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WO2021189797A1 - Preparation method for high-thermal-conductivity and high-temperature-resistant composite copper alloy heat dissipation material - Google Patents

Preparation method for high-thermal-conductivity and high-temperature-resistant composite copper alloy heat dissipation material Download PDF

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Publication number
WO2021189797A1
WO2021189797A1 PCT/CN2020/118474 CN2020118474W WO2021189797A1 WO 2021189797 A1 WO2021189797 A1 WO 2021189797A1 CN 2020118474 W CN2020118474 W CN 2020118474W WO 2021189797 A1 WO2021189797 A1 WO 2021189797A1
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powder
heat dissipation
copper alloy
high temperature
dissipation material
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Chinese (zh)
Inventor
刘凯
王文斌
李刚
姚培建
王小军
张石松
李鹏
师晓云
贺德永
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Shaanxi Sirui Advanced Materials Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C24/00Coating starting from inorganic powder
    • C23C24/08Coating starting from inorganic powder by application of heat or pressure and heat
    • C23C24/10Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
    • C23C24/103Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
    • 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
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/16Metallic particles coated with a non-metal
    • 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
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/17Metallic particles coated with metal
    • 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
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/0068Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for particular articles not mentioned below
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C32/00Non-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
    • C22C32/0047Non-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 carbides, nitrides, borides or silicides as the main non-metallic constituents
    • C22C32/0052Non-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 carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C9/00Alloys based on copper
    • 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
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling

Definitions

  • the invention relates to the field of non-ferrous metal material manufacturing, in particular to a method for preparing a high thermal conductivity and high temperature resistant composite copper alloy heat dissipation material.
  • the present invention proposes a method for preparing high thermal conductivity and high temperature resistant composite copper alloys.
  • the heat dissipation material designed and manufactured by the present invention adopts a high temperature resistant copper alloy design at the contact part with the high temperature source.
  • the pure copper design has good heat dissipation while ensuring that it is not deformed at high temperatures.
  • heat-dissipating copper alloy materials that work in high-temperature working environments are mainly used to regularly replace copper alloy heat sinks, or to sacrifice part of the heat dissipation, using chromium-zirconium-copper, copper-chromium-niobium and other materials to maintain high-temperature strength characteristics.
  • the high temperature working environment of chromium zirconium copper is above 600 degrees, which cannot be used at higher temperatures.
  • the cost of copper chromium niobium remains high and cannot meet the cost requirements.
  • the present invention provides a method for preparing a high thermal conductivity and high temperature resistant composite copper alloy heat dissipation material.
  • a preparation method of high thermal conductivity and high temperature resistant composite copper alloy heat dissipation material mainly includes the following steps:
  • the raw materials selected to prepare high thermal conductivity and high temperature resistant composite heat dissipation copper materials mainly include: pure copper powder with a powder particle size of less than 50 ⁇ m and a sphericity greater than 80% and a second element used to improve the high temperature resistance of the composite copper alloy.
  • the two elements are any one of 4-11wt% WC, 4-10wt% TiC, 5-7wt% VC or 5-14wt% Cr 2 Nb.
  • the above second elements are all ceramic materials, and these second elements are selected They are all high-temperature resistant materials. After being added to copper, they will be wrapped in nano-crystal grains on the surface of copper powder.
  • these ceramic materials do not dissolve with Cu, which prevents the recrystallization of copper at high temperatures and improves copper alloys.
  • the softening temperature is good high temperature resistance.
  • the addition of a small amount of nanoparticles has little effect on the conductivity and heat dissipation of copper itself.
  • Powder mixing prefabrication Load the weighed pure copper powder and the second element into the atmosphere protection ball mill, and set the milling time to 3-8h;
  • the cladding thickness is set to be between 0.1 and 1mm.
  • the pure copper powder in S1 adopts the atomized copper powder after supersonic atomization of the copper material.
  • the atomized copper powder after supersonic atomization has more delicate powder and can exert its characteristics better, so that the prepared copper The alloy is of higher quality.
  • the particle size of the atomized copper powder is below 70 ⁇ m, and the atomized copper powder below 70 ⁇ m has high performance, strong sintering activity and a more developed surface.
  • the ball-to-material ratio is set between 1-5% to ensure that the nano-ceramic powder and the copper powder are fully mixed and uniform.
  • the outside of the radiator in S3 is made of pure copper, and 3-10mm surface cladding size requirements are reserved to ensure sufficient operating space.
  • the particle size of the second element WC, TiC, VC, and Cr 2 Nb powder is between 500nm-5 ⁇ m, which makes the mixing more uniform, the ratio is more accurate, and the material of the prefabricated composite copper alloy heat dissipation material can be improved. performance.
  • the present invention has the following beneficial effects:
  • the present invention uses atomized copper powder and the second element WC, TiC, VC, Cr 2 Nb in the selection of raw materials.
  • the second element is a high-temperature resistant ceramic material.
  • the crystal grains are wrapped on the surface of the copper powder. According to our research, these ceramic materials do not dissolve with Cu, which prevents the recrystallization of copper at high temperatures and increases the softening temperature of the copper alloy, which means that it has good high temperature resistance.
  • the addition of a small amount of nanoparticles has little effect on the conductivity and heat dissipation of copper itself.
  • the present invention is aimed at improving the use of high-strength and high-conductivity copper alloys in high-temperature working environments.
  • the high-thermal-conductivity and high-temperature-resistant composite heat-dissipating copper extracted by the present invention has high thermal conductivity and high-temperature-resistant copper alloys that have a high temperature below 900 degrees.
  • the feature of non-softening and deformation during work can ensure the structural strength under high temperature conditions.
  • the present invention has better heat dissipation.
  • the copper composite heat sink prepared by the above steps of the present invention has a conductivity of more than 80% IACS with a high-temperature contact surface, and a softening temperature of 700-900°C.
  • Figure 1 is a flow chart of the steps of the present invention
  • Fig. 2 is an X100-fold metallographic diagram of the CuWc 8 high temperature resistant copper alloy material prepared by the preparation method of Example 1.
  • a preparation method of high thermal conductivity and high temperature resistant composite copper alloy heat dissipation material mainly includes the following steps:
  • the raw materials selected to prepare high thermal conductivity and high temperature resistant composite heat dissipation copper materials mainly include: pure copper powder with a powder particle size of less than 50 ⁇ m and a sphericity greater than 80% and a mixture of 8wt% Wc as the second element for improving the high temperature resistance of the composite copper alloy ;
  • Powder mixing prefabrication Load the weighed pure copper powder and the second element WC into the atmosphere protection ball mill, and set the ball milling time to 5;
  • heat treatment of the prefabricated radiator the heat treatment process is: heat treatment temperature is 600 degrees, heat preservation for 3 hours, after heat treatment is completed, after finishing, high thermal conductivity and high temperature resistant composite copper alloy heat dissipation material can be obtained.
  • the pure copper powder in S1 adopts finer copper powder, and the copper material is atomized copper powder after supersonic atomization.
  • the particle size of the atomized copper powder is 55 ⁇ m.
  • the ball-to-material ratio is set to 3% to ensure that the nano-ceramic powder and the copper powder are fully mixed and uniform.
  • the outside of the radiator in S3 is made of pure copper, and 8mm surface cladding size requirements are reserved.
  • the particle size of the second element WC powder is 800 nm.
  • the second element added in this embodiment is Cr 2 Nb, the content of which is 12 wt%, and the powder particle size is 800 nm.
  • the high temperature resistant copper alloy material prepared by selecting the components selected in this embodiment is used to make the relevant performance parameter table 2.
  • the difference from the second embodiment is that the second element added in this embodiment is 6 wt% Cr 2 Nb.
  • the high temperature resistant copper alloy material prepared by selecting the selected components of this embodiment is used to make the relevant performance parameter table 3.
  • Table 3 Related performance parameters of the high temperature resistant copper alloy material prepared in this embodiment:
  • the difference from the third embodiment is that the second element added in this embodiment is 5 wt% Tic.
  • the high temperature resistant copper alloy material prepared by selecting the components selected in this embodiment is selected to make the relevant performance parameter Table 4.
  • Table 4 Related performance parameters of the high temperature resistant copper alloy material prepared in this embodiment:
  • the difference from the fourth embodiment is that the second element added in this embodiment is 6 wt% Vc.
  • the high temperature resistant copper alloy material prepared by selecting the components selected in this example is used to make the relevant performance parameter table 5.
  • Table 5 Related performance parameters of the high temperature resistant copper alloy material prepared in this embodiment:
  • Embodiment 6 is a diagrammatic representation of Embodiment 6
  • the second element added in this embodiment is Wc, the content of which is 4 wt%, and the powder particle size is 800 nm.
  • the high temperature resistant copper alloy material prepared by selecting the selected components in this embodiment is used to make the relevant performance parameter table 6.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Powder Metallurgy (AREA)

Abstract

A preparation method for a high-thermal-conductivity and high-temperature-resistant composite copper alloy heat dissipation material, mainly comprising the following steps: raw material selection, powder mixing and pre-making, surface cladding, and machining. The components of the material mainly comprise: a second element and atomized copper powder, wherein the second element is any one of 4-11 wt% of WC, 4-10 wt% of TiC, 5-7 wt% of VC and 5-14 wt% of Cr2Nb. The weighed pure copper powder and the weighed second element are put into an atmosphere-protected ball mill to be subjected to ball-milling, the mixed powder is put into a powder-feeding laser cladding device to be subjected to surface cladding, and then preparation is completed by means of finish machining. A high-thermal-conductivity and high-temperature-resistant copper alloy that is designed and developed has the characteristic of avoiding softening deformation during working at the high temperature of 900°C or below, also has good heat dissipation performance, and is suitable for wide promotion due to the excellent heat dissipation characteristic while ensuring the high-temperature structural strength.

Description

一种高导热耐高温复合铜合金散热材料制备方法Preparation method of high thermal conductivity and high temperature resistant composite copper alloy heat dissipation material

本申请要求申请日为2020/3/23的中国专利申请202010206850.2的优先权。本申请引用上述中国专利申请的全文。This application claims the priority of the Chinese patent application 202010206850.2 whose filing date is 2020/3/23. This application quotes the full text of the aforementioned Chinese patent application.

技术领域Technical field

本发明涉及有色金属材料制造领域,尤其涉及一种高导热耐高温复合铜合金散热材料制备方法。The invention relates to the field of non-ferrous metal material manufacturing, in particular to a method for preparing a high thermal conductivity and high temperature resistant composite copper alloy heat dissipation material.

背景技术Background technique

纯铜及铜合金由于极好的导电、导热、耐腐蚀性及韧性等特点,被应用于散热方面,如蒸气轮机、锅炉、飞机喷口等方面,但是铜合金具有较低的软化温度,长期在高温环境中工作,会造成软化变形,无法保证原有的设计结构,存在安全隐患。为提高高温散热铜合金目前存在的问题,本发明提出了一种高导热耐高温复合铜合金的制备方法,本发明设计制造的散热材料,与高温源接触部位采用耐高温铜合金设计,外部采用纯铜设计,在保证高温不变形的同时,具有良好的散热性。Pure copper and copper alloys are used in heat dissipation, such as steam turbines, boilers, aircraft nozzles, etc., due to their excellent electrical conductivity, thermal conductivity, corrosion resistance and toughness. However, copper alloys have a lower softening temperature and have been used for a long time Working in a high temperature environment will cause softening and deformation, the original design structure cannot be guaranteed, and there are potential safety hazards. In order to improve the current problems of high temperature heat dissipation copper alloys, the present invention proposes a method for preparing high thermal conductivity and high temperature resistant composite copper alloys. The heat dissipation material designed and manufactured by the present invention adopts a high temperature resistant copper alloy design at the contact part with the high temperature source. The pure copper design has good heat dissipation while ensuring that it is not deformed at high temperatures.

目前在高温工作环境中工作的散热铜合金材料,主要采用的办法是定期更换铜合金散热片,或是牺牲一部分散热性,采用铬锆铜、铜铬铌等材料来保持高温强度特性。但是铬锆铜的耐高温工作环境最高在600度以上,无法在更高温度下使用,铜铬铌成本居高不下,无法满足成本需求。At present, heat-dissipating copper alloy materials that work in high-temperature working environments are mainly used to regularly replace copper alloy heat sinks, or to sacrifice part of the heat dissipation, using chromium-zirconium-copper, copper-chromium-niobium and other materials to maintain high-temperature strength characteristics. However, the high temperature working environment of chromium zirconium copper is above 600 degrees, which cannot be used at higher temperatures. The cost of copper chromium niobium remains high and cannot meet the cost requirements.

发明内容Summary of the invention

为解决上述技术问题,本发明提供了一种高导热耐高温复合铜合金散热材料制备方法。In order to solve the above technical problems, the present invention provides a method for preparing a high thermal conductivity and high temperature resistant composite copper alloy heat dissipation material.

本发明的技术要点为:The technical points of the present invention are:

一种高导热耐高温复合铜合金散热材料制备方法,主要包括以下步骤:A preparation method of high thermal conductivity and high temperature resistant composite copper alloy heat dissipation material mainly includes the following steps:

S1、选择制备高导热耐高温复合散热铜材料的原材料主要包括:粉末粒度为50μm以下,球形度大于80%的纯铜粉和用于提高复合铜合金耐高温性的第二元素,所述第二元素为4-11wt%WC、4-10wt%TiC、5-7wt%的VC或5-14wt%Cr 2Nb其中的任意一种,以上第二元素均为陶瓷材料,选取的这些第二元素均为耐高温材料,添加到铜中后,会以纳米晶粒包裹在铜粉表面,经我们研究,这些陶瓷材料不与Cu相互溶,有阻止高温下铜的 再结晶长大,提高铜合金的软化温度,也就是耐高温性好。同时,少量的纳米颗粒添加,又对铜本身的导电、散热性影响小。 S1. The raw materials selected to prepare high thermal conductivity and high temperature resistant composite heat dissipation copper materials mainly include: pure copper powder with a powder particle size of less than 50 μm and a sphericity greater than 80% and a second element used to improve the high temperature resistance of the composite copper alloy. The two elements are any one of 4-11wt% WC, 4-10wt% TiC, 5-7wt% VC or 5-14wt% Cr 2 Nb. The above second elements are all ceramic materials, and these second elements are selected They are all high-temperature resistant materials. After being added to copper, they will be wrapped in nano-crystal grains on the surface of copper powder. According to our research, these ceramic materials do not dissolve with Cu, which prevents the recrystallization of copper at high temperatures and improves copper alloys. The softening temperature is good high temperature resistance. At the same time, the addition of a small amount of nanoparticles has little effect on the conductivity and heat dissipation of copper itself.

S2、粉末混合预制:将称量好的纯铜粉和第二元素装入气氛保护球磨机中,设置球磨时间为3-8h;S2. Powder mixing prefabrication: Load the weighed pure copper powder and the second element into the atmosphere protection ball mill, and set the milling time to 3-8h;

S3、表面熔覆:将所述S2中混好的混合粉装入送粉式激光熔覆设备中,预制一台散热器放置于基台上,然后将送粉式激光熔覆设备抽真空至1000Pa以下,根据通过UG所建立的3D建模图型,在散热器高温接触面进行熔覆工作,将激光功率设置在3-20KW之间,步进线速度设置为3m/min,步距设置为0.1-1mm,送粉量设置为1-500g/min,保护气量设置为5-100L/min,每层熔覆厚度设置为0.1-1mm之间,得到预制的复合铜合金散热材料,在溶覆过程中,厚度过大易造成层与层之间由于热应力分层,所以不能每层太厚。如果熔覆太薄,效率会变低,并且下层的基体会被熔化,故熔覆厚度设置为0.1-1mm之间最佳。S3. Surface cladding: Put the mixed powder mixed in S2 into the powder-feeding laser cladding equipment, prefabricate a radiator and place it on the base, and then evacuate the powder-feeding laser cladding equipment to Below 1000Pa, according to the 3D modeling pattern established by UG, the cladding work is performed on the high temperature contact surface of the radiator, the laser power is set between 3-20KW, the step linear speed is set to 3m/min, and the step distance is set 0.1-1mm, the powder feeding rate is set to 1-500g/min, the shielding gas rate is set to 5-100L/min, and the cladding thickness of each layer is set to be between 0.1-1mm. The prefabricated composite copper alloy heat dissipation material is obtained. During the coating process, too large thickness can easily cause layer-to-layer delamination due to thermal stress, so each layer should not be too thick. If the cladding is too thin, the efficiency will be low, and the underlying substrate will be melted, so the cladding thickness is set to be between 0.1 and 1mm.

S4、机械加工:将预制的复合铜合金散热材料进行热处理,热处理工艺为:热处理温度在400-800度,保温2-4小时,热处理完成后,经精加工,即可得到高导热耐高温复合铜合金散热材料,在激光熔覆时,由于冷却速度过度,材料组织中存在残余应力,容易变形,对材料进行热处理可有利去除内应力。S4. Mechanical processing: heat treatment of the prefabricated composite copper alloy heat dissipation material. The heat treatment process is: the heat treatment temperature is 400-800 degrees, and the heat preservation is 2-4 hours. After the heat treatment is completed, the high thermal conductivity and high temperature resistant composite can be obtained after finishing the heat treatment. Copper alloy heat dissipation material, during laser cladding, due to excessive cooling rate, residual stress exists in the material structure, which is easy to deform. Heat treatment of the material can help remove the internal stress.

进一步的,S1中的纯铜粉采用将铜材料超音速雾化后的雾化铜粉,超音速雾化后的雾化铜粉其粉末更加细腻,更能发挥其特性,使制备出的铜合金质量更高。Furthermore, the pure copper powder in S1 adopts the atomized copper powder after supersonic atomization of the copper material. The atomized copper powder after supersonic atomization has more delicate powder and can exert its characteristics better, so that the prepared copper The alloy is of higher quality.

更进一步的,所述雾化铜粉其粒度在70μm以下,70μm以下的雾化铜粉其具有高性能、烧结活性强和更发达的表面。Furthermore, the particle size of the atomized copper powder is below 70 μm, and the atomized copper powder below 70 μm has high performance, strong sintering activity and a more developed surface.

进一步的,S2中在进行粉末混合时设置球料比在1-5%之间,保证纳米陶瓷粉末与铜粉充分混合均匀。Furthermore, in S2, when the powder is mixed, the ball-to-material ratio is set between 1-5% to ensure that the nano-ceramic powder and the copper powder are fully mixed and uniform.

进一步的,S3中的散热器外部采用纯铜加工而成,并预留3-10mm表面熔覆尺寸要求,以保证足够的操作空间。Furthermore, the outside of the radiator in S3 is made of pure copper, and 3-10mm surface cladding size requirements are reserved to ensure sufficient operating space.

进一步的,所述第二元素WC、TiC、VC、Cr 2Nb粉末粒度为均在500nm-5μm之间,使混合更加均匀,配比更加精准,可提高预制出的复合铜合金散热材料的材料性能。 Further, the particle size of the second element WC, TiC, VC, and Cr 2 Nb powder is between 500nm-5μm, which makes the mixing more uniform, the ratio is more accurate, and the material of the prefabricated composite copper alloy heat dissipation material can be improved. performance.

与现有技术相比,本发明的有益效果在于:Compared with the prior art, the present invention has the following beneficial effects:

第一,本发明在原料的选取上采用雾化铜粉和第二元素WC、TiC、VC、Cr 2Nb,其中第二元素均为耐高温的陶瓷材料,添加到铜中后,会以纳米晶粒包裹在铜粉表面,经我们研究,这些陶瓷材料不与Cu相互溶,有阻止高温下铜的再结晶长大,提高铜合金的软化温度,也就是耐高温性好。同时,少量的纳米颗粒添加,又对铜本身的导电、散热性 影响小。 First, the present invention uses atomized copper powder and the second element WC, TiC, VC, Cr 2 Nb in the selection of raw materials. The second element is a high-temperature resistant ceramic material. The crystal grains are wrapped on the surface of the copper powder. According to our research, these ceramic materials do not dissolve with Cu, which prevents the recrystallization of copper at high temperatures and increases the softening temperature of the copper alloy, which means that it has good high temperature resistance. At the same time, the addition of a small amount of nanoparticles has little effect on the conductivity and heat dissipation of copper itself.

第二,本发明针对在高温工作环境下对高强高导铜合金的使用需求进行改进,本发明提炼出的高导热耐高温复合散热铜具备的高导热、耐高温铜合金具有在900度以下高温工作不软化变形的特点,可以保证高温条件下的结构强度。Second, the present invention is aimed at improving the use of high-strength and high-conductivity copper alloys in high-temperature working environments. The high-thermal-conductivity and high-temperature-resistant composite heat-dissipating copper extracted by the present invention has high thermal conductivity and high-temperature-resistant copper alloys that have a high temperature below 900 degrees. The feature of non-softening and deformation during work can ensure the structural strength under high temperature conditions.

第三,通过在散热器高温接触面进行熔覆工作,且散热器外部采用纯铜加工而成,并预留3-10mm表面熔覆尺寸要求,相比于现有技术而言,本发明的更具备更优的散热性。Third, by performing cladding work on the high-temperature contact surface of the radiator, and the outside of the radiator is made of pure copper, and 3-10mm surface cladding size requirements are reserved. Compared with the prior art, the present invention It has better heat dissipation.

第四、本发明以上步骤制备的铜复合散热件,与高温接触面导电率达到80%IACS以上,软化温度可达到700-900℃。Fourth, the copper composite heat sink prepared by the above steps of the present invention has a conductivity of more than 80% IACS with a high-temperature contact surface, and a softening temperature of 700-900°C.

附图说明Description of the drawings

图1是本发明的步骤流程图;Figure 1 is a flow chart of the steps of the present invention;

图2是实施例一的制备方法制备出的CuWc 8耐高温铜合金材料X100倍金相图。 Fig. 2 is an X100-fold metallographic diagram of the CuWc 8 high temperature resistant copper alloy material prepared by the preparation method of Example 1.

具体实施方式Detailed ways

实施例一:Example one:

一种高导热耐高温复合铜合金散热材料制备方法,主要包括以下步骤:A preparation method of high thermal conductivity and high temperature resistant composite copper alloy heat dissipation material mainly includes the following steps:

S1、选择制备高导热耐高温复合散热铜材料的原材料主要包括:粉末粒度为50μm以下,球形度大于80%的纯铜粉和用于提高复合铜合金耐高温性的第二元素8wt%Wc混合;S1. The raw materials selected to prepare high thermal conductivity and high temperature resistant composite heat dissipation copper materials mainly include: pure copper powder with a powder particle size of less than 50 μm and a sphericity greater than 80% and a mixture of 8wt% Wc as the second element for improving the high temperature resistance of the composite copper alloy ;

S2、粉末混合预制:将称量好的纯铜粉和第二元素WC装入气氛保护球磨机中,设置球磨时间为5;S2. Powder mixing prefabrication: Load the weighed pure copper powder and the second element WC into the atmosphere protection ball mill, and set the ball milling time to 5;

S3、表面熔覆:将所述S2中混好的混合粉装入送粉式激光熔覆设备中,预制一台散热器放置于基台上,然后将送粉式激光熔覆设备抽真空至800Pa,根据通过UG所建立的3D建模图型,在散热器高温接触面进行熔覆工作,将激光功率设置在12Kw,步进线速度设置为3m/min,步距设置为0.5mm,送粉量设置为200g/min,保护气量设置为45L/min,每层熔覆厚度设置为0.4mm,得到预制的复合铜合金散热材料。S3. Surface cladding: Put the mixed powder mixed in S2 into the powder-feeding laser cladding equipment, prefabricate a radiator and place it on the base, and then evacuate the powder-feeding laser cladding equipment to 800Pa, according to the 3D modeling pattern established by UG, the cladding work is performed on the high temperature contact surface of the radiator, the laser power is set to 12Kw, the step linear speed is set to 3m/min, the step distance is set to 0.5mm, The powder quantity is set to 200g/min, the shielding gas quantity is set to 45L/min, and the cladding thickness of each layer is set to 0.4mm to obtain a prefabricated composite copper alloy heat dissipation material.

S4、机械加工:将预制的散热器进行热处理,热处理工艺为:热处理温度在600度,保温3小时,热处理完成后,经精加工,即可得到高导热耐高温复合铜合金散热材料。S4. Mechanical processing: heat treatment of the prefabricated radiator, the heat treatment process is: heat treatment temperature is 600 degrees, heat preservation for 3 hours, after heat treatment is completed, after finishing, high thermal conductivity and high temperature resistant composite copper alloy heat dissipation material can be obtained.

S1中的纯铜粉采用更细的铜粉末,将铜材料超音速雾化后的雾化铜粉。The pure copper powder in S1 adopts finer copper powder, and the copper material is atomized copper powder after supersonic atomization.

所述雾化铜粉其粒度为55μm。The particle size of the atomized copper powder is 55 μm.

S2中在进行粉末混合时设置球料比为3%,保证纳米陶瓷粉末与铜粉充分混合均匀。In S2, when the powder is mixed, the ball-to-material ratio is set to 3% to ensure that the nano-ceramic powder and the copper powder are fully mixed and uniform.

S3中的散热器外部采用纯铜加工而成,并预留8mm表面熔覆尺寸要求。The outside of the radiator in S3 is made of pure copper, and 8mm surface cladding size requirements are reserved.

所述第二元素WC粉末粒度为800nm。The particle size of the second element WC powder is 800 nm.

选取制备出的耐高温铜合金材料作出相关性能参数表1。Select the prepared high temperature resistant copper alloy materials to make the relevant performance parameters Table 1.

表1:本实施例所制备出的复合铜合金散热材料相关性能参数Table 1: Related performance parameters of the composite copper alloy heat dissipation material prepared in this embodiment

Figure PCTCN2020118474-appb-000001
Figure PCTCN2020118474-appb-000001

实施例二:Embodiment two:

与所述实施例一不同之处在于本此实施例中加入的第二元素为Cr 2Nb,其含量为12wt%,粉末粒度为800nm。 The difference from the first embodiment is that the second element added in this embodiment is Cr 2 Nb, the content of which is 12 wt%, and the powder particle size is 800 nm.

选取本实施例所选成分制备出的耐高温铜合金材料作出相关性能参数表2。The high temperature resistant copper alloy material prepared by selecting the components selected in this embodiment is used to make the relevant performance parameter table 2.

表2:本实施例所制备出的复合铜合金散热材料相关性能参数:Table 2: Related performance parameters of the composite copper alloy heat dissipation material prepared in this embodiment:

Figure PCTCN2020118474-appb-000002
Figure PCTCN2020118474-appb-000002

实施例三:Example three:

与所述实施例二不同之处在于本此实施例中加入的第二元素为为6wt%Cr 2Nb。 The difference from the second embodiment is that the second element added in this embodiment is 6 wt% Cr 2 Nb.

选取本实施例所选成分制备出的耐高温铜合金材料作出相关性能参数表3。The high temperature resistant copper alloy material prepared by selecting the selected components of this embodiment is used to make the relevant performance parameter table 3.

表3:本实施例所制备出的耐高温铜合金材料相关性能参数:Table 3: Related performance parameters of the high temperature resistant copper alloy material prepared in this embodiment:

Figure PCTCN2020118474-appb-000003
Figure PCTCN2020118474-appb-000003

实施例四:Embodiment four:

与所述实施例三不同之处在于本此实施例中加入的第二元素为为5wt%Tic。The difference from the third embodiment is that the second element added in this embodiment is 5 wt% Tic.

选取本实施例所选成分制备出的耐高温铜合金材料作出相关性能参数表4。The high temperature resistant copper alloy material prepared by selecting the components selected in this embodiment is selected to make the relevant performance parameter Table 4.

表4:本实施例所制备出的耐高温铜合金材料相关性能参数:Table 4: Related performance parameters of the high temperature resistant copper alloy material prepared in this embodiment:

Figure PCTCN2020118474-appb-000004
Figure PCTCN2020118474-appb-000004

实施例五:Embodiment five:

与所述实施例四不同之处在于本此实施例中加入的第二元素为为6wt%Vc。The difference from the fourth embodiment is that the second element added in this embodiment is 6 wt% Vc.

选取本实施例所选成分制备出的耐高温铜合金材料作出相关性能参数表5。The high temperature resistant copper alloy material prepared by selecting the components selected in this example is used to make the relevant performance parameter table 5.

表5:本实施例所制备出的耐高温铜合金材料相关性能参数:Table 5: Related performance parameters of the high temperature resistant copper alloy material prepared in this embodiment:

Figure PCTCN2020118474-appb-000005
Figure PCTCN2020118474-appb-000005

实施例六:Embodiment 6:

与所述实施例五不同之处在于本此实施例中加入的第二元素为Wc,其含量为4wt%,粉末粒度为800nm。The difference from the fifth embodiment is that the second element added in this embodiment is Wc, the content of which is 4 wt%, and the powder particle size is 800 nm.

选取本实施例所选成分制备出的耐高温铜合金材料作出相关性能参数表6。The high temperature resistant copper alloy material prepared by selecting the selected components in this embodiment is used to make the relevant performance parameter table 6.

表6:本实施例所制备出的复合铜合金散热材料相关性能参数:Table 6: Related performance parameters of the composite copper alloy heat dissipation material prepared in this embodiment:

Figure PCTCN2020118474-appb-000006
Figure PCTCN2020118474-appb-000006

经过上述实施例和表1-6的数据显示,实施例二中所制备的复合铜合金散热材料CuCr 8Nb 4的综合材料性能能最优,CuWc 4其导电性能最优,CuWc 8的软化温度最高。 The data in the above examples and Tables 1-6 show that the composite copper alloy heat dissipation material CuCr 8 Nb 4 prepared in Example 2 has the best overall material performance, CuWc 4 has the best electrical conductivity, and CuWc 8 has the best softening temperature Highest.

虽然以上描述了本发明的具体实施方式,但是本领域的技术人员应当理解,这些仅是举例说明,在不背离本发明的原理和实质的前提下,可以对这些实施方式做出多种变更或修改。因此,本发明的保护范围由所附权利要求书限定。Although the specific embodiments of the present invention are described above, those skilled in the art should understand that these are only examples, and various changes or modifications can be made to these embodiments without departing from the principle and essence of the present invention. Revise. Therefore, the protection scope of the present invention is defined by the appended claims.

Claims (6)

一种高导热耐高温复合铜合金散热材料制备方法,其特征在于,主要包括以下步骤:A method for preparing high thermal conductivity and high temperature resistant composite copper alloy heat dissipation material is characterized in that it mainly includes the following steps: S1、选择制备高导热耐高温复合散热铜材料的原材料主要包括:粉末粒度为50μm以下,球形度大于80%的纯铜粉和用于提高复合铜合金耐高温性的第二元素,所述第二元素为4-11wt%WC、4-10wt%TiC、5-7wt%的VC或5-14wt%Cr 2Nb其中的任意一种; S1. The raw materials for selecting and preparing high thermal conductivity and high temperature resistant composite heat dissipation copper materials mainly include: pure copper powder with a powder particle size of less than 50 μm and a sphericity greater than 80% and a second element used to improve the high temperature resistance of the composite copper alloy. The two elements are any one of 4-11wt% WC, 4-10wt% TiC, 5-7wt% VC or 5-14wt% Cr 2 Nb; S2、粉末混合预制:将称量好的纯铜粉和第二元素装入气氛保护球磨机中,球磨时间为3-8h;S2. Powder mixing prefabrication: Load the weighed pure copper powder and the second element into the atmosphere protection ball mill, and the ball milling time is 3-8h; S3、表面熔覆:将所述S2中混好的混合粉装入送粉式激光熔覆设备中,预制一台散热器放置于基台上,然后将送粉式激光熔覆设备抽真空至1000Pa以下,根据通过UG所建立的3D建模图型,在散热器高温接触面进行熔覆工作,将激光功率设置在3-20KW之间,步进线速度设置为3m/min,步距设置为0.1-1mm,送粉量设置为1-500g/min,保护气量设置为5-100L/min,每层熔覆厚度设置为0.1-1mm之间,得到预制的复合铜合金散热材料。S3. Surface cladding: Put the mixed powder mixed in S2 into the powder-feeding laser cladding equipment, prefabricate a radiator and place it on the base, and then evacuate the powder-feeding laser cladding equipment to Below 1000Pa, according to the 3D modeling pattern established by UG, the cladding work is performed on the high temperature contact surface of the radiator, the laser power is set between 3-20KW, the step linear speed is set to 3m/min, and the step distance is set It is 0.1-1mm, the powder feeding rate is set to 1-500g/min, the shielding gas rate is set to 5-100L/min, and the cladding thickness of each layer is set to be between 0.1-1mm to obtain a prefabricated composite copper alloy heat dissipation material. S4、机械加工:将预制的复合铜合金散热材料进行热处理,热处理工艺为:热处理温度在400-800度,保温2-4小时,热处理完成后,经精加工,即可得到高导热耐高温复合铜合金散热材料。S4. Mechanical processing: heat treatment of the prefabricated composite copper alloy heat dissipation material. The heat treatment process is: the heat treatment temperature is 400-800 degrees, and the heat preservation is 2-4 hours. After the heat treatment is completed, the high thermal conductivity and high temperature resistant composite can be obtained after finishing the heat treatment. Copper alloy heat dissipation material. 如权利要求1所述的一种高导热耐高温复合铜合金散热材料制备方法,其特征在于,S1中的纯铜粉采用将铜材料超音速雾化后的雾化铜粉。The method for preparing a high thermal conductivity and high temperature resistant composite copper alloy heat dissipation material according to claim 1, wherein the pure copper powder in S1 adopts atomized copper powder after supersonic atomization of the copper material. 如权利要求1或2所述的一种高导热耐高温复合铜合金散热材料制备方法,其特征在于,所述雾化铜粉其粒度在70μm以下。The method for preparing a high thermal conductivity and high temperature resistant composite copper alloy heat dissipation material according to claim 1 or 2, characterized in that the particle size of the atomized copper powder is less than 70 μm. 如权利要求1-3中任一项所述的一种高导热耐高温复合铜合金散热材料制备方法,其特征在于,S2中在进行粉末混合时设置球料比在1-5%之间。The method for preparing a high thermal conductivity and high temperature resistant composite copper alloy heat dissipation material according to any one of claims 1 to 3, wherein the ball-to-material ratio is set between 1-5% during powder mixing in S2. 如权利要求1-4中任一项所述的一种高导热耐高温复合铜合金散热材料制备方法,其特征在于,S3中的散热器外部采用纯铜加工而成,并预留3-10mm表面熔覆尺寸要求。The method for preparing a high thermal conductivity and high temperature resistant composite copper alloy heat dissipation material according to any one of claims 1-4, wherein the outside of the heat sink in S3 is made of pure copper, and 3-10mm is reserved. Surface cladding size requirements. 如权利要求1-5中任一项所述的一种高导热耐高温复合铜合金散热材料制备方法,其特征在于,所述第二元素WC或TiC或VC或Cr 2Nb粉末粒度为均在500nm-5μm之间。 The method for preparing a high thermal conductivity and high temperature resistant composite copper alloy heat dissipation material according to any one of claims 1-5, wherein the second element WC or TiC or VC or Cr 2 Nb powder has a particle size of Between 500nm-5μm.
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