CN105855745B - A kind of copper-based solder and its preparation method and application method - Google Patents
A kind of copper-based solder and its preparation method and application method Download PDFInfo
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- CN105855745B CN105855745B CN201610303962.3A CN201610303962A CN105855745B CN 105855745 B CN105855745 B CN 105855745B CN 201610303962 A CN201610303962 A CN 201610303962A CN 105855745 B CN105855745 B CN 105855745B
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- Prior art keywords
- powder
- copper
- tih
- graphite
- solder
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/302—Cu as the principal constituent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/36—Selection 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
- B23K35/3601—Selection 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
- B23K35/3608—Titania or titanates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K2103/00—Materials to be soldered, welded or cut
- B23K2103/18—Dissimilar materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K2103/00—Materials to be soldered, welded or cut
- B23K2103/50—Inorganic 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 present invention relates to a kind of copper-based solders that can be used for preparing tungsten/copper and graphite/copper sleeve, are micron-sized Cu powder and TiH2The powder of powder after mixing, wherein TiH2Mass percent shared by powder is that mass percent shared by 20%~25%, Cu powder is 75%~80%, the preparation method of the copper-based solder, and it is micron-sized Cu powder and TiH to choose grain size2Powder;By Cu powder and TiH2Powder is put into after mixing in proportion in mortar;It is subsequently poured into alcohol, and is ground, until alcohol volatilizees completely, obtains powder solder.Main advantages of the present invention are:(1) preparation process is simple;(2) connector bonding strength is higher;(3) therefore process costs are relatively low.
Description
Technical field
The invention belongs to field of dissimilar material connection, are related to the connection of tungsten/copper and graphite/copper, specifically, referring to one kind
The copper-based solder of tungsten/copper and graphite/copper sleeve can be used for preparing.
Background technology
Tungsten and its alloy material are recognized due to having many advantages, such as high fusing point, low vapour pressure and low sputtering etching rate
To be most promising facing plasma material (Plasma Facing Materials, PFMs), as PFMs, it is not only
Will have with the good compatibility of plasma, to be also amenable to the bombardment of high energy particle.In order to which the heat on its surface will be deposited on
Amount conducts, and PFMs needs are connect with the heat sink material copper of high heat conduction, therefore the preparation of tungsten/copper sleeve is in nuclear fusion device
With important research significance.In currently used connection method, soldering is considered as a kind of convenience and effective method, still
The physical property of tungsten and copper especially coefficient of thermal expansion difference is especially big, and connector is caused to be easy tod produce during preparing and being on active service
High thermal stress, so it is the key that prepare tungsten/copper sleeve to select suitable solder.
Graphite has light, high specific strength, heat-resisting, corrosion-resistant, electrical and thermal conductivity performance well and good in thermal shock
Etc. characteristics, have a wide range of applications in the industry.It needs graphite connecting with copper in the preparation of novel automobile carbon commutator, to carry
The wearability of high commutator, to extend its service life, therefore the preparation of graphite/copper sleeve have in automotive field it is important
Research significance.Connection graphite/copper effect the best way is also method for brazing at present, but when use method for brazing connection graphite/copper,
There is a problem of copper in graphite surface wetability difference.For the problem, mainly solved at present using the method for active solder.
Connection for tungsten/copper and graphite/copper, common solder mainly have Ag-Cu-Ti, Ni parent metal and amorphous state Ti-
Zr-Cu-Ni solders etc..Since Ag can be transformed into Cd after neutron irradiation, the vapour pressure of Cd is higher volatile to lead to plasma
Pollution, therefore, Ag-Cu-Ti solders can not be applied in nuclear fusion device.Ni parent metals are high temperature alloy solders, are also easy to produce
Higher thermal stress leads to the fracture of tungsten/copper and graphite/copper sleeve.The preparation process of amorphous state Ti-Zr-Cu-Ni solders is more multiple
Miscellaneous, cost is also higher.
Invention content
The present invention provides a kind of copper-based weldering for connecting tungsten/copper and graphite/copper for deficiency present in existing solder
Material, the copper-based solder can be used for preparing tungsten/copper and graphite/copper sleeve.
Technical solution is used by the present invention solves the above problems:A kind of copper-based solder, be micron-sized Cu powder and
TiH2The powder of powder after mixing, wherein TiH2Mass percent shared by powder is that mass percent shared by 20%~25%, Cu powder is
75%~80%.
By said program, the micron-sized Cu powder and TiH2The grain size of powder is 50 μm.
The preparation method of the copper-based solder, it is micron-sized Cu powder and TiH to choose grain size2Powder;By Cu powder and TiH2Powder
It is put into mortar after mixing in proportion;It is subsequently poured into alcohol, and is ground, until alcohol volatilizees completely, obtains powder solder.
By said program, the micron-sized Cu powder and TiH2The grain size of powder is 50 μm.
By said program, wherein TiH2Mass percent shared by powder is that mass percent shared by 20%~25%, Cu powder is
75%~80%.
The application process of the copper-based solder, it is characterised in that:For the preparation of tungsten/copper and graphite/copper sleeve, use
Condition is:10~20min is kept the temperature at 870~930 DEG C, application pressure is 9~10kPa.
The articulamentum even compact obtained after the above method connects, joint interface are well combined.
The basic principle of the present invention:The present invention copper-based solder during the connection process, TiH2It decomposes first and generates Ti, soldering
When, Cu-Ti alloys form liquid.For tungsten/copper sleeve, articulamentum between Cu based solid solutions and Ti-Cu metals mainly by changing
Close the compositions such as object;For graphite/copper sleeve, with graphite interfacial reaction occurs for Ti, forms relatively thin TiC conversion zones, connects
Layer is mainly made of Cu based solid solutions and Ti-Cu intermetallic compounds etc..
Main advantages of the present invention are:
(1) copper-based solder of the invention is mainly made of powder body material, and of low cost, preparation process is simple;
(2) copper-based solder of the invention is used to prepare tungsten/copper and graphite/copper sleeve, and connector bonding strength is higher, wherein
The shear strength of tungsten/copper sleeve is up to 95MPa or more;The shear strength of graphite/copper sleeve is 16.9~20.2MPa, is equivalent to
The 78%~93.3% of graphite strength of parent;
(3) in use, with cladding process, therefore process costs are relatively low for copper-based solder of the invention.
Description of the drawings
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of copper-based solder;
Fig. 2 is that embodiment 1 uses Cu-TiH2Solder prepares microscopic appearance and the energy spectrum analysis of tungsten/copper sleeve interface zone
Collection of illustrative plates;
Fig. 3 is that embodiment 1 uses Cu-TiH2Solder prepares the XRD spectrum of tungsten/copper sleeve interface zone;
Fig. 4 is that embodiment 2 uses Cu-TiH2Solder prepares the microscopic appearance of graphite/copper sleeve interface zone.
Specific implementation mode
Below by embodiment, the present invention is further illustrated, and embodiment is merely to illustrate the copper-based solder of the present invention
It is feasible, it is not used in the interest field that the limitation present invention protects.
Embodiment 1 prepares tungsten/copper sleeve using copper-based solder provided by the invention
The processing step that solder provided by the invention is used to prepare tungsten/copper sleeve is as follows:
(A) preparation of solder,
Choose the Cu powder and TiH that grain size is about 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, alcohol and hand lapping is added, until alcohol is waved completely
Hair, obtains powder solder.
(B) base material surface preparation,
Tungsten and copper are waited for that connecting end surface is polished step by step with abrasive paper for metallograph, then puts into and cleans 20min in supersonic wave cleaning machine,
Then it is dried up with hair-dryer spare;
(C) Joining Technology,
Solder made from a small amount of above-mentioned steps (A) is taken, glycerine solvent is added and reconciles into sticky paste, then welds paste
Material is coated in through on step (B) treated connecting end surface;Then two connecting end surfaces are closed and is placed in graphite jig, connect
It and is put into vacuum drying oven, apply the pressure of 10kPa;Heating schedule is opened, and keeps the temperature 15min at 880 DEG C, is then cooled to the furnace
Room temperature takes out sample, obtains 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 group
At.
Fig. 2 is using Cu-TiH2Solder prepares scanning electron microscope (SEM) the microcosmic picture at tungsten/copper sleeve interface, by
SEM figures are as can be seen that the left side is articulamentum, and the right is tungsten, and interface cohesion is good between articulamentum and tungsten, without apparent hole
And defect;Articulamentum Oxford gray region and black region are mainly Ti-Cu intermetallic compounds, and light gray areas is mainly Cu
Based solid solution.
Fig. 3 is using Cu-TiH2Solder prepares the XRD spectrum of tungsten/copper sleeve interface zone, as seen from the figure, connection
Layer is mainly by copper-based solid solution and Ti-Cu intermetallic compounds (TiCu4、Ti2Cu and Ti3Cu etc.) composition.
Embodiment 2 prepares graphite/copper sleeve using copper-based solder provided by the invention
The processing step that copper-based solder provided by the invention is used to prepare graphite/copper sleeve is as follows:
(A) preparation of solder,
Choose the Cu powder and TiH that grain size is about 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, alcohol and hand lapping is added, until alcohol is waved completely
Hair, obtains powder solder.
(B) base material surface preparation,
Graphite and copper are waited for that connecting end surface is polished step by step with abrasive paper for metallograph, then puts into supersonic wave cleaning machine and cleans
Then 30min is dried up spare with hair-dryer;
(C) Joining Technology,
Solder made from a small amount of above-mentioned steps (A) is taken, glycerine solvent is added and reconciles into sticky paste, then welds paste
Material is coated in through on step (B) treated connecting end surface;Then two connecting end surfaces are closed and is placed in graphite jig, connect
It and is put into vacuum drying oven, apply the pressure of 9.6kPa;Heating schedule is opened, and keeps the temperature 10min, then furnace cooling at 900 DEG C
To room temperature, sample is taken out, graphite/copper jointing is obtained.
Fig. 4 is using Cu-TiH2Solder prepares the microcosmic pictures of SEM of graphite/copper sleeve interface zone.By that can be seen in figure
Go out, upper black area is graphite, and lower section light gray areas is copper, and intermediate greyish black alternate part is articulamentum, and thickness is about
It is 100 μm.There are relatively thin TiC conversion zones between graphite and articulamentum, interface cohesion is good between articulamentum and graphite, and nothing is split
The defects of line, hole, and there is solder to penetrate into the trepanning gap of graphite base material.
Claims (3)
- It is micron-sized Cu powder and TiH 1. a kind of copper-based solder is used for the preparation of tungsten/copper and graphite/copper sleeve2Powder is through mixed Powder after conjunction, wherein TiH2Mass percent shared by powder is that mass percent shared by 20 % ~ 25 %, Cu powder is the % of 75 % ~ 80, The micron-sized Cu powder and TiH2The grain size of powder is 50 μm.
- 2. the preparation method of copper-based solder described in claim 1, it is micron-sized Cu powder and TiH to choose grain size2Powder;By Cu powder And TiH2Powder is put into after mixing in proportion in mortar;It is subsequently poured into alcohol, and is ground, until alcohol volatilizees completely, obtains powder Body solder, the micron-sized Cu powder and TiH2The grain size of powder is 50 μm, wherein TiH2Mass percent shared by powder is 20 % Mass percent shared by ~ 25 %, Cu powder is the % of 75 % ~ 80.
- 3. the application process of copper-based solder described in claim 1, it is characterised in that:System for tungsten/copper and graphite/copper sleeve Standby, use condition is:10~20 min are kept the temperature at 870 ~ 930 DEG C, application pressure is 9~10 kPa.
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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 |
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 |
WO2023281862A1 (en) * | 2021-07-06 | 2023-01-12 | 株式会社アライドマテリアル | Composite material |
JP7192165B1 (en) * | 2021-07-06 | 2022-12-19 | 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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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 |
JP2005139057A (en) * | 2003-11-06 | 2005-06-02 | Taiyo Material:Kk | Method for metallizing powder sintered ceramics |
WO2011152553A1 (en) * | 2010-05-31 | 2011-12-08 | 東邦チタニウム株式会社 | Titanium alloy compound powder combined with copper powder, chrome powder or iron powder, titanium alloy material using said powder as raw material and production method thereof |
CN101987402B (en) * | 2010-11-30 | 2012-09-05 | 哈尔滨工业大学 | Method for brazing Ti2AlC ceramics and Cu with Cu-Sn-Ti solder |
CN103658904B (en) * | 2012-09-04 | 2016-01-20 | 核工业西南物理研究院 | A kind of tungsten copper composite block vacuum brazing Joining Technology |
CN103223537B (en) * | 2013-04-09 | 2015-03-11 | 武汉工程大学 | Method for connecting high-strength graphite with copper alloy |
CN105014257B (en) * | 2014-04-29 | 2017-08-11 | 中国科学院上海硅酸盐研究所 | A kind of solder connected for SiC based composites |
CN104708161B (en) * | 2015-02-12 | 2016-11-30 | 武汉工程大学 | A kind of composite solder |
CN105171270B (en) * | 2015-10-30 | 2017-04-05 | 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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