CN108326314B - Preparation method of composite material and continuous extrusion equipment thereof - Google Patents

Preparation method of composite material and continuous extrusion equipment thereof Download PDF

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CN108326314B
CN108326314B CN201711424746.5A CN201711424746A CN108326314B CN 108326314 B CN108326314 B CN 108326314B CN 201711424746 A CN201711424746 A CN 201711424746A CN 108326314 B CN108326314 B CN 108326314B
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graphene
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CN108326314A (en
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陈长科
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
    • 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
    • C22C1/05Mixtures 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
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/02Ferrous alloys, e.g. steel alloys containing silicon
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/04Ferrous alloys, e.g. steel alloys containing manganese
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/18Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/22Ferrous alloys, e.g. steel alloys containing chromium with molybdenum or tungsten
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/18Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/24Ferrous alloys, e.g. steel alloys containing chromium with vanadium
    • 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
    • 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
    • B22F2999/00Aspects linked to processes or compositions used in powder metallurgy

Abstract

The invention provides a preparation method of a composite material and continuous extrusion equipment thereof. The graphene alloy wire prepared by the technical scheme provided by the invention has the strength and the conductivity of the alloy; 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

Preparation method of composite material and continuous extrusion equipment thereof
Technical Field
The invention relates to a preparation method of a composite material, in particular to a preparation method of a composite material and a continuous extrusion device thereof.
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 using conventional powder metallurgy is the production discontinuity, the limited wire length, anda series of auxiliary operations such as separating excess pressure and filling blanks are needed between the extrusion of the rear blanks, and the production efficiency of the aluminum conductor 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 wire. The graphene alloy 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 preparation of the high-density low-porosity graphene alloy wire is realized.
The purpose of the invention is realized by adopting the following technical scheme:
a method of making a composite material, the method comprising the steps of:
(1) emulsifying graphene with alcohol;
(2) ultrasonically dispersing graphene emulsified by alcohol for 0.5-1.0 h to obtain a graphene and alcohol mixed solution;
(3) adding alloy powder of-200-400 meshes into the mixed solution of graphene and alcohol in batches, and 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/alloy mixed powder;
(4) carrying out vacuum degassing on the graphene/alloy mixed powder and then continuously extruding;
the alloy comprises the following components in percentage by mass: less than or equal to 0.25 percent of Si, less than or equal to 0.4 percent of Fe, less than or equal to 0.05 percent of Cu, less than or equal to 0.05 percent of Mn, less than or equal to 0.07 percent of Zn, less than or equal to 0.05 percent of Ti, and the balance of Al.
According to a first preferable scheme of the preparation method of the composite material, in the step (1), graphene accounts for 0.5-1.0% of the total mass of the composite material.
In a second preferable scheme of the preparation method of the composite material, in the step (2), an ultrasonic cell pulverization instrument is adopted for ultrasonic dispersion, and 60-70% of graphene with less than 10 layers is obtained.
In the third preferred scheme of the preparation method of the composite material, in the step (2), in the step (3), alloy powder is added at the speed of 100-150 g/10 min.
In a fourth preferred scheme of the preparation method of the composite material, in the step (2), in the step (4), vacuum degassing is performed 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.
According to a fifth preferred scheme of the preparation method of the composite material, in the step (2), 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.
A continuous extrusion device of a composite material preparation method 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, 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.
In a first preferred scheme of the continuous extrusion equipment, the outer wall of the extrusion wheel 1 is provided with a groove which is vertical to the axis of the extrusion wheel.
In a second preferred embodiment of the continuous extrusion apparatus, the extrusion wheel is made of a material comprising, in mass percent: 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.
Compared with the closest prior art, the technical scheme provided by the invention has the following excellent effects:
(1) the prepared graphene alloy wire has the strength and the conductivity of the alloy, the strength (240-260 MPa) is equivalent to that of the traditional aluminum wire, and the resistivity (28.5n omega. m) is equivalent to that of the 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 method of making a composite material, the method comprising the steps of:
(1) weighing graphene and alloy powder with a particle size 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 2h at the rotating speed of 100r/min and the temperature of 40 ℃ 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 1.0L/min, a heating temperature of 300 ℃ and a vacuum degree of 2.0 × 10-3Pa;
(6) And continuously extruding the graphene alloy 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 method of making a composite material, the method comprising the steps of:
(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/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 method of making a composite material, the method comprising the steps of:
(1) weighing graphene and alloy powder with a particle size 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 graphene/alcohol mixed solution in batches, and mixing for 1.5 hours 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 each embodiment comprises the following components in percentage by mass: less than or equal to 0.25 percent of Si, less than or equal to 0.4 percent of Fe, less than or equal to 0.05 percent of Cu, less than or equal to 0.05 percent of Mn, less than or equal to 0.07 percent of Zn, less than or equal to 0.05 percent of Ti, and the balance of Al.
As shown in fig. 1, an annular channel formed by a groove with a rectangular cross section on a rotating extrusion wheel and a fixed die holder plays a role of an extrusion cylinder in a common extrusion method, and when the extrusion wheel rotates, graphene alloy mixed powder is continuously fed by virtue 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 to 0.45 percent of C, 0.8 to 1.2 percent of Si, 0.2 to 0.5 percent of Mn, 4.75 to 5.5 percent of Cr, 1.1 to 1.75 percent of Mo, 0.8 to 1.2 percent of V, less than or equal to 0.03 percent of P, less than or equal to 0.03 percent of S, and the balance of Fe
The products obtained in the above examples 1 to 3 were analyzed for their properties, and the wire specifications were all wire rods with a diameter of 3.0 to 4.0mm, and the results are shown in the following table 1:
TABLE 1 comparison of the performance of composite wires prepared according to the invention with conventional aluminum wires
Figure BDA0001523764180000051
Compared with the traditional aluminum wire, the graphene alloy composite wire 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 compared with that of a medium-strength aluminum alloy wire, and the matching degree of mechanical property and 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 (3)

1. A method of making a composite material, the method comprising the steps of:
(1) emulsifying graphene with alcohol;
(2) ultrasonically dispersing graphene emulsified by alcohol for 0.5-1.0 h to obtain a graphene and alcohol mixed solution;
(3) adding aluminum alloy powder of-200-400 meshes to the graphene and alcohol mixed solution in batches, and mixing at the rotating speed of 100-500 r/min and the temperature of 40-60 ℃ for 1-2 h to obtain semi-solid pasty graphene/aluminum alloy mixed powder;
(4) carrying out vacuum degassing on the graphene/aluminum alloy mixed powder and then continuously extruding;
the aluminum alloy comprises the following components in percentage by mass: less than or equal to 0.25 percent of Si, less than or equal to 0.4 percent of Fe, less than or equal to 0.05 percent of Cu, less than or equal to 0.05 percent of Mn, less than or equal to 0.07 percent of Zn, less than or equal to 0.05 percent of Ti, and the balance of Al;
in the step (4), the graphene accounts for 0.5-1.0% of the total mass of the composite material;
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;
in the step (3), adding the aluminum 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. A continuous extrusion apparatus for a method of manufacturing a composite material according to claim 1, wherein the continuous extrusion apparatus 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;
the outer wall of the extrusion wheel (1) is provided with a groove vertical to the axial lead of the extrusion wheel.
3. Continuous extrusion apparatus according to claim 2, characterised in that the extrusion wheel is made of a material comprising, in mass percent: 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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CN111331127A (en) * 2018-12-18 2020-06-26 有研工程技术研究院有限公司 Preparation method of graphene/copper composite wire
CN110560501A (en) * 2019-10-17 2019-12-13 大连交通大学 Stepped continuous extrusion device using metal powder as raw material

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CN106566963A (en) * 2016-11-08 2017-04-19 中航装甲科技有限公司 Preparation method and stirring device of aluminum alloy composite armor material

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