CN116552092A - Preparation method of superconducting thermal diamond-copper composite foil - Google Patents

Preparation method of superconducting thermal diamond-copper composite foil Download PDF

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Publication number
CN116552092A
CN116552092A CN202310521876.XA CN202310521876A CN116552092A CN 116552092 A CN116552092 A CN 116552092A CN 202310521876 A CN202310521876 A CN 202310521876A CN 116552092 A CN116552092 A CN 116552092A
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China
Prior art keywords
dia
composite foil
copper
foil
diamond
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Pending
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CN202310521876.XA
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Chinese (zh)
Inventor
胡万里
穆莹莹
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Shenzhen Dixing Jing Technology Co ltd
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Shenzhen Dixing Jing Technology Co ltd
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Priority to CN202310521876.XA priority Critical patent/CN116552092A/en
Publication of CN116552092A publication Critical patent/CN116552092A/en
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
    • H01L21/48Manufacture or treatment of parts, e.g. containers, prior to assembly of the devices, using processes not provided for in a single one of the subgroups H01L21/06 - H01L21/326
    • H01L21/4814Conductive parts
    • H01L21/4871Bases, plates or heatsinks
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21BROLLING OF METAL
    • B21B1/00Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
    • B21B1/40Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling foils which present special problems, e.g. because of thinness
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/06Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/10Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
    • B32B37/1018Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure using only vacuum
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00Ancillary operations in connection with laminating processes
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00Details of semiconductor or other solid state devices
    • H01L23/34Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
    • H01L23/36Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
    • H01L23/373Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
    • H01L23/3735Laminates or multilayers, e.g. direct bond copper ceramic substrates
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/14Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers
    • B32B37/24Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with at least one layer not being coherent before laminating, e.g. made up from granular material sprinkled onto a substrate
    • B32B2037/243Coating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00Properties of the layers or laminate
    • B32B2307/30Properties of the layers or laminate having particular thermal properties
    • B32B2307/302Conductive
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2553/00Packaging equipment or accessories not otherwise provided for
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E40/00Technologies for an efficient electrical power generation, transmission or distribution
    • Y02E40/60Superconducting electric elements or equipment; Power systems integrating superconducting elements or equipment

Abstract

The invention discloses a preparation method of a superconductive thermal diamond-copper composite foil, which comprises the following steps: s1, purifying copper; s2, hot-rolling the copper block to prepare copper foil; s3, selecting diamond particles with the particle size of 0.05-0.1 mm, and modifying the surfaces of the diamond particles; s4, uniformly coating the modified diamond particles on the surface of the copper foil, and then pressing the diamond particles on the surface of the copper foil through hot pressing treatment, so that the thickness of the integral Dia/Cu composite foil is 0.12mm-0.2mm; s5, placing the Dia/Cu composite foil in a vacuum environment for heating; s6, carrying out hot pressing treatment on the heated Dia/Cu composite foil in vacuum; s7, covering a copper foil with the thickness of 0.08-0.15 mm on the surface of the diamond powder layer of the Dia/Cu composite foil, and then placing the Cu/Dia/Cu composite foil in a vacuum environment for heating; s8, carrying out vacuum hot-pressing treatment on the heated Cu/Dia/Cu composite foil to enable the thickness of the Cu/Dia/Cu composite foil to be 0.15mm-0.2mm; the interface thermal resistance is high due to the fact that the interface of the Dia/Cu composite foil is not mutually wetted, and therefore the thermal conductivity of the Dia/Cu composite foil is improved.

Description

Preparation method of superconducting thermal diamond-copper composite foil
Technical Field
The invention relates to the technical field of heat conducting materials, in particular to a preparation method of a superconductive heat diamond-copper composite foil.
Background
With the increasing integration scale of electronic components and circuits, the heat generated by the circuit operation is correspondingly increased, and higher requirements are put on the thermal conductivity of packaging materials matched with the integrated circuit chips. In theory, the comprehensive performance of the diamond/copper composite material is very suitable for being used for an electronic packaging material, but in practice, the actual thermal conductivity of the diamond/copper composite material applied to production is lower, which is mainly caused by the immature processing technology of the diamond/copper composite material and the complex preparation process, and the main influencing factors are the intrinsic thermal conductivity of a copper matrix, the interfacial thermal conductivity, the intrinsic thermal conductivity of the diamond, the volume fraction and the particle size, and in general, the lower the nitrogen content in the diamond, the higher the thermal conductivity, the more complete the crystal form and the higher the thermal conductivity; in addition, the surface of the diamond is easily transformed into a graphite-like phase with poor heat conductivity due to the influence of high temperature, catalytic elements and the like, the intrinsic heat conductivity of the diamond is seriously influenced, and for the preparation of the composite material, mutual infiltration among components is a necessary preceding condition for compounding, is an important factor influencing an interface structure and an interface bonding state, and interface thermal resistance is very high due to the condition that the interface of the diamond and Cu is not mutually wetted, so that the heat conductivity of the composite material is influenced.
The existing preparation technology of the diamond/copper composite material mainly comprises a High-temperature High-pressure sintering (HTHP), a vacuum hot-pressing sintering (VHPS), a spark plasma sintering (Sparkplasma sintering, SPS), a melt Infiltration (Infiltration) and the like, and the density of the diamond/copper composite material prepared by the High-temperature High-pressure method is High, the formed diamond skeleton is favorable for heat conduction, but the HTHP has extremely High requirements on a die, and the prepared sample is small in size and High in cost, so that the diamond/copper composite material is difficult to be widely applied at present; the VHPS is limited by a die, the pressure is generally below 100MPa, the degree of interface bonding between copper and diamond is limited, and the requirements on the control of sintering parameters and the selection and addition of active elements are high. The preparation efficiency of the VHPS is also low, and the preparation of Dia/Cu with excellent thermal performance has certain difficulty; the spark plasma sintering is fast in temperature rise and reduction, the sintering temperature is relatively low, the efficiency is high, the sintering temperature of Dia/Cu is generally 800-970 ℃, the melting point of copper is not exceeded, the sintering die in the temperature range is generally a graphite die, the breaking strength of the graphite die is smaller than 100MPa, the sintering pressure is generally 50-80 MPa, the composite material is difficult to be fully dense in the sintering pressure range, the thermal resistance of gaps in the material can be increased, and the thermal conductivity of Dia/Cu is reduced; pressure impregnation is a complex process, the preparation of reinforcement prefabricated members, the smelting of a matrix, the flow of gas in the impregnation process and the solidification of the matrix have great influence on the performance of a sample, and the design of a graphite die, the control of sintering parameters and the selection of sintering equipment are high by adopting the method. Therefore, the preparation process of Dia/Cu needs to be further improved.
Disclosure of Invention
In view of the above, the present invention mainly provides a method for preparing a superconducting hot diamond-copper composite foil, which can avoid the interface thermal resistance high caused by the non-wetting condition of the interface of the Dia/Cu composite foil, thereby improving the thermal conductivity of the Dia/Cu composite foil.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a preparation method of a superconducting thermal diamond-copper composite foil comprises the following steps:
s1, purifying copper to ensure that the purity of copper blocks reaches more than 99.99 percent;
s2, hot-rolling the copper block into copper foil with the thickness of 0.08mm-0.15mm;
s3, selecting diamond particles with the particle size of 0.05-0.1 mm, and modifying the surfaces of the diamond particles;
s4, uniformly coating the modified diamond particles on the surface of the copper foil, and then pressing the diamond particles on the surface of the copper foil through hot pressing treatment to form a diamond powder layer on the surface of the copper foil, wherein the thickness of the whole thermally pressed Dia/Cu composite foil is 0.12-0.2 mm;
s5, placing the Dia/Cu composite foil prepared in the step S4 in a vacuum environment for heating, wherein the heating temperature is 1000-1050 ℃ and the heating time lasts for 8-10 minutes;
s6, carrying out hot pressing treatment on the heated Dia/Cu composite foil in vacuum to ensure that the thickness of the whole Dia/Cu composite foil is 0.1-0.18 mm;
s7, covering a copper foil with the thickness of 0.08-0.15 mm on the surface of the diamond powder layer of the Dia/Cu composite foil, and then placing the Cu/Dia/Cu composite foil in a vacuum environment for heating;
s8, carrying out hot pressing treatment on the heated Cu/Dia/Cu composite foil in vacuum, so that the thickness of the whole Cu/Dia/Cu composite foil is 0.15mm-0.2mm.
In the step S5, after the Dia/Cu composite foil is heated, a layer of modified diamond particles with the particle size of 0.02-0.05 mm is uniformly coated on the surface of the diamond particle layer of the Dia/Cu composite foil.
As a preferable scheme, in the step S5, the heating temperature is 1000-1050 ℃ for 8-10 minutes;
as a preferred scheme, the method further comprises the following steps:
s9, edge sealing treatment is carried out on the edge of the Cu/Dia/Cu composite foil.
Compared with the prior art, the method has obvious advantages and beneficial effects, and particularly, the technical scheme mainly comprises the steps of firstly carrying out modification treatment on diamond particles, and then pressing the diamond particles on the surface of the high-temperature copper foil through a process of vacuum hot pressing for a plurality of times, so that the Cu/Dia/Cu composite foil is manufactured, and the interface thermal resistance is high due to the condition that the interface of the Dia/Cu composite foil is mutually non-wetting, so that the thermal conductivity of the Dia/Cu composite foil is improved.
In order to more clearly illustrate the structural features and efficacy of the present invention, the present invention will be described in detail below with reference to the accompanying drawings and examples.
Drawings
FIG. 1 is a process flow diagram of an embodiment of the present invention;
FIG. 2 is a schematic diagram of the structure of a Dia/Cu composite foil after first hot pressing according to an embodiment of the present invention;
FIG. 3 is a schematic diagram of a second hot press of a Dia/Cu composite foil according to an embodiment of the invention;
FIG. 4 is a schematic diagram of the structure of a Cu/Dia/Cu composite foil after a third hot press according to an embodiment of the present invention.
Detailed Description
For the purpose of making the technical solution and advantages of the present invention more apparent, the present invention will be further described in detail below with reference to the accompanying drawings and examples of implementation. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
It will be understood that when an element is referred to as being "fixed to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The terms "vertical," "horizontal," "left," "right," and the like are used herein for illustrative purposes only.
Referring to fig. 1 to 4, the embodiment of the invention provides a method for preparing a superconducting hot diamond-copper composite foil, which is characterized in that: the method comprises the following steps:
s1, purifying copper to ensure that the purity of copper blocks reaches more than 99.99 percent;
s2, hot-rolling the copper block into copper foil with the thickness of 0.08-0.15 mm, melting and casting the copper block into an ingot at about 1200 ℃, and reducing the thickness of the copper alloy ingot by hot rolling, namely melting, ingot casting, hot rolling, cold rolling, annealing, cold rolling, degreasing and surface treatment.
S3, selecting diamond particles with the particle size of 0.05-0.1 mm, modifying the surfaces of the diamond particles, and because of the characteristics of low thermal expansion, difficult wetting with metal, welding and the like of the diamond film, the assembly and application processes of the diamond film and other devices and welding materials are greatly limited, so that the diamond surfaces are required to be modified, the surface metallization of the diamond particles means that uniform metal or metal carbide layers are formed on the surfaces of the diamond particles by adopting a physical method or a chemical method, so that the surfaces of the diamond particles have the performance of metal or metalloid, the diamond particles subjected to the surface metallization can be used for converting direct contact of a copper matrix with diamond into contact with the metal or metal carbide layers in the preparation process of the composite material, so that the tight bonding state of an interface is realized, the thermal conductivity of the composite material is improved, for example, the thermal conductivity of the diamond interface is improved by plating Mo, ti, W, cr and other active elements on the enhanced phase surface, and the thickness of the plated Cr layer is 0.2-8 mu m;
s4, uniformly coating the modified diamond particles on the surface of the copper foil, and then pressing the diamond particles on the surface of the copper foil through hot pressing treatment, wherein the temperature is 800-900 ℃ and the pressure is 80-120MPa during hot pressing; forming a diamond powder layer on the surface of the copper foil, wherein the thickness of the whole Dia/Cu composite foil after hot pressing is 0.12mm-0.2mm; in this step, it is easy to form a discontinuity of the diamond powder layer as shown in fig. 2, thereby affecting the thermal conductivity of the composite foil;
s5, placing the Dia/Cu composite foil manufactured in the step S4 in a vacuum environment for heating, wherein the heating temperature is 1000-1050 ℃, the duration is 8-10 minutes, the melting point of copper is 1083.4 ℃, and the heating temperature enables copper to reach a state to be melted, so that the copper foil is softened and convenient for carrying out next hot-pressing leaching;
s6, carrying out hot pressing treatment on the heated Dia/Cu composite foil in vacuum to ensure that the thickness of the whole Dia/Cu composite foil is 0.1-0.18 mm, the temperature is 800-900 ℃ and the pressure is 80-120MPa during hot pressing, carrying out hot pressing on the softened copper foil layer again to reduce the porosity of the Dia/Cu composite foil and reduce the interface thermal resistance, and carrying out vacuum hot pressing has the advantages of uniform temperature, slow cooling speed and capability of effectively reducing the thermal stress generated by the composite material in the hot pressing process, and the components of the composite material are easier to control.
S7, covering a copper foil with the thickness of 0.08-0.15 mm on the surface of the diamond powder layer of the Dia/Cu composite foil, and then placing the Cu/Dia/Cu composite foil in a vacuum environment for heating at the temperature of 1000-1050 ℃ for 8-10 minutes;
s8, carrying out hot pressing treatment on the heated Cu/Dia/Cu composite foil in vacuum to ensure that the thickness of the whole Cu/Dia/Cu composite foil is 0.15mm-0.2mm, and the temperature and the pressure during hot pressing are 800-900 ℃ and 80-120MPa, so as to form the Cu/Dia/Cu composite foil shown in figure 4;
s9, edge sealing treatment is carried out on the edge of the Cu/Dia/Cu foil.
In this embodiment, in step S5, after heating of the Dia/Cu composite foil, a layer of modified diamond particles with a particle size of 0.02mm-0.05mm is uniformly coated on the surface of the diamond particle layer of the Dia/Cu composite foil, and a diamond particle layer with a certain thickness is formed as shown in fig. 3.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the invention, but any modifications, equivalents, improvements, etc. within the principles of the present invention should be included in the scope of the present invention.

Claims (4)

1. A preparation method of a superconducting thermal diamond-copper composite foil is characterized by comprising the following steps: the method comprises the following steps:
s1, purifying copper to ensure that the purity of copper blocks reaches more than 99.99 percent;
s2, hot-rolling the copper block into copper foil with the thickness of 0.08mm-0.15mm;
s3, selecting diamond particles with the particle size of 0.05-0.1 mm, and modifying the surfaces of the diamond particles;
s4, uniformly coating the modified diamond particles on the surface of the copper foil, and then pressing the diamond particles on the surface of the copper foil through hot pressing treatment to form a diamond powder layer on the surface of the copper foil, wherein the thickness of the whole thermally pressed Dia/Cu composite foil is 0.12-0.2 mm;
s5, placing the Dia/Cu composite foil prepared in the step S4 in a vacuum environment for heating, wherein the heating temperature is 1000-1050 ℃ and the heating time lasts for 8-10 minutes;
s6, carrying out hot pressing treatment on the heated Dia/Cu composite foil in vacuum to ensure that the thickness of the whole Dia/Cu composite foil is 0.1-0.18 mm;
s7, covering a copper foil with the thickness of 0.08-0.15 mm on the surface of the diamond powder layer of the Dia/Cu composite foil, and then placing the Cu/Dia/Cu composite foil in a vacuum environment for heating;
s8, carrying out hot pressing treatment on the heated Cu/Dia/Cu composite foil in vacuum, so that the thickness of the whole Cu/Dia/Cu composite foil is 0.15mm-0.2mm.
2. The method for preparing the superconducting hot diamond-copper composite foil according to claim 1, wherein the method comprises the following steps: and S5, after the heating of the Dia/Cu composite foil is finished, uniformly coating a layer of modified diamond particles with the particle size of 0.02-0.05 mm on the surface of the diamond particle layer of the Dia/Cu composite foil.
3. The method for preparing the superconducting hot diamond-copper composite foil according to claim 1, wherein the method comprises the following steps: in the step S5, the heating temperature is 1000-1050 ℃ for 8-10 minutes.
4. The method for preparing the superconducting hot diamond-copper composite foil according to claim 1, wherein the method comprises the following steps: the method also comprises the following steps:
s9, edge sealing treatment is carried out on the edge of the Cu/Dia/Cu composite foil.
CN202310521876.XA 2023-05-10 2023-05-10 Preparation method of superconducting thermal diamond-copper composite foil Pending CN116552092A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202310521876.XA CN116552092A (en) 2023-05-10 2023-05-10 Preparation method of superconducting thermal diamond-copper composite foil

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202310521876.XA CN116552092A (en) 2023-05-10 2023-05-10 Preparation method of superconducting thermal diamond-copper composite foil

Publications (1)

Publication Number Publication Date
CN116552092A true CN116552092A (en) 2023-08-08

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Family Applications (1)

Application Number Title Priority Date Filing Date
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Country Status (1)

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