that in the step (4), vacuum degassing is carried out at the flow rate of 1.0-5.0L/min, the temperature of 300-400 ℃ and the vacuum degree of 2.0-5.0 x 10 < -3 > Pa.
According to a fifth preferred scheme of the continuous extrusion preparation method of the graphene aluminum alloy wire, in the step (4), continuous extrusion is carried out at the temperature of 300-400 ℃, the rotating speed of an extrusion wheel is 5-15 r/min, and the extrusion ratio is 20-30.
According to a sixth preferred scheme of the continuous extrusion preparation method of the graphene aluminum alloy wire, a groove vertical to the axis of an extrusion wheel is formed in the outer wall of the extrusion wheel (1).
According to a seventh preferred scheme of the continuous extrusion preparation method of the graphene aluminum alloy wire, an extrusion wheel is prepared from the following materials in percentage by mass: 0.32-0.45% of C, 0.8-1.2% of Si, 0.2-0.5% of Mn, 4.75-5.5% of Cr, 1.1-1.75% of Mo1, 0.8-1.2% of V, less than or equal to 0.03% of P, less than or equal to 0.03% of S, and the balance of Fe.
Compared with the closest prior art, the technical scheme provided by the invention has the following excellent effects:
(1) the prepared graphene alloy composite wire has the strength of aluminum alloy and the conductivity of pure aluminum. The strength (240 MPa-260 MPa) is equivalent to that of the traditional aluminum alloy wire, and the resistivity (28.5n omega. m) is equivalent to that of a pure aluminum wire;
(2) the structure uniformity is good, and the performance stability is good;
(3) the material utilization rate is high and can generally reach 95 percent;
(4) the heat generated by friction is utilized to raise the temperature without heating, thereby saving energy;
(5) the working procedures are less, the production efficiency is high, and the product yield is high;
(6) the continuous production of the product can be realized without interval time;
(7) is suitable for mass production and small-batch multi-variety production;
(8) the product has good performance, high dimensional accuracy and good smoothness.
Drawings
FIG. 1 is a schematic view of a continuous extrusion apparatus;
wherein: 1. an extrusion wheel; 2. a boot base; 3. a feed inlet; 4. a stopper; 5. and (5) extruding the die.
Detailed Description
The technical solutions of the present invention will be described in detail with reference to the following embodiments and drawings, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
a preparation method of a graphene-aluminum alloy composite material comprises the following steps:
(1) weighing graphene and aluminum alloy powder of-200-400 meshes, wherein the graphene accounts for 0.5% of the total mass;
(2) carrying out ultrasonic dispersion on graphene in an alcohol solution for 0.5h to obtain a graphene and alcohol mixed solution;
(3) adding the alloy powder into the graphene and alcohol mixed solution in batches, mixing for 2 hours at the rotating speed of 100r/min and the temperature of 40 ℃ to obtain semi-solid pasty graphene and alloy mixed powder;
(4) placing the uniformly mixed graphene and alloy mixed powder at a feeding position of continuous extrusion equipment;
(5) opening a feed valve, and performing dynamic vacuum degassing in the downward flow process of the graphene and alloy mixed powder at a flow rate of 1.0L/min, a heating temperature of 300 ℃ and a vacuum degree of 2.0 × 10-3Pa;
(6) And continuously extruding the graphene and alloy mixed powder subjected to vacuum degassing to obtain the graphene alloy wire. The extrusion temperature is 300 ℃, the rotating speed of an extrusion wheel is 5r/min, and the extrusion ratio is 20.
Example 2:
a preparation method of a graphene-aluminum alloy composite material comprises the following steps:
(1) weighing graphene and alloy powder with a particle size of-200-400 meshes, wherein the graphene accounts for 1.0% of the total mass;
(2) carrying out ultrasonic dispersion on graphene in an alcohol solution for 1.0h to obtain a graphene and alcohol mixed solution;
(3) adding the alloy powder into the graphene and alcohol mixed solution in batches, mixing for 1h at the rotating speed of 500r/min and the temperature of 60 ℃ to obtain semi-solid pasty graphene alloy mixed powder;
(4) placing the uniformly mixed graphene alloy powder at a feeding position of continuous extrusion equipment;
(5) opening a feed valve, and performing dynamic vacuum degassing in the downward flow process of the graphene alloy mixed powder at a flow rate of 5.0L/min, a heating temperature of 400 ℃ and a vacuum degree of 5.0 multiplied by 10-3Pa;
(6) And continuously extruding the graphene alloy powder subjected to vacuum degassing to obtain the graphene alloy wire. The extrusion temperature is 400 ℃, the rotating speed of an extrusion wheel is 15r/min, and the extrusion ratio is 30.
Example 3:
a preparation method of a graphene-aluminum alloy composite material comprises the following steps:
(1) weighing graphene and aluminum alloy powder of-200-400 meshes, wherein the graphene accounts for 0.7% of the total mass;
(2) carrying out ultrasonic dispersion on graphene in an alcohol solution for 1.5h to obtain a graphene and alcohol mixed solution;
(3) adding the alloy powder into the mixed solution of graphene and alcohol in batches, mixing for 1.5h at the rotating speed of 250r/min and the temperature of 50 ℃ to obtain semi-solid pasty graphene alloy mixed powder;
(4) placing the uniformly mixed graphene alloy powder at a feeding position of continuous extrusion equipment;
(5) opening a feed valve, and performing dynamic vacuum degassing in the downward flow process of the graphene alloy mixed powder at a flow rate of 3.5L/min, a heating temperature of 350 ℃ and a vacuum degree of 3.5 multiplied by 10-3Pa;
(6) And continuously extruding the graphene alloy powder subjected to vacuum degassing to obtain the graphene alloy wire. The extrusion temperature is 350 ℃, the rotation speed of an extrusion wheel is 10r/min, and the extrusion ratio is 25.
The alloy in the above embodiment contains the following components in percentage by mass: 0.1% of Cu; 4.0-4.9% of Mg; si, 0.4%; 0.15 percent of Ti; 0.4 percent of Fe; 0.25 percent of Zn; 0.40-1.0% of Mn; 0.05-0.25% of Cr; the balance being Al.
As shown in fig. 1, an annular channel composed of a groove with a rectangular cross section and a fixed shoe on a rotating extrusion wheel functions as an extrusion cylinder in a common extrusion method, and when the extrusion wheel rotates, graphene alloy mixed powder is continuously fed by means of friction force on a groove wall to realize continuous extrusion, so that a graphene alloy wire with unlimited length is obtained.
The extrusion wheel is made of materials containing the following components in percentage by mass: 0.32-0.45% of C, 0.8-1.2% of Si, 0.2-0.5% of Mn, 4.75-5.5% of Cr, 1.1-1.75% of Mo, 0.8-1.2% of V, less than or equal to 0.03% of P, less than or equal to 0.03% of S, and the balance of Fe.
The performance analysis of the products prepared in the above examples shows that the wire specifications are all 3.0-4.0 mm diameter wires, and the results are shown in the following table 1:
TABLE 1 comparison of the performance of the inventive wires with conventional aluminum wires
Figure BDA0001523413950000051
Compared with the traditional aluminum alloy conductor, the graphene/aluminum composite conductor prepared by the invention can meet the tensile strength of 240-260 MPa, the resistivity can be reduced to 28.0-28.5 n omega-m, the elongation is improved to a certain extent, and the matching degree of the mechanical property and the electrical property is better. The method can obviously reduce the power line loss of the medium-low voltage overhead conductor and the copper material consumption of the medium-low voltage overhead conductor, and has wide application prospect and obvious economic and social benefits.
Finally, it should be noted that: the above embodiments are only intended to illustrate the technical solution of the present invention and not to limit the same, and it should be understood by those skilled in the art that the specific embodiments of the present invention can be modified or substituted with equivalents with reference to the above embodiments, and any modifications or equivalents without departing from the spirit and scope of the present invention should be covered by the claims of the present invention.

Claims (5)

1. A continuous extrusion preparation method of a graphene aluminum alloy wire is characterized by comprising the following steps:
(1) weighing graphene and alloy powder of-200-400 meshes;
(2) ultrasonically dispersing the graphene in an alcohol solution for 0.5-1.0 h to obtain a graphene and alcohol mixed solution;
(3) adding alloy powder into the graphene and alcohol mixed solution in batches, mixing for 1-2 hours at the rotating speed of 100-500 r/min and the temperature of 40-60 ℃ to obtain semi-solid pasty graphene and alloy mixed powder;
(4) carrying out vacuum degassing and continuous extrusion on the graphene and alloy mixed powder;
the alloy comprises the following components in percentage by mass: 0.1% of Cu; 4.0-4.9% of Mg; si, 0.4%; 0.15 percent of Ti; 0.4 percent of Fe; 0.25 percent of Zn; 0.40-1.0% of Mn; 0.05-0.25% of Cr; the balance of Al;
wherein the continuous extrusion equipment comprises an extrusion module and a powder degassing module; the extrusion module comprises an extrusion wheel (1) and an arc shoe base (2); the arc shoe base (2) is positioned at the tail end of the feed port (3); the outer surface of one side of the extrusion wheel (1) is matched with the arc-shaped shoe base (2); the feeding hole (3) is arranged above the extrusion wheel (1), a powder heating and degassing device is arranged between the extrusion wheel (1) and the feeding hole (3), the arc length of the arc shoe base (2) contacted with the extrusion wheel (1) is smaller than the arc length of a semicircle of the extrusion wheel (1), and an extrusion die (5) and a stop block (4) are sequentially arranged between the tail ends of the contact parts of the extrusion wheel (1) and the arc shoe base (2) along an arc;
in the step (3), adding the alloy powder at a speed of 100-150 g/10 min;
in the step (4), the vacuum degassing is carried out at a flow rate of 1.0-5.0L/min, a temperature of 300-400 ℃ and a vacuum degree of 2.0-5.0 x 10 < -3 > Pa;
in the step (4), the continuous extrusion is carried out at the temperature of 300-400 ℃, the rotating speed of an extrusion wheel is 5-15 r/min, and the extrusion ratio is 20-30.
2. The continuous extrusion preparation method of the graphene aluminum alloy wire according to claim 1, wherein in the step (1), graphene accounts for 0.5-1.0% of the total mass of the composite material.
3. The continuous extrusion preparation method of the graphene aluminum alloy wire according to claim 1, wherein in the step (2), the ultrasonic dispersion is performed by using an ultrasonic cell pulverization instrument, and the graphene with 10 layers or less accounts for 60-70%.
4. The continuous extrusion preparation method of the graphene aluminum alloy wire according to claim 1, wherein the outer wall of the extrusion wheel (1) is provided with a groove perpendicular to the axial line of the extrusion wheel.
5. The continuous extrusion preparation method of the graphene aluminum alloy wire according to claim 1, wherein the extrusion wheel is made of a material containing the following components in percentage by mass: 0.32-0.45% of C, 0.8-1.2% of Si, 0.2-0.5% of Mn, 4.75-5.5% of Cr, 1.1-1.75% of Mo, 0.8-1.2% of V, less than or equal to 0.03% of P, less than or equal to 0.03% of S, and the balance of Fe.
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