CN105855745A - Copper-based solder and preparation method and application method thereof - Google Patents

Copper-based solder and preparation method and application method thereof Download PDF

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Publication number
CN105855745A
CN105855745A CN201610303962.3A CN201610303962A CN105855745A CN 105855745 A CN105855745 A CN 105855745A CN 201610303962 A CN201610303962 A CN 201610303962A CN 105855745 A CN105855745 A CN 105855745A
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China
Prior art keywords
powder
copper
tih
based solder
solder
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CN201610303962.3A
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Chinese (zh)
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CN105855745B (en
Inventor
毛样武
彭良荥
王升高
马志斌
余思
陈喆
邓泉荣
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Wuhan Institute of Technology
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Wuhan Institute of Technology
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Publication of CN105855745B publication Critical patent/CN105855745B/en
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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/24Selection of soldering or welding materials proper
    • B23K35/30Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
    • B23K35/302Cu as the principal constituent
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/36Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
    • B23K35/3601Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest with inorganic compounds as principal constituents
    • B23K35/3608Titania or titanates
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K2103/00Materials to be soldered, welded or cut
    • B23K2103/18Dissimilar materials
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K2103/00Materials to be soldered, welded or cut
    • B23K2103/50Inorganic material, e.g. metals, not provided for in B23K2103/02 – B23K2103/26

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention relates to copper-based solder capable of being used for preparing tungsten/copper and graphite/copper connectors. The copper-based solder is powder obtained after micro-grade Cu powder and micro-grade TiH2 powder are mixed, wherein the mass percent of the TiH2 powder is 20-25%, and the mass percent of the Cu powder is 75-80%. A preparation method of the copper-based solder comprises the steps that the micro-grade Cu powder and the micro-grade TiH2 powder are selected; the Cu powder and the TiH2 powder are mixed in proportion and then put into a mortar, then ethyl alcohol is poured into the mortar, and the mixture is ground till the ethyl alcohol is completely volatilized; and the powdery solder is obtained. The copper-based solder has the main advantages that (1) the preparation process is simple; (2) the connection intensity of connectors is high; and (3) the process cost is low.

Description

A kind of copper-based solder and its preparation method and application method
Technical field
The invention belongs to field of dissimilar material connection, relate to tungsten/copper and the connection of graphite/copper, specifically, refer to that one can be used Prepare tungsten/copper and the copper-based solder of graphite/copper sleeve.
Background technology
Tungsten and alloy material thereof owing to having the advantages such as high fusing point, low vapour pressure and low sputtering etching rate it is considered to be Promising facing plasma material (Plasma Facing Materials, PFMs), as PFMs, it not only to have with The compatibility that plasma is good, the bombardment of high energy particle to be amenable to.In order to the heat being deposited on its surface is conducted, PFMs needs to be connected with the heat sink material copper of high heat conduction, and therefore the preparation of tungsten/copper sleeve has important grinding in nuclear fusion device Study carefully meaning.In the most conventional method of attachment, soldering is considered as a kind of convenient and effective method, but tungsten and the physics of copper Performance especially thermal coefficient of expansion difference is big especially, causes joint easily to produce high thermal stress, institute during preparation and military service It is the key preparing tungsten/copper sleeve to select suitable solder.
Graphite has that light weight, high specific strength, heat-resisting, corrosion-resistant, electrical and thermal conductivity performance be good and the spy such as good in thermal shock Property, have a wide range of applications in the industry.Need to be connected graphite with copper in prepared by novel automobile carbon commutator, change to improve To the wearability of device, thus extending its service life, therefore the preparation of graphite/copper sleeve has important research at automotive field Meaning.Connecting graphite/copper effect the best way at present is also method for brazing, but when using method for brazing to connect graphite/copper, there is copper Problem in graphite surface wetability difference.For this problem, the method for active solder is currently mainly used to solve.
For tungsten/copper and the connection of graphite/copper, conventional solder mainly has Ag-Cu-Ti, Ni parent metal and amorphous state Ti-Zr-Cu-Ni Solder etc..Owing to Ag can be transformed into the higher volatile pollution causing plasma of vapour pressure of Cd, Cd after neutron irradiation, Therefore, Ag-Cu-Ti solder cannot be applied in nuclear fusion device.Ni parent metal is high temperature alloy solder, and being easily generated higher thermal should Power causes tungsten/copper and the fracture of graphite/copper sleeve.The preparation technology of amorphous state Ti-Zr-Cu-Ni solder is complex, and cost is the most relatively High.
Summary of the invention
The present invention is directed to deficiency present in existing solder, it is provided that a kind of for connecting tungsten/copper and the copper-based solder of graphite/copper, described Copper-based solder can be used to prepare tungsten/copper and graphite/copper sleeve.
The present invention solves the problems referred to above and be the technical scheme is that a kind of copper-based solder, and it is micron-sized Cu powder and TiH2 Powder powder after mixing, wherein TiH2Mass percent shared by powder is 20%~25%, and mass percent shared by Cu powder is 75 %~80%.
By such scheme, described micron-sized Cu powder and TiH2The particle diameter of powder is 50 μm.
The preparation method of described copper-based solder, choosing particle diameter is micron-sized Cu powder and TiH2Powder;By Cu powder and TiH2Powder Put in mortar after mixing in proportion;It is subsequently poured into alcohol, and grinds, until alcohol volatilizees completely, obtain powder solder.
By such scheme, described micron-sized Cu powder and TiH2The particle diameter of powder is 50 μm.
By such scheme, wherein TiH2Mass percent shared by powder is 20%~25%, and mass percent shared by Cu powder is 75%~80 %.
The application process of described copper-based solder, it is characterised in that: for tungsten/copper and the preparation of graphite/copper sleeve, use condition is: Being incubated 10~20min at 870~930 DEG C, applying pressure is 9~10kPa.
The articulamentum even compact obtained after said method connects, joint interface is well combined.
The general principle of the present invention: the copper-based solder of the present invention in connection procedure, TiH2First decompose and generate Ti, during soldering, Cu-Ti alloy forms liquid.For tungsten/copper sleeve, articulamentum is mainly by Cu based solid solution and Ti-Cu intermetallic compound Deng composition;For graphite/copper sleeve, Ti and graphite generation interfacial reaction, form relatively thin TiC conversion zone, articulamentum master To be made up of Cu based solid solution and Ti-Cu intermetallic compound etc..
Present invention have the main advantage that
(1) copper-based solder of the present invention is mainly made up of powder body material, with low cost, and preparation technology is simple;
(2) copper-based solder of the present invention is used for preparing tungsten/copper and graphite/copper sleeve, and joint bonding strength is higher, wherein tungsten/copper sleeve Shear strength up to more than 95MPa;The shear strength of graphite/copper sleeve is 16.9~20.2MPa, is equivalent to graphite mother metal strong The 78%~93.3% of degree;
(3) copper-based solder of the present invention is in use, and with cladding process, therefore process costs is relatively low.
Accompanying drawing explanation
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of copper-based solder;
Fig. 2 is that embodiment 1 uses Cu-TiH2Microscopic appearance and the energy spectrum analysis collection of illustrative plates of tungsten/copper sleeve interface zone prepared by solder;
Fig. 3 is that embodiment 1 uses Cu-TiH2The XRD spectrum of tungsten/copper sleeve interface zone prepared by solder;
Fig. 4 is that embodiment 2 uses Cu-TiH2The microscopic appearance of graphite/copper sleeve interface zone prepared by solder.
Detailed description of the invention
Below by embodiment, the present invention is further illustrated, and the copper-based solder that embodiment is merely to illustrate the present invention is feasible, It is not used in the interest field limiting present invention protection.
The copper-based solder that embodiment 1 applies the present invention to provide prepares tungsten/copper sleeve
The solder that the present invention provides is as follows for the processing step preparing tungsten/copper sleeve:
(A) preparation of solder,
Choose particle diameter and be about Cu powder and the TiH of 50 μm2Powder;By Cu powder and TiH2Powder is mixed to get mixed-powder, wherein TiH2 The mass percent of powder is 22%;Mixed-powder is placed in mortar, adds alcohol hand lapping, until alcohol volatilizees completely, Obtain powder solder.
(B) mother metal surface preparation,
The end face abrasive paper for metallograph to be connected of tungsten with copper is polished step by step, then puts cleaning 20min in supersonic wave cleaning machine into, then Dry up standby with hair-dryer;
(C) Joining Technology,
Take the solder that a small amount of above-mentioned steps (A) is prepared, add glycerine solvent and reconcile into thickness paste, then cream solder is coated with Overlay on the connecting end surface after step (B) processes;Then two connecting end surfaces are closed and be placed in graphite jig, then put Enter in vacuum drying oven, apply the pressure of 10kPa;Open heating schedule, and be incubated 15min at 880 DEG C, then cool down with stove To room temperature, take out sample, obtain tungsten/copper jointing.
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of copper-based solder, it is recognised that solder is by Cu powder and TiH from figure2Powder Composition.
Fig. 2 is for using Cu-TiH2SEM (SEM) the microcosmic picture at tungsten/copper sleeve interface prepared by solder, by SEM Figure is it can be seen that the left side is articulamentum, and the right is tungsten, and between articulamentum and tungsten, interface cohesion is good, do not have obvious hole and Defect;Articulamentum Oxford gray region and black region are mainly Ti-Cu intermetallic compound, and light gray areas is mainly Cu base Solid solution.
Fig. 3 is for using Cu-TiH2Solder prepares the XRD spectrum of tungsten/copper sleeve interface zone, as seen from the figure, articulamentum Main by copper-based solid solution and Ti-Cu intermetallic compound (TiCu4、Ti2Cu and Ti3Cu etc.) composition.
The copper-based solder that embodiment 2 applies the present invention to provide prepares graphite/copper sleeve
The copper-based solder that the present invention provides is as follows for the processing step preparing graphite/copper sleeve:
(A) preparation of solder,
Choose particle diameter and be about Cu powder and the TiH of 50 μm2Powder;By Cu powder and TiH2Powder is mixed to get mixed-powder, wherein TiH2 The mass percent of powder is 23%;Mixed-powder is placed in mortar, adds alcohol hand lapping, until alcohol volatilizees completely, Obtain powder solder.
(B) mother metal surface preparation,
The end face abrasive paper for metallograph to be connected of graphite with copper is polished step by step, then puts cleaning 30min in supersonic wave cleaning machine into, so Dry up standby afterwards with hair-dryer;
(C) Joining Technology,
Take the solder that a small amount of above-mentioned steps (A) is prepared, add glycerine solvent and reconcile into thickness paste, then cream solder is coated with Overlay on the connecting end surface after step (B) processes;Then two connecting end surfaces are closed and be placed in graphite jig, then put Enter in vacuum drying oven, apply the pressure of 9.6kPa;Open heating schedule, and be incubated 10min at 900 DEG C, then cool down with stove To room temperature, take out sample, obtain graphite/copper jointing.
Fig. 4 is for using Cu-TiH2The SEM microcosmic picture of graphite/copper sleeve interface zone prepared by solder.As can be seen from Figure, Upper black area is graphite, and lower section light gray areas is copper, and middle greyish black alternate part is articulamentum, and its thickness is about 100 μm.Having relatively thin TiC conversion zone between graphite and articulamentum, between articulamentum and graphite, interface cohesion is good, flawless, The defects such as hole, and have solder to penetrate in the perforate gap of graphite mother metal.

Claims (6)

1. a copper-based solder, it is micron-sized Cu powder and TiH2Powder powder after mixing, wherein TiH2Quality hundred shared by powder Proportion by subtraction is 20%~25%, and mass percent shared by Cu powder is 75%~80%.
2. the copper-based solder described in claim 1, it is characterised in that described micron-sized Cu powder and TiH2The particle diameter of powder is 50 μm.
3. the preparation method of the copper-based solder described in claim 1, choosing particle diameter is micron-sized Cu powder and TiH2Powder;By Cu powder And TiH2Powder mixes in proportion to be put in mortar afterwards;It is subsequently poured into alcohol, and grinds, until alcohol volatilizees completely, To powder solder.
The preparation method of copper-based solder the most according to claim 3, it is characterised in that: described micron-sized Cu powder and TiH2 The particle diameter of powder is 50 μm.
The preparation method of copper-based solder the most according to claim 3, it is characterised in that: wherein TiH2Mass percent shared by powder Being 20%~25%, mass percent shared by Cu powder is 75%~80%.
6. the application process of the copper-based solder described in claim 1, it is characterised in that: for tungsten/copper and the preparation of graphite/copper sleeve, Use condition is: be incubated 10~20min at 870~930 DEG C, and applying pressure is 9~10kPa.
CN201610303962.3A 2016-05-10 2016-05-10 A kind of copper-based solder and its preparation method and application method Expired - Fee Related CN105855745B (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106583967A (en) * 2017-01-16 2017-04-26 武汉工程大学 TiH2-Ni-Cu-TiC composite welding flux as well as preparing method and application thereof
CN107378163A (en) * 2017-08-14 2017-11-24 武汉工程大学 A kind of graphite/Cu alloy-junctions and preparation method thereof
CN107916347A (en) * 2017-11-15 2018-04-17 广西塔锡科技有限公司 A kind of alloy welding powder and preparation method thereof
CN108746910A (en) * 2018-06-15 2018-11-06 武汉工程大学 A kind of tungsten/copper sleeve and preparation method thereof of copper base solder addition copper foil
CN113084176A (en) * 2021-04-09 2021-07-09 武汉工程大学 Self-supporting diamond film/Cu composite heat sink material and preparation method thereof
JP7192165B1 (en) * 2021-07-06 2022-12-19 株式会社アライドマテリアル Composite material
WO2023281862A1 (en) * 2021-07-06 2023-01-12 株式会社アライドマテリアル Composite material
CN116921914A (en) * 2023-08-24 2023-10-24 广州汉源微电子封装材料有限公司 Composite metal composition and preparation method and application thereof

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CN104708161A (en) * 2015-02-12 2015-06-17 武汉工程大学 Welding method for graphite/copper connector and composite solder of graphite/copper connector
CN105014257A (en) * 2014-04-29 2015-11-04 中国科学院上海硅酸盐研究所 Brazing filler metal for SiC base composite material connection
CN105171270A (en) * 2015-10-30 2015-12-23 江苏科技大学 Brazing filler metal for brazing dissimilar component W-Cu alloy, preparation method and brazing method

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JPH0292872A (en) * 1988-09-28 1990-04-03 Kyocera Corp Bonding between ceramic material and copper material
US6187071B1 (en) * 1999-01-14 2001-02-13 Norton Company Bond for abrasive tool
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Cited By (10)

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Publication number Priority date Publication date Assignee Title
CN106583967A (en) * 2017-01-16 2017-04-26 武汉工程大学 TiH2-Ni-Cu-TiC composite welding flux as well as preparing method and application thereof
CN106583967B (en) * 2017-01-16 2018-12-14 武汉工程大学 A kind of TiH2- Ni-Cu+TiC composite solder and its preparation method and application
CN107378163A (en) * 2017-08-14 2017-11-24 武汉工程大学 A kind of graphite/Cu alloy-junctions and preparation method thereof
CN107916347A (en) * 2017-11-15 2018-04-17 广西塔锡科技有限公司 A kind of alloy welding powder and preparation method thereof
CN108746910A (en) * 2018-06-15 2018-11-06 武汉工程大学 A kind of tungsten/copper sleeve and preparation method thereof of copper base solder addition copper foil
CN113084176A (en) * 2021-04-09 2021-07-09 武汉工程大学 Self-supporting diamond film/Cu composite heat sink material and preparation method thereof
CN113084176B (en) * 2021-04-09 2023-08-18 武汉工程大学 Self-supporting diamond film/Cu composite heat sink material and preparation method thereof
JP7192165B1 (en) * 2021-07-06 2022-12-19 株式会社アライドマテリアル Composite material
WO2023281862A1 (en) * 2021-07-06 2023-01-12 株式会社アライドマテリアル Composite material
CN116921914A (en) * 2023-08-24 2023-10-24 广州汉源微电子封装材料有限公司 Composite metal composition and preparation method and application thereof

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