CN106334882B - A kind of AgCuTi solder and preparation method thereof - Google Patents
A kind of AgCuTi solder and preparation method thereof Download PDFInfo
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- CN106334882B CN106334882B CN201610955634.1A CN201610955634A CN106334882B CN 106334882 B CN106334882 B CN 106334882B CN 201610955634 A CN201610955634 A CN 201610955634A CN 106334882 B CN106334882 B CN 106334882B
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- 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
- B23K35/3006—Ag as the principal constituent
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- 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
- B23K35/40—Making wire or rods for soldering or welding
Abstract
A kind of AgCuTi solder is the transition zone of solid solution and the generation diffusion reaction formation of Titanium electroplated layer in AgCu matrix solder between matrix solder and Titanium electroplated layer including AgCu matrix solder and the Titanium electroplated layer being coated on outside AgCu matrix solder.The preparation method of AgCuTi foil solder provided by the invention, it is simple, convenient, the technical bottleneck that conventional method prepares solder is breached, provides a kind of new Method of Green Manufacture for the high-quality active solder of neomorph.For AgCuTi solder, improve the content of active element Ti in AgCuTi solder, it overcomes traditional AgCuTi solder and is difficult to the shortcomings that shaping and melt salt system Titanium Electroplating, this method has many advantages, such as easily to shape, is high in machining efficiency, at low cost, provides one kind new technological approaches for the manufacture production of AgCuTi solder.
Description
Technical field
The present invention relates to brazing materials, more particularly, to the preparation method of a kind of AgCuTi solder and the AgCuTi solder.
Background technique
AgCuTi solder is widely used in vacuum brazing field, but tradition AgCuTi solder is difficult as a kind of active solder
It is a great problem that puzzlement is brazed worker both at home and abroad with forming.
Titanium has many advantages, such as that specific strength height, corrosion resistance are strong as a kind of strategic light metal, is usually used in submarine, on aircraft,
Play a great role in navigation, aviation field, in metal surface electrodeposition of titanium can play the role of protection it is corrosion-resistant, can be applied to as
Ocean, corrosive environment of sea water are medium.
The discharge potential of Titanium is low, realizes that the deposition of titanium is more difficult, while the electroplating technology of titanium is immature also not perfect.Mesh
Preceding common method is as follows: first is that electric arc ionize electro-plating method, ionize in vacuum or inert gas using Titanium be titanium from
Then bombarding cathode implements plating to son；Second is that second-level titanizing method, first plates one layer of active metal (such as mainly on matrix
Magnesium), it is then cleaned with titanium tetrachloride solution, Titanium is displaced by magnesium and is then plated on matrix；Third is that fuse salt
Electro-plating method, using carbon oxygen titanium as anode, plating metal be cathode, fuse salt is that electrolyte implements plating.But electric arc ionization electricity
Electroplating method processing step is more, and energy consumption is high, and process is complicated, and operation difficulty is big；The electrode potential of magnesium is same in second-level titanizing method
Sample is lower, and plating is difficult to realize；Fuse salt electro-plating method includes that titanium is smelted and titanium two processes of plating, coating quality and stability
It is poor.
The preparation method of AgCuTi solder mainly has two kinds of electric arc melting, vacuum melting at present.In electric arc melting method by
It is small in arc light heated perimeter, the AgCuTi solder prepared every time less than 1000g, can not industrialization production, while electric arc melting side
The AgCuTi solder of method preparation is easy to appear tissue odds, Ti element part segregation phenomenon since arc light irradiation area is narrow, so that
AgCuTi solder performance deteriorates, it is difficult to normal use.And vacuum smelting method has one in terms of preparing powdery AgCuTi solder
Fixed advantage, but when preparing AgCuTi foil solder, due to easily entraining Impurity Fe, C etc. in course of hot rolling, so that
Processing performance, the mechanical properties decrease of AgCuTi solder, it is subsequent to cannot be processed shape, while being difficult to meet the performance of engineer application
Index request.Therefore, electric arc melting and vacuum smelting method have certain limitation in terms of preparing AgCuTi foil solder.
Summary of the invention
It is an object of the invention to the deficiencies and Titanium Electroplating technology for above-mentioned existing AgCuTi solder forming, provide one kind
The AgCuTi solder haveing excellent performance, and easily forming, preparation method high in machining efficiency, at low cost are provided.
The object of the present invention is achieved in the following manner:
A kind of AgCuTi solder, including AgCu matrix solder and the Titanium electroplated layer that is coated on outside AgCu matrix solder,
It is the solid solution and Titanium electroplated layer generation diffusion reaction in AgCu matrix solder between matrix solder and Titanium electroplated layer
The transition zone of formation.
Percentage thickness between the AgCu matrix solder, transition zone and titanium electroplated layer be respectively as follows: matrix solder 65.0 ~
92.0 %, 7.5 ~ 33.5 % of transition zone, 0.5 ~ 1.5 % of metal layer.
The AgCuTi solder with a thickness of 15 ~ 85 μm.
The element Y for being also matrix solder 0.5-1.0 % containing quality in the AgCu matrix solder.
The preparation method of AgCuTi solder as described above, comprising the following steps:
(1) prefabricated AgCu matrix solder；
(2) using AgCu matrix solder as cathode, simple substance titanium is anode, in AgCu matrix solder electroplating surface titanium coating；
(3) after titanium technique to be electroplated, 1 ~ 10 min is permeated into its vacuum drying at 1650 ~ 1700 DEG C, then
After spreading 2 ~ 30 h in 1550 ~ 1650 DEG C of vacuum drying ovens, AgCuTi solder is made after cooling.
The step (2) specifically: first in every 1000mL deionized water be added 0.146 ~ 0.208 moL of titanium sulfate,
0.07 ~ 0.176 moL of sodium sulphate, 0.736 ~ 1.288moL of sulfuric acid, 10 ~ 25 g of surfactant are configured to electroplate liquid, then will
Cathode AgCu matrix solder, anode simple substance titanium, which immerse in electroplate liquid, implements Titanium Electroplating.
0.003 ~ 0.008 moL of sodium vanadate is additionally added in every 1000mL electroplate liquid.
The surfactant is alkyl ether surfactant.
The alkyl ether surfactant be OP-10, ethoxylated dodecyl alcohol, polyethylene glycol trimethyl nonyl ethers,
Any one of nonylphenol polyoxyethylene ether.
The electrodeposition of titanium carries out under vacuum environment or inert gas shielding environment, technological parameter are as follows: current density 0.5
~5 A/dm2, 35 ~ 50 DEG C of electroplating solution temperature, 2 ~ 15 min of plating time.
The preparation method of AgCuTi foil solder provided by the invention, it is simple, convenient, breach conventional method preparation
The technical bottleneck of solder provides a kind of new Method of Green Manufacture for the high-quality active solder of neomorph.To AgCuTi pricker
For material, the content of active element Ti in AgCuTi solder is improved, traditional AgCuTi solder is overcome and is difficult to shape and melt
The shortcomings that salt system Titanium Electroplating, this method have many advantages, such as easily shape, it is high in machining efficiency, at low cost, be AgCuTi solder system
It makes production and a kind of new technological approaches is provided.
In addition, using binary and the above silver alloy as matrix, such as silver-colored nickel, silver-colored manganese, Ag-Cu-Zn, silver-bearing copper nickel, using the present invention
Preparation method prepares titaniferous silver-base alloy or silver solder in the invention patent protection scope in its ti coat on diamond.
Specific embodiment
Embodiment 1
A kind of AgCuTi solder, including AgCu matrix solder and the Titanium electroplated layer that is coated on outside AgCu matrix solder,
It is the solid solution and Titanium electroplated layer generation diffusion reaction in AgCu matrix solder between matrix solder and Titanium electroplated layer
The transition zone of formation；Percentage thickness between AgCu matrix solder, transition zone and titanium electroplated layer is respectively as follows: matrix solder
65.0 ~ 92.0 %, 7.5 ~ 33.5 % of transition zone, 0.5 ~ 1.5 % of metal layer；AgCuTi solder with a thickness of 15 ~ 85 μm；Into
One step is also matrix solder containing quality in addition to the Ag containing 50-70 %, the Cu of 29.0-49.5 % in AgCu matrix solder
The Y of 0.5-1.0%, Y, which is added, can refine the tissue of matrix solder, improve the mechanical property of matrix solder, be the forming of matrix solder
It lays the foundation.
The preparation method of AgCuTi solder as described above, comprising the following steps:
(1) prefabricated AgCu matrix solder: raw metal Ag, Cu and micro Y are put into smelting furnace first, cast, are moved back
Fire squeezes, roll forming, is made as AgCu matrix solder in advance；
(2) using AgCu matrix solder as cathode, simple substance titanium is anode, in AgCu matrix solder electroplating surface titanium coating；
(3) after titanium technique to be electroplated, dry infiltration 1 ~ 10 in the vacuum environment at 1650 ~ 1700 DEG C by it
Min, then after 1550 ~ 1650 DEG C of 2 ~ 30 h of diffusion in vacuum, to form transition zone；Then furnace cooling, be made with a thickness of 15 ~
85 μm of AgCuTi solder.Wherein, transition zone facilitates matrix solder and titanium coating forms metallurgical bonding, improves between the two
Binding force, while the mechanical property of AgCuTi solder can be improved, regulates and controls combination interface tissue and object phase composition, help to enhance
The active function of AgCuTi solder；If titanium electroplated layer (1660 DEG C) and (770 ~ 795 DEG C) of matrix solder are molten without transition zone
It is larger to change temperature difference, silver-bearing copper titanium alloy is difficult to shape, is easy embrittlement, does not have the effect of active solder.
Step (2) specifically: using AgCu matrix solder as cathode, using simple substance titanium as anode, to be added in every 1000mL water
0.146 ~ 0.208 moL of titanium sulfate, 0.07 ~ 0.176 moL of sodium sulphate, 0.736 ~ 1.288moL of sulfuric acid, surfactant 10 ~ 25
G is formulated as electroplate liquid, and electric current, voltage is arranged, and under vacuum environment or inert gas shielding environment, implements electrodeposition of titanium；Electricity is heavy
Product titanium technological parameter are as follows: 0.5 ~ 5 A/dm of current density2, 3 ~ 6 V of voltage, 35 ~ 50 DEG C of electroplating solution temperature, plating time 2 ~
15 min。
Preferably, 0.003 ~ 0.008 moL of dispersing agent sodium vanadate, the surface-active are additionally added in every 1000mL electroplate liquid
Agent is alkyl ether surfactant, is further OP-10, ethoxylated dodecyl alcohol, polyethylene glycol trimethyl nonyl ethers, nonyl
Any one of base phenol polyethenoxy ether.
The invention has the following advantages that
1) electrodeposition of titanium-infiltration-diffusion composite preparation process provided by the invention, overcomes traditional AgCuTi foil solder
It is difficult to shape and the deficiency of conventional electroplating method, provides a kind of new way for the forming of neomorph AgCuTi solder；2) matrix pricker
Contain microelement Y in material, can refine the tissue of matrix solder, improve the mechanical property of matrix solder, be matrix solder at
Shape lays the foundation；3) electrodeposition of titanium method provided by not only can implement titanizing, but also weld in monometallic, alloy surface
Material surface titanizing is connect, the forming for neomorph metal material especially titaniferous welding material provides a kind of new approaches；4) electricity is heavy
Bath temperature applied in product titanium process is low, the time is short, and deposition rate is high, has energy conservation, consumption reduction effect；5) electro-deposition
Titanium-infiltration-diffusion composite preparation process is implemented under vacuum environment (or inert gas shielding), and the AgCuTi solder of preparation is clean
Degree is high, does not contain any impurity；6) current density, bath temperature, plating time, bath concentration multi-parameter Collaborative Control skill are used
Art improves the content of active element Ti in AgCuTi solder by the thickness of regulation titanium electroplated layer, transition zone.
Embodiment 2
A kind of AgCuTi solder contains yttrium 0.5% by matrix solder BAg55Cu() and be coated on outside BAg55Cu matrix solder
Titanium electroplated layer composition, transition zone be AgTi compound phase and CuTi, CuYTi compound phase composition.Matrix solder, transition
Layer, the percentage thickness of electroplated layer are as follows, matrix solder: 85.0 %, transition zone: 14.5 %, electroplated layer: 0.5 %.
The preparation method of AgCuTi solder as described above, comprising the following steps:
550 g of metallic silver, 445 g of copper, 5 g of yttrium are placed in smelting furnace first, through casting, annealing, extruding, roll forming,
It is made as in advance with a thickness of 30 μm of ribbon base solder BAg55Cu；Then positive and negative in BAg55Cu matrix solder using Titanium Electroplating technique
Face Titanium Electroplating (10 μm of single side thickness)；After technique to be electroplated, puts it into 1700 DEG C of vacuum oven and permeate 8
Min is then placed in after spreading 20 h in 1650 DEG C of vacuum drying oven, furnace cooling, and the AgCuTi solder with a thickness of 35 μm is made.
Wherein: plating titanium solution is by 50 g/L(0.208moL/L of titanium sulfate), 25 g/L(0.176moL/L of sodium sulphate), matter
Amount score is 98% concentrated sulfuric acid, 70 ml/L(1.288moL/L), 25 g of OP-10/L, 1000 ml of deionized water composition.Specific electricity
Technology for plating titanium parameter is as follows: 5 A/dm of current density2, 3 V of voltage, 50 DEG C of solution temperature, 4 min of plating time, the Titanium Electroplating
Technique carries out in helium protection environment.
The AgCuTi solder of above method preparation, compared with matrix solder BAg55Cu, silver content reduces by 9.3%, soaks face
Product improves 12.5 %.
Embodiment 3
A kind of AgCuTi solder, by matrix solder BAg60Cu(0.8 % containing yttrium) and be coated on outside BAg60Cu matrix solder
Titanium electroplated layer composition, transition zone be AgTi compound phase and CuTi, CuYTi compound phase composition.Matrix solder, transition
Layer, the percentage thickness of electroplated layer are as follows, matrix solder: 92.0 %, transition zone: 7.5 %, electroplated layer: 0.5 %.
The preparation method of AgCuTi solder as described above, comprising the following steps:
600 g of metallic silver, 392 g of copper, 8 g of yttrium are placed in smelting furnace first, through casting, annealing, extruding, roll forming,
It is made as in advance with a thickness of 40 μm of ribbon base solder BAg60Cu；Then positive and negative in BAg60Cu matrix solder using Titanium Electroplating technique
Face Titanium Electroplating (15 μm of single side thickness)；After titanium technique to be electroplated, puts it into 1700 DEG C of vacuum oven and permeate 10
Min is then placed in after spreading 30 h in 1650 DEG C of vacuum drying oven, furnace cooling, and the AgCuTi solder with a thickness of 43 μm is made.
Wherein: plating titanium solution is by titanium sulfate 35g/L(0.146moL/L), 10 g/L(0.07moL/L of sodium sulphate), quality
Score is 98% concentrated sulfuric acid, 40 ml/L(0.736moL/L), 10 g of ethoxylated dodecyl alcohol/L, 1000 ml group of deionized water
At.Specific electroplating technological parameter is as follows: 1.5 A/dm of current density2, 3.5 V of voltage, 35 DEG C of solution temperature, plating time 15
Min, the Titanium Electroplating technique carry out in vacuum environment.
The AgCuTi solder of above method preparation, compared with matrix solder BAg60Cu, silver content reduces by 7.2 %, soaks face
Product improves 9.5 %.
Embodiment 4
A kind of AgCuTi solder, by matrix solder BAg50Cu(0.6 % containing yttrium) and be coated on outside matrix solder BAg50Cu
Titanium electroplated layer composition, transition zone be AgTi compound phase and CuTi, CuYTi compound phase composition.Matrix solder, transition
Layer, the percentage thickness of electroplated layer are as follows, matrix solder: 65.0 %, transition zone: 33.5 %, electroplated layer: 1.5 %.
The preparation method of AgCuTi solder as described above, comprising the following steps:
500 g of metallic silver, 494 g of copper, 6 g of yttrium are placed in smelting furnace first, through casting, annealing, extruding, roll forming,
It is made as in advance with a thickness of 10 μm of ribbon base solder BAg50Cu；Then positive and negative in BAg50Cu matrix solder using Titanium Electroplating technique
Face Titanium Electroplating (5 μm of single side thickness)；After technique to be electroplated, puts it into 1650 DEG C of vacuum oven and permeate 1
Min is then placed in after spreading 2 h in 1550 DEG C of vacuum drying oven, furnace cooling, and the AgCuTi solder with a thickness of 15 μm is made.
Wherein: plating titanium solution is by 40 g/L(0.167moL/L of titanium sulfate), 20 g/L(0.141moL/L of sodium sulphate), matter
Amount score is 98% concentrated sulfuric acid, 55 ml/L(1.012moL/L), 15 g of polyethylene glycol trimethyl nonyl ethers/L, deionized water 1000
Ml composition.Specific electroplating technological parameter is as follows: 3.5 A/dm of current density2, 6 V of voltage, 40 DEG C of solution temperature, plating time 2
Min, the Titanium Electroplating technique carry out in argon gas protection environment.
The AgCuTi solder of above method preparation, compared with matrix solder BAg50Cu, silver content reduces by 8.5%, soaks face
Product improves 20.7 %.
Embodiment 5
A kind of AgCuTi solder contains yttrium 0.9% by matrix solder BAg70Cu() and be coated on outside matrix solder BAg70Cu
Titanium electroplated layer composition, transition zone are AgTi compound phase and CuTi, CuYTi compound phase composition.Matrix solder, transition
Layer, the percentage thickness of electroplated layer are as follows, matrix solder: 75.0 %, transition zone: 24.0 %, electroplated layer: 1.0 %.As described above
AgCuTi solder preparation method, comprising the following steps:
700 g of metallic silver, 291 g of copper, 9 g of yttrium are placed in smelting furnace first, through casting, annealing, extruding, roll forming,
It is made as in advance with a thickness of 65 μm of ribbon base solder BAg70Cu；Then positive and negative in BAg70Cu matrix solder using Titanium Electroplating technique
Face Titanium Electroplating (15 μm of single side thickness)；After technique to be electroplated, puts it into 1700 DEG C of vacuum oven and permeate 6
Min is then placed in after spreading 24 h in 1650 DEG C of vacuum drying oven, furnace cooling, and the AgCuTi solder with a thickness of 85 μm is made.
Wherein: plating titanium solution is by 45 g/L(0.188moL/L of titanium sulfate), 22 g/L(0.155moL/L of sodium sulphate), matter
Amount score is 98% concentrated sulfuric acid, 60 ml/L(1.104moL/L), 18 g of nonylphenol polyoxyethylene ether/L, 1000 ml of deionized water
Composition.Specific electroplating technological parameter is as follows: 3.5 A/dm of current density2, 5 V of voltage, 42 DEG C of solution temperature, plating time 8
Min, the Titanium Electroplating technique carry out in helium protection environment.
The AgCuTi solder of above method preparation, compared with matrix solder BAg70Cu, silver content reduces by 7.6 %, soaks face
Product improves 16.8 %.
Embodiment 6
A kind of AgCuTi solder, by matrix solder BAg65Cu(1.0 % containing yttrium) and be coated on outside matrix solder BAg65Cu
Titanium electroplated layer composition, transition zone be AgTi compound phase and CuTi, CuYTi compound phase composition.Matrix solder, transition
Layer, the percentage thickness of electroplated layer are as follows, matrix solder: 68.5 %, transition zone: 30.0 %, electroplated layer: 1.5 %.
The preparation method of AgCuTi solder as described above, comprising the following steps:
650 g of metallic silver, 340 g of copper, 10 g of yttrium are placed in smelting furnace first, through casting, annealing, extruding, roll forming,
It is made as in advance with a thickness of 50 μm of ribbon base solder BAg65Cu；Then positive and negative in BAg65Cu matrix solder using Titanium Electroplating technique
Face Titanium Electroplating (15 μm of single side thickness)；After technique to be electroplated, puts it into 1650 DEG C of vacuum oven and permeate 6
Min is then placed in after spreading 20 h in 1550 DEG C of vacuum drying oven, furnace cooling, and the AgCuTi solder with a thickness of 72 μm is made.
Wherein: plating titanium solution is by 40 g/L(0.167moL/L of titanium sulfate), 20 g/L(0.141moL/L of sodium sulphate), matter
Amount score is 98% concentrated sulfuric acid, 55 ml/L(1.012moL/L), 20 g/L of polyethylene glycol trimethyl nonyl ethers, deionized water 1000
Ml composition.Specific electroplating technological parameter is as follows: 3.2 A/dm of current density2, 6 V of voltage, 45 DEG C of solution temperature, plating time
6.5 min, the Titanium Electroplating technique carry out in vacuum environment.
The AgCuTi solder of above method preparation, compared with matrix solder BAg65Cu, silver content reduces by 6.5 %, soaks face
Product improves 11.7 %.
Embodiment 7
A kind of AgCuTi solder, by matrix solder BAg50Cu(0.5 % containing yttrium) and be coated on outside matrix solder BAg50Cu
Titanium electroplated layer composition, transition zone be AgTi compound phase and CuTi, CuYTi compound phase composition.Matrix solder, transition
Layer, the percentage thickness of electroplated layer are as follows, matrix solder: 80%, transition zone: and 18.8%, electroplated layer: 1.2 %.
The preparation method of AgCuTi solder as described above, comprising the following steps:
500 g of metallic silver, copper 495g, 5 g of yttrium are placed in smelting furnace first, through casting, annealing, extruding, roll forming, in advance
It is made as with a thickness of 50 μm of ribbon base solder BAg50Cu；Then using Titanium Electroplating technique in BAg50Cu matrix solder front and back sides
Titanium Electroplating (10 μm of single side thickness)；After technique to be electroplated, puts it into 1680 DEG C of vacuum oven and permeates 4 min,
It is then placed in after spreading 2 h in 1600 DEG C of vacuum drying oven, furnace cooling, the AgCuTi solder with a thickness of 60 μm is made.
Wherein: plating titanium solution is by titanium sulfate 0.18moL/L, sodium sulphate 0.12moL/L, sodium vanadate 0.008moL/L, matter
Amount score is 98% concentrated sulfuric acid 1moL/L, 20 g/L of nonylphenol polyoxyethylene ether, 1000 ml of deionized water composition.Specific galvanizer
Skill parameter is as follows: 0.5 A/dm of current density2, 3 V of voltage, 45 DEG C of solution temperature, plating time 15min, the Titanium Electroplating technique
It is carried out in helium protection environment.
The AgCuTi solder of above method preparation, compared with matrix solder BAg50Cu, silver content reduces by 6.1%, soaks face
Product improves 10.5%.
Embodiment 8
A kind of AgCuTi solder, by matrix solder BAg55Cu(1 % containing yttrium) and be coated on outside matrix solder BAg55Cu
Titanium electroplated layer composition, transition zone are AgTi compound phase and CuTi, CuYTi compound phase composition.Matrix solder, transition
Layer, the percentage thickness of electroplated layer are as follows, matrix solder: 90%, transition zone: and 9%, electroplated layer: 1 %.
The preparation method of AgCuTi solder as described above, comprising the following steps:
550 g of metallic silver, copper 440g, 10 g of yttrium are placed in smelting furnace first, through casting, annealing, extruding, roll forming,
It is made as in advance with a thickness of 50 μm of ribbon base solder BAg55Cu；Then positive and negative in BAg55Cu matrix solder using Titanium Electroplating technique
Face Titanium Electroplating (12 μm of single side thickness)；After technique to be electroplated, puts it into 1670 DEG C of vacuum oven and permeate 8
Min is then placed in after spreading 15 h in 1600 DEG C of vacuum drying oven, furnace cooling, and the AgCuTi solder with a thickness of 50 μm is made.
Wherein: plating titanium solution is by titanium sulfate 0.16moL/L, sodium sulphate 0.07moL/L, sodium vanadate 0.005moL/L, matter
Amount score is 98% concentrated sulfuric acid 1.2moL/L, 18 g/L of ethoxylated dodecyl alcohol, 1000 ml of deionized water composition.Specific plating
Technological parameter is as follows: 2 A/dm of current density2, 3.5 V of voltage, 40 DEG C of solution temperature, plating time 10min, the Titanium Electroplating work
Skill carries out in argon gas protection environment.
The AgCuTi solder of above method preparation, compared with matrix solder BAg55Cu, silver content reduces by 8.5%, soaks face
Product improves 11.4%.
Embodiment 9
A kind of AgCuTi solder, by matrix solder BAg65Cu(1 % containing yttrium) and be coated on outside matrix solder BAg65Cu
Titanium electroplated layer composition, transition zone are AgTi compound phase and CuTi, CuYTi compound phase composition.Matrix solder, transition
Layer, the percentage thickness of electroplated layer are as follows, matrix solder: 70%, transition zone: and 29.2%, electroplated layer: 0.8 %.
The preparation method of AgCuTi solder as described above, comprising the following steps:
650 g of metallic silver, copper 340g, 10 g of yttrium are placed in smelting furnace first, through casting, annealing, extruding, roll forming,
It is made as in advance with a thickness of 20 μm of ribbon base solder BAg65Cu；Then positive and negative in BAg65Cu matrix solder using Titanium Electroplating technique
Face Titanium Electroplating (6 μm of single side thickness)；After technique to be electroplated, puts it into 1660 DEG C of vacuum oven and permeate 5
Min is then placed in after spreading 25 h in 1580 DEG C of vacuum drying oven, furnace cooling, and the AgCuTi solder with a thickness of 25 μm is made.
Wherein: plating titanium solution is by titanium sulfate 0.2moL/L, sodium sulphate 0.15moL/L, sodium vanadate 0.003moL/L, quality
Score is 98% concentrated sulfuric acid 0.9moL/L, polyethylene glycol trimethyl nonyl ethers 25 g/L, 1000 ml of deionized water composition.Specific electricity
Depositing process parameter is as follows: 1 A/dm of current density2, 3.2 V of voltage, 35 DEG C of solution temperature, plating time 4min, the Titanium Electroplating work
Skill carries out in vacuum environment.
The AgCuTi solder of above method preparation, compared with matrix solder BAg65Cu, silver content reduces by 5.8%, soaks face
Product improves 9.6%.
What has been described above is only a preferred embodiment of the present invention, it is noted that for those skilled in the art,
Without depart from that overall concept of the invention, several changes and improvements can also be made, these also should be considered as of the invention
Protection scope.
Claims (9)
1. a kind of AgCuTi solder, it is characterised in that: including AgCu matrix solder and the metal being coated on outside AgCu matrix solder
Titanium electroplated layer occurs for the solid solution in AgCu matrix solder with Titanium electroplated layer between matrix solder and Titanium electroplated layer
The transition zone that diffusion reaction is formed；
Preparation method includes the following steps:
(1) prefabricated AgCu matrix solder；
(2) using AgCu matrix solder as cathode, simple substance titanium is anode, in AgCu matrix solder electroplating surface titanium coating；
(3) after titanium technique to be electroplated, 1 ~ 10 min is permeated into its vacuum drying at 1650 ~ 1700 DEG C, then in
After spreading 2 ~ 30 h in 1550 ~ 1650 DEG C of vacuum drying ovens, AgCuTi solder is made after cooling.
2. AgCuTi solder as described in claim 1, it is characterised in that: the AgCu matrix solder, transition zone and titanium plating
Percentage thickness between layer is respectively as follows: 65.0 ~ 92.0 % of matrix solder, 7.5 ~ 33.5 % of transition zone, metal layer 0.5 ~ 1.5
%。
3. AgCuTi solder as described in claim 1, it is characterised in that: the AgCuTi solder with a thickness of 15 ~ 85 μm.
4. AgCuTi solder as described in claim 1, it is characterised in that: also containing quality in the AgCu matrix solder is base
The element Y of body solder 0.5-1.0 %.
5. the preparation method of AgCuTi solder according to claim 4, it is characterised in that: the step (2) specifically: first
First 0.146 ~ 0.208 moL of titanium sulfate, 0.07 ~ 0.176 moL of sodium sulphate, sulfuric acid to be added in every 1000mL deionized water
0.736 ~ 1.288moL, 10 ~ 25 g of surfactant are configured to electroplate liquid, then by cathode AgCu matrix solder, anode simple substance
Titanium, which immerses in electroplate liquid, implements Titanium Electroplating.
6. the preparation method of AgCuTi solder according to claim 5, it is characterised in that: in every 1000mL electroplate liquid
It is additionally added 0.003 ~ 0.008 moL of sodium vanadate.
7. the preparation method of AgCuTi solder according to claim 4, it is characterised in that: the surfactant is alkyl
Ether surfactant.
8. the preparation method of AgCuTi solder according to claim 7, it is characterised in that: the alkyl ether surface-active
Agent is any one of OP-10, ethoxylated dodecyl alcohol, polyethylene glycol trimethyl nonyl ethers, nonylphenol polyoxyethylene ether.
9. the preparation method of AgCuTi solder according to claim 5, it is characterised in that: the Titanium Electroplating is in vacuum environment
Or carried out under inert gas shielding environment, technological parameter are as follows: 0.5 ~ 5 A/dm of current density2, 35 ~ 50 DEG C of electroplating solution temperature,
2 ~ 15 min of plating time.
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