WO2023109667A1 - Matériau composite à base de cuivre-graphène modifié par des terres rares, son procédé de préparation et son application - Google Patents

Matériau composite à base de cuivre-graphène modifié par des terres rares, son procédé de préparation et son application Download PDF

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WO2023109667A1
WO2023109667A1 PCT/CN2022/137820 CN2022137820W WO2023109667A1 WO 2023109667 A1 WO2023109667 A1 WO 2023109667A1 CN 2022137820 W CN2022137820 W CN 2022137820W WO 2023109667 A1 WO2023109667 A1 WO 2023109667A1
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copper
graphene
rare earth
composite material
based composite
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PCT/CN2022/137820
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English (en)
Chinese (zh)
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薛冬峰
黄维扬
王鑫
王晓明
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深圳先进技术研究院
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • 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
    • 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
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B60—VEHICLES IN GENERAL
    • B60M—POWER SUPPLY LINES, AND DEVICES ALONG RAILS, FOR ELECTRICALLY- PROPELLED VEHICLES
    • B60M1/00—Power supply lines for contact with collector on vehicle
    • B60M1/12—Trolley lines; Accessories therefor
    • B60M1/13—Trolley wires
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/182—Graphene
    • C01B32/194—After-treatment
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
    • C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
    • C22C32/0021—Matrix based on noble metals, Cu or alloys thereof
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper
    • G—PHYSICS
    • G06—COMPUTING; CALCULATING OR COUNTING
    • G06N—COMPUTING ARRANGEMENTS BASED ON SPECIFIC COMPUTATIONAL MODELS
    • G06N20/00—Machine learning
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • 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
    • H01B1/026—Alloys based on copper
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy

Definitions

  • the invention belongs to the field of materials, in particular to the field of modification of graphene copper-based composite materials, in particular to a rare earth modified graphene copper-based composite material and its preparation method and application.
  • High-strength and high-conductivity copper alloy refers to a class of copper alloy materials that have both high strength and high conductivity, and are widely used in fields such as electric power, electronics, automobiles, home appliances, aerospace, military industry, and nuclear energy.
  • the "Thirteenth Five-Year Plan” pointed out: "In terms of new materials, accelerate the research and development of key strategic materials such as high-strength and high-conductivity copper alloys.”
  • more than 80% of domestic high-end high-strength and high-conductivity copper materials rely on imports, which has become a "stuck neck” problem that restricts the development of corresponding fields in my country.
  • Carbon can form different allotropes due to its valence, including one-dimensional carbon nanotubes, two-dimensional graphene, three-dimensional fullerenes, graphite, carbon fibers, diamonds, etc.
  • These carbon nanomaterials, especially carbon nano Tubes and graphene, due to their excellent intrinsic properties, are expected to be used as reinforcements to achieve ultrahigh conductivity of copper-based composites.
  • rare earth elements are called "industrial monosodium glutamate". Rare earth doping can refine the particle size of copper particles, toughen and strengthen, effectively improve the microstructure and structural defects of copper metal materials, and improve the mechanical strength and resistance of copper-based materials. Corrosive etc.
  • Rare earth modified graphene copper matrix composite material is a composite material that improves its mechanical strength and corrosion resistance without reducing its electrical and thermal conductivity by adding graphene and rare earth elements to copper, which can greatly reduce the contact line and locomotive
  • the loss caused by the sliding contact of the pantograph slide plate to transmit the current can be widely used in the field of high-speed electrified railways, and effectively improve my country's key core technology innovation capabilities.
  • Rare earth resources are important strategic resources in my country, and the high-value utilization of rare earth resources is urgent. With the continuous development of my country's high-tech field, the market capacity and added value of rare earth modified copper-based composite materials will also be further expanded.
  • "Nonferrous Metals Industry Development Plan (2016-2020)” pointed out that high-performance copper-based materials are the key basic materials for the development of high-tech fields in my country. In terms of market, my country's high-end integrated circuits, high-speed rail contact network and various high-performance cutting-edge power transmission copper-based composite materials such as high-conductivity copper alloy strips are heavily dependent on imports.
  • Copper-tin material contact wires and copper-magnesium material contact wires are used on high-speed railways above and above; Germany and Spain use copper-silver material contact wires at speeds of 250-300km/h, and copper-magnesium material contact wires at speeds above 300km/h.
  • the invention provides a rare earth modified graphene copper-based composite material and its preparation method and application.
  • the present invention adopts the intelligent creation technology of rare-earth modified graphene copper-based composite materials by machine learning (analog calculation is based on the model of high-strength and high-conductivity rare-earth modified graphene copper-based composite materials).
  • Copper crystal model and fully consider the influence mechanism of different crystal orientations, different exposed crystal planes and crystal defect density on conductivity, so as to realize the accurate prediction of copper crystal model with ultra-high conductivity.
  • combine DFT calculation with machine learning to study the influence mechanism of the introduction of rare earth elements on the conductivity, strength, hardness, wear resistance and corrosion resistance of copper matrix composites, and establish graphene crystallization in copper nanocrystal materials at different scales.
  • the research on the large-scale application of terminal products of graphene copper-based composite materials can be carried out, which can effectively amplify the copper mirror reaction and establish the macro-preparation process route of graphene copper nanocomposites.
  • the heat exchange between the press die and the extrusion wheel environment, as well as the thermomechanical coupling effect during the molding process can reveal the influence of different molding processes on the performance of end-application products, so as to explore the rules of continuous extrusion molding and realize the optimization of continuous extrusion process parameters. Optimized design.
  • the present invention is based on the following ideas to develop a preparation strategy for rare earth modified graphene copper-based composite materials with high strength and high conductivity: (1) first use machine learning to study the effect of rare earth element introduction on the conductivity, strength, hardness, The impact mechanism of wear resistance and corrosion resistance; (2) Construct a uniform and stable graphene-amine salt-copper ion complex system to effectively solve the problem of poor dispersion of graphene in the copper matrix, and achieve Good interfacial recombination between graphene and copper; (3) preparation of rare earth oxide dispersion-strengthened graphene-copper-based composites with dual nanostructures by mechanical alloying and plasma sintering, establishing and perfecting the plasma sintering mechanism of copper-based materials , performance regulation method and mechanism; (4) further reveal the interfacial recombination mechanism of graphene in the crystallization process of copper crystals, and clarify the wettability mechanism, interfacial bonding law, grain size and distribution of the matrix and reinforcement phase in the
  • a preparation method of rare earth modified graphene copper-based composite material comprising the steps of:
  • the graphene copper-based composite material is ball-milled with the rare earth oxide to obtain a mixed powder, and the obtained mixed powder is subjected to discharge plasma sintering to obtain the rare-earth modified graphene copper-based composite material.
  • the mass ratio of graphite to organic amine is 1:1-1:50;
  • the mass ratio of the first alcohol substance to graphite is 10:1-100:1;
  • the first alcoholic substance and the second alcoholic substance are sec-butanol;
  • the organic amine is selected from one or more of methylamine, ethylenediamine, isopropylamine, isobutylamine, cyclopropylamine, sec-butylamine-tert-butylamine, hexylamine, dodecylamine, hexadecylamine and octadecylamine.
  • the graphite is flake graphite.
  • the concentration of the copper salt in the mixture is 0.5 mol/L-50 mol/L;
  • the percentage of the graphene in the rare earth oxide-modified graphene-copper-based composite material is 0.1wt%-3wt%;
  • the molar ratio of the copper salt to the reducing agent is 1:1-1:10;
  • the copper salt is selected from one or more of copper sulfate, copper nitrate, copper acetate, copper chloride, copper isooctanoate and copper tartrate;
  • the reducing agent is selected from one or more of formaldehyde, acetaldehyde, hydrazine hydrate and sodium borohydride;
  • the second alcohol is sec-butanol.
  • the percentage of the rare earth oxide in the graphene copper matrix composite material modified by the rare earth oxide is 0.1 wt%-0.5wt%;
  • the rare earth oxide is selected from one or more of cerium oxide, lanthanum oxide, rhenium oxide, zirconium oxide and aluminum oxide.
  • step (1) the speed of ball milling in step (1) is 100-800 r/min, ball milling time is 1-36 h;
  • the mass ratio of balls to material is 5:1-20:1.
  • the rotational speed of the centrifugal separation in step (1) is 0-2000 r/min, 2000-6000 r/min, 6000-9000 r/min or >9000 r/min.
  • step (2) the stirring speed in step (2) is 200-800 r/min, and the time is 10-100 min;
  • the temperature of the reduction is 25-80° C., and the time is 10-100 min.
  • step (3) the speed of ball milling in step (3) is 100-800 r/min, ball milling time is 1-36 h;
  • the mass ratio of balls to materials during ball milling in step (3) is 10:1;
  • the pressure environment of the spark plasma sintering is 5-50 MPa, the temperature is 673-1073 K, and the time is 1-10 min;
  • it also includes washing and vacuum drying the mixed powder in step (3).
  • the rare earth modified graphene copper-based composite material prepared by the preparation method described in any one of the above.
  • the contact wire for high-speed rail with a speed of 400 km per hour.
  • the present invention provides a preparation method of rare earth modified graphene copper-based composite material, the specific steps include: separating graphite, organic amines and alcohols in different centrifugal intervals, and dispersing the obtained products in The dispersion liquid is obtained in alcohols, and then copper mirror reaction occurs with copper salt and reduced to prepare graphene copper-based composite materials, mixed with rare earth oxides and ball milled to obtain mixed powder, and finally spark plasma sintering is carried out to obtain rare earth modified graphene copper base composite material.
  • the amount of organic amines modified on the graphene surface can be regulated by changing the amount of organic amines added, and the type of organic amines on the surface of graphene can be regulated by changing the chain length of organic amines.
  • the graphene with specific size and layer number can be obtained by adjusting the interval of centrifugation.
  • the reduction reaction rate can be precisely regulated by changing the amount and type of organic amines on the graphene surface, such as increasing the number of organic amines on the graphene surface or increasing the chain of organic amines can effectively reduce the reduction reaction rate.
  • the plasma sintering mechanism, performance regulation method and mechanism of copper-based materials can be established and improved through the process research of plasma sintering to obtain rare earth modified graphene copper-based composite materials.
  • the present invention proposes to prepare a graphene-copper-based composite material by constructing a uniform and stable graphene-amine salt-copper ion system to solve the problem of poor interfacial bonding between graphene and copper; it proposes to use rare earth oxides to disperse
  • the design and preparation of reinforced copper-based composite materials can greatly improve its mechanical strength without significantly reducing its electrical conductivity. It meets the requirements for high-speed rail contact lines with a speed of 400km per hour.
  • the strength is not less than 800 MPa, the conductivity is not less than 110 IACS%, and the elongation
  • the rate is not less than 3.0%, all of which are superior to similar foreign products, and can occupy a clear advantage in the high-speed railway market.
  • the large-scale and stable preparation technology is a pilot line of copper contact wire for high-speed railways, with an annual production capacity of more than 1,000 tons. economic benefits.
  • Figure 1 is a scheme roadmap for the synthesis of rare earth modified graphene copper matrix composites.
  • step (3) the graphene copper-based composite material powder described in step (2) and 0.1 Wt% lanthanum oxide is mixed, and poured into the ball mill tank according to the ratio of ball:material mass ratio of about 10:1, set the speed at 400 r/min, ball mill 2 h, make it fully mixed evenly, and then wash the mixed product several times to remove excess impurities, and dry it in a vacuum oven at 60°C.
  • the dried composite powder was passed through the MPa and 973 Spark plasma sintering at K5 min, molded into a cake shape of ⁇ 20*10 to prepare rare earth-modified graphene-copper matrix composites.
  • step (2) Fully mix the graphene copper-based composite material powder described in step (2) with 0.5wt% cerium oxide, and pour it into the ball mill tank according to the ratio of ball:material mass ratio of about 10:1, and set the speed at 400 r/min, ball mill 2 h, make it fully mixed evenly, and then wash the mixed product several times to remove excess impurities, and dry it in a vacuum oven at 60°C.
  • the dried composite powder was passed through the MPa and 973 Spark plasma sintering at K5 min, molded into a cake shape of ⁇ 20*10 to prepare rare earth-modified graphene-copper matrix composites.
  • the rare earth modified graphene copper-based composite material obtained in the embodiment is prepared as a contact wire, and its performance is tested according to the corresponding national standards, and its inspection items, methods and performance requirements are shown in Table 1:
  • the contact angle between rare earth oxide and copper substrate is less than 60 degrees
  • the grain size is less than 1 micron
  • the material strength is not less than 800 MPa
  • conductivity not less than 110 IACS% the elongation rate is not less than 3.0%
  • the indicators are better than the level of similar foreign products. Its advantages can occupy a clear advantage in the high-speed railway market and have huge economic benefits.

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Abstract

Matériau composite à base de cuivre-graphène modifié par des terres rares, son procédé de préparation et son application. Les étapes spécifiques du procédé de préparation comprennent : après la réalisation d'un broyage à boulets sur du graphite, une amine organique et une substance alcoolique, la réalisation d'une séparation à différents intervalles de centrifugation ; la dispersion du produit obtenu dans une substance alcoolique pour obtenir un liquide de dispersion, puis la réalisation d'une réaction de miroir de cuivre avec un sel de cuivre, et la réalisation d'une réduction pour préparer un matériau composite à base de cuivre-graphène ; la réalisation d'un broyage à boulets mixte avec un oxyde de terres rares pour obtenir une poudre mélangée, et enfin la réalisation d'un frittage flash, pour obtenir un matériau composite à base de cuivre-graphène modifié par des terres rares. Le matériau composite à base de cuivre-graphène est préparé par construction d'un système d'ions graphène-sel d'amine-cuivre uniforme et stable, résolvant le problème de mauvaise liaison d'interface entre le graphène et le cuivre ; grâce à la conception et à la préparation d'un matériau composite à base de cuivre renforcé par dispersion d'oxyde de terres rares, la résistance mécanique d'un matériau composite à base de cuivre peut être considérablement améliorée tandis que la conductivité électrique n'est pas évidemment réduite.
PCT/CN2022/137820 2021-12-15 2022-12-09 Matériau composite à base de cuivre-graphène modifié par des terres rares, son procédé de préparation et son application WO2023109667A1 (fr)

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CN202111538654.6A CN114480899B (zh) 2021-12-15 2021-12-15 一种稀土改性石墨烯铜基复合材料及其制备方法和应用

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CN116079014B (zh) * 2023-02-13 2023-07-04 常州罗尼斯特种导体有限责任公司 一种高强高导银铜合金线材及其制备方法
CN116043054B (zh) * 2023-03-22 2023-06-16 厦门凯纳石墨烯技术股份有限公司 一种改性石墨烯复合金属材料及其制备方法

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CN110695372A (zh) * 2019-10-10 2020-01-17 天津大学 一种稀土元素改善铜—石墨烯界面的制备方法
CN114480899A (zh) * 2021-12-15 2022-05-13 深圳先进技术研究院 一种稀土改性石墨烯铜基复合材料及其制备方法和应用

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