CN106282651B - A kind of copper silver rare-earth alloy superfine wire and its production method - Google Patents
A kind of copper silver rare-earth alloy superfine wire and its production method Download PDFInfo
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- CN106282651B CN106282651B CN201610827707.9A CN201610827707A CN106282651B CN 106282651 B CN106282651 B CN 106282651B CN 201610827707 A CN201610827707 A CN 201610827707A CN 106282651 B CN106282651 B CN 106282651B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
- H01B1/026—Alloys based on copper
Abstract
The present invention provides a kind of copper silver rare-earth alloy superfine wires, and the method for the production copper silver rare-earth alloy superfine wire.The copper silver rare-earth alloy superfine wire includes following component：1 ~ 25wt% silver, 0.01 ~ 0.04wt% yttriums, surplus are copper and inevitable impurity；Or 1 ~ 25wt% silver, 0.10 ~ 0.30 wt% lanthanums, surplus are copper and inevitable impurity；Or 1 ~ 25wt% silver, 0.01 ~ 0.02 wt% yttriums, 0.05 ~ 0.15wt% lanthanums, surplus are copper and inevitable impurity.The trace rare-earth that the method passes through addition; play the role of purifying tissue, crystal grain thinning, improve material comprehensive performance; and use anaerobic production technology and non-vacuum continuous fusion-cast method; it being capable of continuous charging melting under inert gas protection; it is continuously cast into copper silver rare-earth alloy bar, realizes continuous production；Moreover, the copper silver rare-earth alloy bar obtained smooth can be drawn into the wire rod of diameter of phi≤0.05mm through follow-up deep processing, final superfine wire product tissue is pure uniformly, oxygen content is low, tensile strength higher, elongation at break bigger, it is not easy to break.
Description
Technical field
The invention belongs to high-end electronic Material Fields, and in particular to a kind of copper silver rare-earth alloy superfine wire, and production institute
The method for stating copper silver rare-earth alloy superfine wire.
Background technology
Kufil is due to having high intensity and highly conductive characteristic concurrently, and with excellent bending, torsion, antifatigue, resistance to
Therefore the comprehensive performances such as heat are processed into ultra-fine wire rod using Kufil conductor and are widely used in Ultrathin coaxial cable, heat-resisting
Electric wire, medical electric wire, audio wire and cable, small-sized vibrations coil, miniature motor etc..
With making rapid progress for science and technology, the information terminals product such as network, space equipment and Medical Devices is to performance
Requirement it is higher and higher, and its volume is smaller and smaller, and weight is more and more lighter, thus corresponding conductor material should also have it is excellent
Comprehensive performance, and with further thin footpath requirement and trend.It follows that this requires associated alloys materials both to have had
Standby performance characteristics, but also with excellent machinability；And Kufil can exactly meet this requirement to a certain extent.
However, when being drawn into 0.05 or less alloy superfine wires of Φ, often there is harsh requirement：Both the alloy in Kufil had been required
Content is high and uniform, and requires impurity content low, otherwise will appear the frequent situation that breaks, to can not achieve the conjunction of long length
Golden superfine wire preparation and application.
In the prior art, CN103572184A discloses a kind of preparation method of high-strength silver-copper alloy material, the conjunction
For golden material according to mass fraction silver content 15-20%, surplus is copper, and the manufacturing method of the alloy material includes mainly：1）Chemistry at
Set up meter separately；2）Vacuum melting prepares Kufil stick；3）Kufil bar is refined using vacuum consumable electrode；4）Hot extrusion；
5）Heat treatment；6）Drawing obtains final products, although obtained Kufil material can have very high intensity and excellent
Different conductivity, however, this method can not realize the continuous production of long length Kufil gold thread, do not refer to yet can be drawn into it is super
Thin wire and still keep high intensity.
For another example, CN104353696A discloses a kind of fine Kufil gold thread manufacturing method, the manufacturing method of the alloy wire
Including：1）The smelting of Cu-Ag alloy blanks and continuous casting；2）The drawing of Kufil bar；3）At the intermediate heat of Cu-Ag alloy wires
Reason；4）Multiple tracks is drawn into fine Kufil gold thread.The wherein smelting of Cu-Ag alloy blanks includes with continuous casting manufacturing method：A) true
Copper silver intermediate alloy is manufactured under the conditions of empty melting+gas shield；B) by copper silver intermediate alloy in vacuum melting+gas shield condition
Lower manufacture Cu-Ag alloy blanks；C) Cu-Ag alloy blanks are cast into Kufil under conditions of vacuum melting+gas shield
Bar.However, this is smelted and continuous casting manufacturing approach craft is complicated, and it is of high cost, though continuously casting can be realized, it can not achieve continuous add
Material, therefore can only the production of property performance period；Also, entire technical process does not roll or extrusion process, to cause following process
As-cast structure in the process cannot completely eliminate, and cause the product mechanical performance of manufacture poor.
At present upward-casting process can founding production high alloy content Kufil, on the one hand since burner hearth area is larger,
It is dumb to produce the adjustment conversion of high alloy content Kufil, on the other hand since burner hearth is generally built up using refractory material, because
During product melting and casting, product is susceptible to refractory material and is mingled with for this, as a result can not continuous drawing superfine wire.
In addition continuous casting and rolling method also can founding production high alloy content Kufil, since its furnace body is much larger than above drawing company
Stove is cast, adjustment conversion is more dumb when to produce high alloy content, and still further aspect is due to generally using hot rolling, oxygen content
Height, therefore be easy to generate hard crisp copper oxide, it is unfavorable for follow-up deep processing.
Therefore, a kind of anaerobic production technology how is scientifically and rationally designed, efficiently to produce the ultra-fine high property of diameter
Energy Kufil gold thread is one of the emphasis that those skilled in the art currently research and develop.
Invention content
In order to solve the above technical problems existing in the prior art, the present invention is intended to provide a kind of high performance copper silver is dilute
Native alloy superfine wire, wherein the trace rare-earth added, plays purification tissue, crystal grain thinning, the work for improving material comprehensive performance
With.To achieve the goals above, inventor has developed a kind of anaerobic production technology, uses non-vacuum continuous fusion-cast method, energy
Enough continuous charging meltings under inert gas protection, are continuously cast into copper silver rare-earth alloy bar, to realize continuous production；And
And the copper silver rare-earth alloy bar obtained smooth can be drawn into the wire rod of diameter of phi≤0.05mm, finally through follow-up deep processing
Product has the characteristics such as tissue is pure uniformly, oxygen content is low, intensity is high.
Therefore, the first aspect of the present invention provides a kind of copper silver rare-earth alloy superfine wire comprising following component：1~
25wt% silver, 0.01 ~ 0.04wt% yttriums, surplus are copper and inevitable impurity；Or 1 ~ 25wt% silver, 0.10 ~ 0.30 wt%
Lanthanum, surplus are copper and inevitable impurity；Or 1 ~ 25wt% silver, 0.01 ~ 0.02 wt% yttriums, 0.05 ~ 0.15wt% lanthanums, surplus
For copper and inevitable impurity.
Preferably, above-mentioned copper silver rare-earth alloy superfine wire includes following component：2 ~ 6wt% silver, 0.012 ~ 0.03wt% yttriums are remaining
Amount is copper and inevitable impurity；Or 2 ~ 6wt% silver, 0.12 ~ 0.25 wt% lanthanums, surplus are copper and inevitable impurity；
Or 2 ~ 6wt% silver, 0.012 ~ 0.015 wt% yttriums, 0.06 ~ 0.12wt% lanthanums, surplus are copper and inevitable impurity.
Preferably, diameter of phi≤0.05mm of above-mentioned copper silver rare-earth alloy superfine wire.
In addition, the second aspect of the present invention, provides a kind of method producing above-mentioned copper silver rare-earth alloy superfine wire, specifically
Include the following steps：
（1）Founding copper silver rare-earth alloy bar, including：
（1-1）Pure copper silver rare-earth alloy blank is prepared using vaccum sensitive stove；
（1-2）Copper silver rare-earth alloy bar is continuously prepared using antivacuum casting furnace；
（2）Using three rollers or the further milling step of two-roller mill（1）Copper silver rare-earth alloy bar obtained, it is dilute to obtain copper silver
Native alloy rolled bar；
（3）The copper silver rare-earth alloy rolled bar is drawn greatly, copper silver rare-earth alloy thick line is drawn into；
（4）Intermediate heat-treatment is carried out to the copper silver rare-earth alloy thick line；
（5）Copper silver rare-earth alloy thick line Jing Guo intermediate heat-treatment is subjected to finish draw, the copper silver rare earth is finally made and closes
Golden superfine wire.
Preferably, in the above-mentioned methods, step（1-1）Including：
Copper, silver, rare earth are proportionally added into the high purity graphite crucible of the vaccum sensitive stove, vacuum meter reading is evacuated to
Number reaches 10-1Pa and after stablizing, is gradually heating to 1200-1300 DEG C, waits for that aluminium alloy starts to splash strongly, stand 20-30 minutes,
To remove the impurity such as O and S in raw material；Then it is cast into copper silver rare-earth alloy blank under vacuum conditions；
In addition, in this step（1-1）In further preferably use following raw material：Self-contained Cu >=the 99.95wt% of copper source
Cathode copper, the silver are originated from the filamentary silver containing Ag >=99.95wt%, the rare earths material content：The wt of Y >=99.9 %, La >=99 wt
%；It should be converted into the pure element quality of 100wt% when actually feeding intake, mentioned component ratio range is then met with pure element quality
It feeds intake.
In this step（1-1）In, melting is further preferably carried out using intermediate frequency vaccum sensitive stove, alloy in blank can be made
Ingredient is more uniform；Using vacuum melting, the part of impurity elements in raw material can be effectively removed.The addition of appropriate rare earth element
It is intended that in next step（1-2）Continuous fusion-cast effectively purifies Kufil matrix, while playing the role of crystal grain thinning, to improve
The comprehensive performance of material product；Excess cannot be added in rare earth element, otherwise can influence the mobility of Kufil liquid, make casting bar
Surface quality declines, and eventually leads to the adverse effect to product comprehensive performance；Rare earth element can not be added very few simultaneously, otherwise
Expected effect and effect are not had.
Preferably, in the above-mentioned methods, step（1-2）Including：
The crucible of the antivacuum casting furnace is high purity graphite crucible, using resistance heating high purity graphite crucible, the height
Pure graphite crucible is provided with blowning installation, and is made of 3 chambers, respectively melt chamber, incubation cavity and casting cavity, chamber and chamber it
Between pass through bottom undercurrent hole be connected to；When production, each chamber is connected with high pure protective gas inside high purity graphite crucible, and crucible periphery uses
Resistive heating device heats, and crucible and a whole set of heating dress are placed in burner hearth, and burner hearth is closed with the external world, use in burner hearth when production
High-purity gas protection is protected, to prevent graphite from aoxidizing at high temperature.Wherein, above-mentioned high pure protective gas is high pure nitrogen（99.999%
More than）Or argon gas（99.999% or more）；It is passed through high pure protective gas in crucible, stirring action can be played, moreover it is possible to realize certain
The deoxygenation of degree or deoxidation effect.Wherein, horizontal casting or continuous up-casting can be selected in fusion-casting process.
Step（1-2）Specified operational procedure it is as follows：By the antivacuum casting furnace with the heating rate of 90-150 DEG C/h
It is gradually heating to 1250-1300 DEG C, i.e. casting temperature, is preferably 1270-1290 DEG C；The blowning installation is opened, it will be high-purity
Nitrogen or argon flow amount are adjusted to 1-2 liters/min；Gradually to addition copper silver rare-earth alloy base in the high purity graphite crucible melting chamber
Material, after molten bath is formed, covers graphite flakes, cladding thickness 20-40mm on melt chamber, incubation cavity, casting cavity；Then into
Row continuous charging keeps the temperature 40-60 minutes, scarfing cinder after aluminium alloy reaches crucible safe capacity；Then, continuously casting Φ=
The copper silver rare-earth alloy bar of 12.5-20mm, casting speed 400-800mm/min, pitch 3-5mm, while continuously casting, root
It continuously feeds into melt chamber according to alloy liquid level and temperature.In order to keep certain static pressure, alloy liquid level to want phase
To stabilization.
Preferably, the above method the step of（2）In：Using arc triangle-circle or ellipse-circular hole system, passage is flat
Equal lengthening coefficient 1.15-1.25, mill speed 10-120m/min.It is further preferred that by the copper silver rare earth of Φ=12.5-20mm
Rod of metal alloy is in this step（2）In be rolled into the thin bar of Φ=6-10mm.
Preferably, the above method the step of（3）The middle draw rate using 50-300m/min is drawn into Φ=2.6-
The copper silver rare-earth alloy thick line of 3mm.
Preferably, in the above-mentioned methods, step（4）Including：
The copper silver rare-earth alloy thick line is put into forvacuum to the inert gas shielding annealing furnace of -0.1MPa, and
Be filled with high pure nitrogen or argon gas thereto, until the inert gas shielding annealing furnace flue in pressure be 0.02 ~
0.05MPa is then warming up to 420-520 DEG C, keeps the temperature 6-8 hours, is finally air-cooled to room temperature with stove.
Preferably, in the above-mentioned methods, step（5）Including：
By the copper silver rare-earth alloy thick line Jing Guo intermediate heat-treatment first be pulled in the draw rate of 400-800m/min Φ=
0.8-1.2mm, passage draft 15-20%；Again Φ=0.15-0.25mm, road are pulled to so that the draw rate of 500-1000m/min is small
Secondary draft 8-13%；Φ=0.025-0.05 mm, passage draft are carefully finally pulled to the draw rate of 800-1500m/min
7-10% obtains the copper silver rare-earth alloy superfine wire.It is further preferred that if it is necessary, can also be after middle drawing, small drawing
Increase an intermediate heat-treatment process before.
Production method step provided by the present invention is simple, easily operated, is suitable for large-scale industrial production；Also, it adopts
The copper silver rare-earth alloy superfine wire oxygen content made from production method provided by the present invention is lower, and impurity content significantly reduces,
Superfine wire made of the drawing is not easy to break, and has conductivity up to standard and higher tensile strength；Therefore, of the present invention
Copper silver rare-earth alloy superfine wire and its production method all have superior application value and good market potential.
Specific implementation mode
The present invention is further elaborated With reference to embodiment, but the present invention is not limited to following embodiment party
Formula.
First aspect provides a kind of copper silver rare-earth alloy superfine wire, including following component：
1 ~ 25wt% silver, 0.01 ~ 0.04wt% yttriums, surplus are copper and inevitable impurity；Or 1 ~ 25wt% silver, 0.10 ~
0.30 wt% lanthanums, surplus are copper and inevitable impurity；Or 1 ~ 25wt% silver, 0.01 ~ 0.02 wt% yttriums, 0.05 ~
0.15wt% lanthanums, surplus are copper and inevitable impurity.
In a preferred embodiment, the copper silver rare-earth alloy superfine wire includes following component：
2 ~ 6wt% silver, 0.012 ~ 0.03wt% yttriums, surplus are copper and inevitable impurity；Or 2 ~ 6wt% silver, 0.12 ~
0.25 wt% lanthanums, surplus are copper and inevitable impurity；Or 2 ~ 6wt% silver, 0.012 ~ 0.015 wt% yttriums, 0.06 ~
0.12wt% lanthanums, surplus are copper and inevitable impurity.
In a preferred embodiment, diameter of phi≤0.05mm of the copper silver rare-earth alloy superfine wire.
Second aspect provides a kind of method of the copper silver rare-earth alloy superfine wire produced described in first aspect present invention, packet
Include following steps：
（1）Founding copper silver rare-earth alloy bar, including：
（1-1）Pure copper silver rare-earth alloy blank is prepared using vaccum sensitive stove；
（1-2）Copper silver rare-earth alloy bar is continuously prepared using antivacuum casting furnace；
（2）Using three rollers or the further milling step of two-roller mill（1）Copper silver rare-earth alloy bar obtained, it is dilute to obtain copper silver
Native alloy rolled bar；
（3）The copper silver rare-earth alloy rolled bar is drawn greatly, copper silver rare-earth alloy thick line is drawn into；
（4）Intermediate heat-treatment is carried out to the copper silver rare-earth alloy thick line；
（5）Copper silver rare-earth alloy thick line Jing Guo intermediate heat-treatment is subjected to finish draw, the copper silver rare earth is finally made and closes
Golden superfine wire.
In a preferred embodiment, step（1-1）Including：
Copper, silver, rare earth are proportionally added into the high purity graphite crucible of the vaccum sensitive stove, vacuum meter reading is evacuated to
Number reaches 10-1Pa and after stablizing, is gradually heating to 1200-1300 DEG C, waits for that aluminium alloy starts to splash strongly, stand 20-30 minutes,
Then copper silver rare-earth alloy blank is cast into graphite casting mould under vacuum conditions.
In a preferred embodiment, step（1-2）Including：
Using resistance heating high purity graphite crucible, the high purity graphite crucible is provided with blowning installation, and by 3 chamber groups
At respectively melt chamber, incubation cavity and casting cavity are connected between chamber and chamber by bottom undercurrent hole；By the antivacuum founding
Stove is gradually heating to 1250-1300 DEG C, opens the blowning installation, and high pure nitrogen or argon flow amount are adjusted to 1-2 liters/min；
Gradually to addition copper silver rare-earth alloy blank in the high purity graphite crucible melting chamber, after molten bath is formed, in melt chamber, heat preservation
Graphite flakes are covered on chamber, casting cavity；Then continuous charging is carried out, after aluminium alloy reaches crucible safe capacity, keeps the temperature 40-
60 minutes, scarfing cinder；Then, the copper silver rare-earth alloy bar of continuously casting Φ=12.5-20mm, casting speed 400-800mm/min,
Pitch 3-5mm continuously feeds into melt chamber while continuously casting according to alloy liquid level and temperature.
In a preferred embodiment, step（2）In：Using arc triangle-circle or ellipse-circular hole system, passage is flat
Equal lengthening coefficient 1.15-1.25, mill speed 10-120m/min.
In a preferred embodiment, step（3）The middle draw rate using 50-300m/min is drawn into Φ=2.6-
The copper silver rare-earth alloy thick line of 3mm.
In a preferred embodiment, step（4）Including：
The copper silver rare-earth alloy thick line is put into forvacuum to the inert gas shielding annealing furnace of -0.1MPa, and
Be filled with high pure nitrogen or argon gas thereto, until the inert gas shielding annealing furnace flue in pressure be 0.02 ~
0.05MPa is then warming up to 420-520 DEG C, keeps the temperature 6-8 hours, is finally air-cooled to room temperature with stove.
In a preferred embodiment, step（5）Including：
By the copper silver rare-earth alloy thick line Jing Guo intermediate heat-treatment first be pulled in the draw rate of 400-800m/min Φ=
0.8-1.2mm, passage draft 15-20%；Again Φ=0.15-0.25mm, road are pulled to so that the draw rate of 500-1000m/min is small
Secondary draft 8-13%；Φ=0.025-0.05 mm, passage draft are carefully finally pulled to the draw rate of 800-1500m/min
7-10% obtains the copper silver rare-earth alloy superfine wire.
Embodiment 1
Prepare copper silver yittrium alloy superfine wire：
（1）Founding copper silver yittrium alloy bar, including：
（1-1）Pure copper silver yittrium alloy blank is prepared using vaccum sensitive stove：
Using the cathode copper of Cu purity 99.99wt%, the 99.9 wt %'s of filamentary silver and Y purity of Ag purity 99.99wt%
Rare-earth yttrium is raw material；According to 2wt%Ag, 0.015wt%Y, surplus is copper and inevitable impurity this proportioning, by the electrolysis
Copper, the filamentary silver are added with the rare-earth yttrium in the high purity graphite crucible of intermediate frequency vaccum sensitive stove, are evacuated to vacuum meter reading
Reach 10-1Pa and after stablizing, is gradually heating to 1250 DEG C, waits for that aluminium alloy starts to splash strongly, stand 20-30 minute, to remove
The impurity such as O and S in raw material；Then it is cast into the copper silver yittrium alloy blank of Φ=50mm under vacuum conditions；
（1-2）Copper silver yittrium alloy bar is continuously prepared using antivacuum casting furnace：
Antivacuum casting furnace is gradually heating to 1250-1260 DEG C with the heating rate of 90 DEG C/h, opens high purity graphite earthenware
Blowning installation in crucible, by high pure nitrogen（99.999% or more）Flow is adjusted to 1 liter/min；Gradually to the high purity graphite crucible
Copper silver yittrium alloy blank is added in melt chamber, after molten bath is formed, graphite flakes are covered on melt chamber, incubation cavity, casting cavity,
Cladding thickness is 30mm；Then it is continuously added to copper silver yittrium alloy blank, after aluminium alloy reaches crucible safe capacity, keeps the temperature 50 points
Clock, scarfing cinder；Then, horizontal casting is at the copper silver yittrium alloy bar of Φ=12.5mm, casting speed 650mm/min, pitch 5mm, even
While continuous casting, continuously fed in time into melt chamber according to alloy liquid level and temperature；
（2）The copper silver yittrium alloy bar of above-mentioned Φ=12.5mm is further rolled into the copper silver yttrium of Φ=8mm through three-high mill
Alloy rolled bar, wherein use arc triangle-round pass system, passage mean coefficient of elongation 1.20, mill speed 60m/min；
（3）The copper silver yittrium alloy rolled bar of above-mentioned Φ=8mm is drawn greatly with the draw rate of 50m/min, is drawn into Φ
The copper silver yittrium alloy thick line of=3mm；
（4）Intermediate heat-treatment is carried out to the copper silver yittrium alloy thick line：
The copper silver yittrium alloy thick line of above-mentioned Φ=3mm is put into forvacuum to the nitrogen protection annealing furnace of -0.1MPa,
And it is filled with high pure nitrogen thereto, until pressure is 0.02MPa in the flue of the nitrogen protection annealing furnace, then heating 1 is small
Up to 420 DEG C, 6 hours are kept the temperature, is finally air-cooled to room temperature with stove；
（5）By the copper silver yittrium alloy thick line Jing Guo intermediate heat-treatment first be pulled in the draw rate of 500m/min Φ=
0.9mm, passage draft 15%；Again Φ=0.16mm, passage draft 13% are pulled to so that the draw rate of 1000m/min is small；Finally
The mm of Φ=0.025 are carefully pulled to the draw rate of 1500m/min, it is super that the copper silver yittrium alloy is finally made in passage draft 7%
Filament.
Embodiment 2
Prepare copper silver lanthanum alloy superfine wire：
（1）Founding copper silver lanthanum alloy bar, including：
（1-1）Pure copper silver lanthanum alloy blank is prepared using vaccum sensitive stove：
Using the cathode copper of Cu purity 99.99wt%, the 99 wt %'s of filamentary silver and La purity of Ag purity 99.99wt% is dilute
Native lanthanum is raw material；According to 4wt%Ag, 0.12wt%La, surplus is copper and inevitable impurity this proportioning, by the electrolysis
Copper, the filamentary silver are added with the Rare Earth Lanthanum in the high purity graphite crucible of intermediate frequency vaccum sensitive stove, are evacuated to vacuum meter reading
Reach 10-1Pa and after stablizing, is gradually heating to 1250 DEG C, waits for that aluminium alloy starts to splash strongly, stand 20-30 minute, to remove
The impurity such as O and S in raw material；Then the copper silver lanthanum alloy blank of Φ=50mm is cast into graphite casting mould under vacuum conditions；
（1-2）Copper silver lanthanum alloy bar is continuously prepared using antivacuum casting furnace：
Antivacuum casting furnace is gradually heating to 1260-1270 DEG C with the heating rate of 120 DEG C/h, opens high purity graphite earthenware
Blowning installation in crucible, by high-purity argon gas（99.999% or more）Flow is adjusted to 1.5 liters/min；Gradually to the high purity graphite earthenware
Copper silver lanthanum alloy blank is added in crucible melt chamber, after molten bath is formed, graphite squama is covered on melt chamber, incubation cavity, casting cavity
Piece, cladding thickness 30mm；Then it is continuously added to copper silver lanthanum alloy blank, after aluminium alloy reaches crucible safe capacity, heat preservation
50 minutes, scarfing cinder；Then, continuous up-casting is at the copper silver lanthanum alloy bar of Φ=16mm, casting speed 550mm/min, pitch 4mm,
While continuously casting, continuously fed in time into melt chamber according to alloy liquid level and temperature；
（2）The copper silver lanthanum that the copper silver lanthanum alloy bar of above-mentioned Φ=16mm is further rolled into Φ=8mm through two-roller mill closes
Golden rolled bar, wherein use ellipse-circular hole system, passage mean coefficient of elongation 1.20, mill speed 80m/min；
（3）The copper silver lanthanum alloy rolled bar of above-mentioned Φ=8mm is drawn greatly with the draw rate of 100m/min, is drawn into
The copper silver lanthanum alloy thick line of Φ=2.6mm；
（4）Intermediate heat-treatment is carried out to the copper silver lanthanum alloy thick line：
The argon gas that the copper silver lanthanum alloy thick line of above-mentioned Φ=2.6mm is put into forvacuum to -0.1MPa is protected into annealing furnace
In, and it is filled with high-purity argon gas thereto, until pressure is 0.02MPa in the flue of argon gas protection annealing furnace, then heats up 1
Hour to 450 DEG C, keeps the temperature 7 hours, is finally air-cooled to room temperature with stove；
（5）By the copper silver lanthanum alloy thick line Jing Guo intermediate heat-treatment first be pulled in the draw rate of 500m/min Φ=
1.2mm, passage draft 15%；Again Φ=0.20mm, passage draft 13% are pulled to so that the draw rate of 1000m/min is small；Finally
The mm of Φ=0.03 are carefully pulled to the draw rate of 1500m/min, it is ultra-fine that the copper silver lanthanum alloy is finally made in passage draft 7%
Line.
Embodiment 3
Prepare copper silver yttrium lanthanum alloy superfine wire：
（1）Founding copper silver yttrium lanthanum alloy bar, including：
（1-1）Pure copper silver yttrium lanthanum alloy blank is prepared using vaccum sensitive stove：
Using the cathode copper of Cu purity 99.99wt%, the filamentary silver of Ag purity 99.99wt%, the rare earth of 99.9 wt % of Y purity
The Rare Earth Lanthanum of 99 wt % of yttrium and La purity is raw material；According to 6wt%Ag, 0.012wt%Y, 0.06wt%La, surplus is copper and can not
Intermediate frequency vacuum sense is added in the cathode copper, the filamentary silver, the rare-earth yttrium and the Rare Earth Lanthanum by this proportioning of the impurity avoided
It answers in the high purity graphite crucible of stove, is evacuated to vacuum meter reading and reaches 10-1Pa and after stablizing, is gradually heating to 1300 DEG C, waits for
Aluminium alloy starts to splash strongly, 20-30 minutes is stood, to remove the impurity such as O and S in raw material；Then under vacuum conditions
The copper silver yttrium lanthanum alloy blank of Φ=50mm is cast as with graphite casting mould；
（1-2）Copper silver yttrium lanthanum alloy bar is continuously prepared using antivacuum casting furnace：
Antivacuum casting furnace is gradually heating to 1270-1280 DEG C with the heating rate of 150 DEG C/h, opens high purity graphite earthenware
Blowning installation in crucible, by high-purity argon gas（99.999% or more）Flow is adjusted to 2 liters/min；Gradually to the high purity graphite crucible
Copper silver yttrium lanthanum alloy blank is added in melt chamber, after molten bath is formed, graphite squama is covered on melt chamber, incubation cavity, casting cavity
Piece, cladding thickness 30mm；Then it is continuously added to copper silver yttrium lanthanum alloy blank, after aluminium alloy reaches crucible safe capacity, is protected
Temperature 50 minutes, scarfing cinder；Then, continuous up-casting is at the copper silver yttrium lanthanum alloy bar of Φ=20mm, casting speed 450mm/min, pitch
3mm continuously feeds into melt chamber while continuously casting according to alloy liquid level and temperature in time；
（2）The copper silver yttrium lanthanum alloy bar of above-mentioned Φ=20mm is further rolled into the copper silver yttrium of Φ=8mm through two-roller mill
Lanthanum alloy rolled bar, wherein use ellipse-circular hole system, passage mean coefficient of elongation 1.20, mill speed 100m/min；
（3）The copper silver yttrium lanthanum alloy rolled bar of above-mentioned Φ=8mm is drawn greatly with the draw rate of 150m/min, is drawn
At the copper silver yttrium lanthanum alloy thick line of Φ=2.8mm；
（4）Intermediate heat-treatment is carried out to the copper silver yttrium lanthanum alloy thick line：
The copper silver yttrium lanthanum alloy thick line of above-mentioned Φ=2.8mm is put into forvacuum to the nitrogen protection annealing furnace of -0.1MPa
In, and it is filled with high pure nitrogen thereto, until pressure is 0.02MPa in the flue of the nitrogen protection annealing furnace, then heats up 1
Hour to 480 DEG C, keeps the temperature 8 hours, is finally air-cooled to room temperature with stove；
（5）By the copper silver yttrium lanthanum alloy thick line Jing Guo intermediate heat-treatment first be pulled in the draw rate of 700m/min Φ=
1.2mm, passage draft 20%；Again Φ=0.25mm, passage draft 12% are pulled to so that the draw rate of 900m/min is small；Finally
The mm of Φ=0.04 are carefully pulled to the draw rate of 1300m/min, it is super that the copper silver yttrium lanthanum alloy is finally made in passage draft 8%
Filament.
Comparative example 1
Prepare Kufil superfine wire：
（1）Founding Kufil bar, including：
（1-1）Kufil blank is prepared using vaccum sensitive stove：
The filamentary silver of the cathode copper and Ag purity 99.99wt% that use Cu purity 99.99wt% is remaining according to 2wt%Ag for raw material
Amount is copper and inevitable impurity this proportioning, and the high-purity of intermediate frequency vaccum sensitive stove is added in the cathode copper, the filamentary silver
In graphite crucible, it is evacuated to vacuum meter reading and reaches 10-1Pa and after stablizing, is gradually heating to 1250 DEG C, waits for that aluminium alloy starts
It is strong to splash, stand 20-30 minutes；Then it is cast into the Kufil blank of Φ=50mm under vacuum conditions；
（1-2）Kufil bar is continuously prepared using antivacuum casting furnace：
Antivacuum casting furnace is gradually heating to 1250-1260 DEG C with the heating rate of 90 DEG C/h, opens high purity graphite earthenware
Blowning installation in crucible, by high pure nitrogen（99.999% or more）Flow is adjusted to 1 liter/min；Gradually to the high purity graphite crucible
Kufil blank is added in melt chamber, after molten bath is formed, covers graphite flakes on melt chamber, incubation cavity, casting cavity, covers
Lid thickness is 30mm；Then it is continuously added to Kufil blank, after aluminium alloy reaches crucible safe capacity, keeps the temperature 50 minutes,
Scarfing cinder；Then, horizontal casting is continuously being cast at the Kufil bar of Φ=12.5mm, casting speed 650mm/min, pitch 5mm
While making, continuously fed in time into melt chamber according to alloy liquid level and temperature；
（2）The Kufil bar of above-mentioned Φ=12.5mm is further rolled into the Kufil of Φ=8mm through three-high mill
Rolled bar, wherein use arc triangle-round pass system, passage mean coefficient of elongation 1.20, mill speed 60m/min；
（3）The Kufil rolled bar of above-mentioned Φ=8mm is drawn greatly with the draw rate of 50m/min, be drawn into Φ=
The Kufil thick line of 3mm；
（4）Intermediate heat-treatment is carried out to the Kufil thick line：
The Kufil thick line of above-mentioned Φ=3mm is put into forvacuum to the nitrogen protection annealing furnace of -0.1MPa, and
It is filled with high pure nitrogen thereto, until pressure is 0.02MPa in the flue of the nitrogen protection annealing furnace, then heats up 1 hour
To 420 DEG C, 6 hours are kept the temperature, is finally air-cooled to room temperature with stove；
（5）By the Kufil thick line Jing Guo intermediate heat-treatment first be pulled in the draw rate of 500m/min Φ=
0.9mm, passage draft 15%；Again Φ=0.16mm, passage draft 13% are pulled to so that the draw rate of 1000m/min is small；Finally
The mm of Φ=0.025 are carefully pulled to the draw rate of 1500m/min, passage draft 7% obtains the Kufil superfine wire.
Comparative example 2
Prepare Kufil superfine wire：
（1）Founding Kufil bar, including：
（1-1）Kufil blank is prepared using vaccum sensitive stove：
The filamentary silver of the cathode copper and Ag purity 99.99wt% that use Cu purity 99.99wt% is raw material；It is remaining according to 4wt%Ag
Amount is copper and inevitable impurity this proportioning, and the high-purity of intermediate frequency vaccum sensitive stove is added in the cathode copper, the filamentary silver
In graphite crucible, it is evacuated to vacuum meter reading and reaches 10-1Pa and after stablizing, is gradually heating to 1250 DEG C, waits for that aluminium alloy starts
It is strong to splash, stand 20-30 minutes；Then the Kufil blank of Φ=50mm is cast into graphite casting mould under vacuum conditions；
（1-2）Kufil bar is continuously prepared using antivacuum casting furnace：
Antivacuum casting furnace is gradually heating to 1260-1270 DEG C with the heating rate of 120 DEG C/h, opens high purity graphite earthenware
Blowning installation in crucible, by high-purity argon gas（99.999% or more）Flow is adjusted to 1.5 liters/min；Gradually to the high purity graphite earthenware
Kufil blank is added in crucible melt chamber, after molten bath is formed, graphite flakes are covered on melt chamber, incubation cavity, casting cavity,
Cladding thickness is 30mm；Then it is continuously added to Kufil blank, after aluminium alloy reaches crucible safe capacity, keeps the temperature 50 points
Clock, scarfing cinder；Then, continuous up-casting is continuously being cast at the Kufil bar of Φ=16mm, casting speed 550mm/min, pitch 4mm
While making, continuously fed in time into melt chamber according to alloy liquid level and temperature；
（2）The Kufil that the Kufil bar of above-mentioned Φ=16mm is further rolled into Φ=8mm through two-roller mill rolls
Bar processed, wherein use ellipse-circular hole system, passage mean coefficient of elongation 1.20, mill speed 80m/min；
（3）The Kufil rolled bar of above-mentioned Φ=8mm is drawn greatly with the draw rate of 100m/min, be drawn into Φ=
The Kufil thick line of 2.6mm；
（4）Intermediate heat-treatment is carried out to the Kufil thick line：
The Kufil thick line of above-mentioned Φ=2.6mm is put into forvacuum to the argon gas protection annealing furnace of -0.1MPa,
And it is filled with high-purity argon gas thereto, until pressure is 0.02MPa in the flue of argon gas protection annealing furnace, then heating 1 is small
Up to 450 DEG C, 7 hours are kept the temperature, is finally air-cooled to room temperature with stove；
（5）By the Kufil thick line Jing Guo intermediate heat-treatment first be pulled in the draw rate of 500m/min Φ=
1.2mm, passage draft 15%；Again Φ=0.20mm, passage draft 13% are pulled to so that the draw rate of 1000m/min is small；Finally
The mm of Φ=0.03 are carefully pulled to the draw rate of 1500m/min, passage draft 7% obtains the Kufil superfine wire.
Comparative example 3
Prepare Kufil superfine wire：
（1）Founding Kufil bar, including：
（1-1）Kufil blank is prepared using vaccum sensitive stove：
The filamentary silver of the cathode copper and Ag purity 99.99wt% that use Cu purity 99.99wt% is raw material；It is remaining according to 6wt%Ag
Amount is copper and inevitable impurity this proportioning, and the high-purity of intermediate frequency vaccum sensitive stove is added in the cathode copper, the filamentary silver
In graphite crucible, it is evacuated to vacuum meter reading and reaches 10-1Pa and after stablizing, is gradually heating to 1300 DEG C, waits for that aluminium alloy starts
It is strong to splash, stand 20-30 minutes；Then the Kufil blank of Φ=50mm is cast into graphite casting mould under vacuum conditions；
（1-2）Kufil bar is continuously prepared using antivacuum casting furnace：
Antivacuum casting furnace is gradually heating to 1270-1280 DEG C with the heating rate of 150 DEG C/h, opens high purity graphite earthenware
Blowning installation in crucible, by high-purity argon gas（99.999% or more）Flow is adjusted to 2 liters/min；Gradually to the high purity graphite crucible
Kufil blank is added in melt chamber, after molten bath is formed, covers graphite flakes on melt chamber, incubation cavity, casting cavity, covers
Lid thickness is 30mm；Then it is continuously added to Kufil blank, after aluminium alloy reaches crucible safe capacity, keeps the temperature 50 minutes,
Scarfing cinder；Then, continuous up-casting is at the Kufil bar of Φ=20mm, casting speed 450mm/min, pitch 3mm, in continuously casting
While, it is continuously fed in time into melt chamber according to alloy liquid level and temperature；
（2）The Kufil that the Kufil bar of above-mentioned Φ=20mm is further rolled into Φ=8mm through two-roller mill rolls
Bar processed, wherein use ellipse-circular hole system, passage mean coefficient of elongation 1.20, mill speed 100m/min；
（3）The Kufil rolled bar of above-mentioned Φ=8mm is drawn greatly with the draw rate of 150m/min, be drawn into Φ=
The Kufil thick line of 2.8mm；
（4）Intermediate heat-treatment is carried out to the Kufil thick line：
The Kufil thick line of above-mentioned Φ=2.8mm is put into forvacuum to the nitrogen protection annealing furnace of -0.1MPa,
And it is filled with high pure nitrogen thereto, until pressure is 0.02MPa in the flue of the nitrogen protection annealing furnace, then heating 1 is small
Up to 480 DEG C, 8 hours are kept the temperature, is finally air-cooled to room temperature with stove；
（5）By the Kufil thick line Jing Guo intermediate heat-treatment first be pulled in the draw rate of 700m/min Φ=
1.2mm, passage draft 20%；Again Φ=0.25mm, passage draft 12% are pulled to so that the draw rate of 900m/min is small；Finally
The mm of Φ=0.04 are carefully pulled to the draw rate of 1300m/min, passage draft 8% obtains the Kufil superfine wire.
In addition, inventor has carried out phase respectively to above example 1 ~ 3 and alloy superfine wire obtained in comparative example 1 ~ 3
Detection is closed, has predominantly detected tensile strength, elongation at break, conductivity, oxygen content this 4 indexs, as a result as shown in table 1 below：
By comparing the data in upper table 1 it is found that using alloy superfine wire and comparative example made from the embodiment of the present invention 1 ~ 3
Alloy superfine wire made from 1 ~ 3 is compared, and causes oxygen content to significantly reduce due to the addition of rare earth element, to higher
The elongation at break of tensile strength and bigger；In other words, provided by the present invention in the case where superfine wire has same diameter Φ
Copper silver rare-earth alloy superfine wire tensile strength bigger, draw more difficult broken string, thus comprehensive performance is more preferable.
Specific embodiments of the present invention are described in detail above, but it is intended only as example, the present invention is simultaneously unlimited
It is formed on particular embodiments described above.To those skilled in the art, it is any to the equivalent modifications that carry out of the present invention and
It substitutes also all among scope of the invention.Therefore, without departing from the spirit and scope of the invention made by impartial conversion and
Modification, all should be contained within the scope of the invention.
Claims (6)
1. a kind of method producing copper silver rare-earth alloy superfine wire, which is characterized in that include the following steps：
(1) founding copper silver rare-earth alloy bar, including：
(1-1) prepares pure copper silver rare-earth alloy blank using vaccum sensitive stove；
(1-2) uses resistance heating high purity graphite crucible, the high purity graphite crucible to be provided with blowning installation, and by 3 chambers
Composition, respectively melt chamber, incubation cavity and casting cavity, are connected between chamber and chamber by bottom undercurrent hole；By antivacuum casting furnace
It is gradually heating to 1250-1300 DEG C, opens the blowning installation, high pure nitrogen or argon flow amount are adjusted to 1-2 liters/min；By
Gradually to copper silver rare-earth alloy blank is added in the high purity graphite crucible melting chamber, after molten bath is formed, melt chamber, incubation cavity,
Graphite flakes are covered on casting cavity；Then continuous charging is carried out, after aluminium alloy reaches crucible safe capacity, keeps the temperature 40-60
Minute, scarfing cinder；Then, the copper silver rare-earth alloy bar of continuously casting Φ=12.5-20mm, casting speed 400-800mm/min, section
Away from 3-5mm, while continuously casting, continuously fed into melt chamber according to alloy liquid level and temperature；
(2) copper silver rare-earth alloy bar made from three rollers or the further milling step of two-roller mill (1) is used, the conjunction of copper silver rare earth is obtained
Golden rolled bar；
(3) the copper silver rare-earth alloy rolled bar is drawn greatly, is drawn into copper silver rare-earth alloy thick line；
(4) intermediate heat-treatment is carried out to the copper silver rare-earth alloy thick line；
(5) the copper silver rare-earth alloy thick line Jing Guo intermediate heat-treatment is subjected to finish draw, finally obtained copper silver rare-earth alloy superfine wire；
The copper silver rare-earth alloy superfine wire includes following component：
1~25wt% silver, 0.01~0.04wt% yttriums, surplus are copper and inevitable impurity；Or 1~25wt% silver,
0.10~0.30wt% lanthanums, surplus are copper and inevitable impurity；Or 1~25wt% silver, 0.01~0.02wt% yttriums,
0.05~0.15wt% lanthanums, surplus are copper and inevitable impurity.
2. according to the method described in claim 1, it is characterized in that, step (1-1) includes：
Copper, silver, rare earth are proportionally added into the high purity graphite crucible of the vaccum sensitive stove, vacuum meter reading is evacuated to and reaches
To 10-1Pa and after stablizing, is gradually heating to 1200-1300 DEG C, waits for that aluminium alloy starts to splash strongly, stand 20-30 minutes, then
It is cast into copper silver rare-earth alloy blank under vacuum conditions.
3. according to the method described in claim 1, it is characterized in that, in step (2)：Using arc triangle-circle or ellipse-circular hole
Type system, passage mean coefficient of elongation 1.15-1.25, mill speed 10-120m/min.
4. according to the method described in claim 1, it is characterized in that, step (3) in using 50-300m/min draw rate,
It is drawn into the copper silver rare-earth alloy thick line of Φ=2.6-3mm.
5. according to the method described in claim 1, it is characterized in that, step (4) includes：
By the copper silver rare-earth alloy thick line be put into forvacuum to -0.1MPa inert gas shielding annealing furnace in, and to its
In be filled with high pure nitrogen or argon gas, until the inert gas shielding annealing furnace flue in pressure be 0.02~0.05MPa, connect
It and is warming up to 420-520 DEG C, keep the temperature 6-8 hours, be finally air-cooled to room temperature with stove.
6. according to the method described in claim 1, it is characterized in that, step (5) includes：
By the copper silver rare-earth alloy thick line Jing Guo intermediate heat-treatment first be pulled in the draw rate of 400-800m/min Φ=
0.8-1.2mm, passage draft 15-20%；It is pulled to Φ=0.15-0.25mm so that the draw rate of 500-1000m/min is small again,
Passage draft 8-13%；Φ=0.025-0.05mm is carefully finally pulled to the draw rate of 800-1500m/min, passage subtracts face
Rate 7-10% obtains the copper silver rare-earth alloy superfine wire.
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| CN114561566B (en) * | 2022-03-03 | 2022-09-20 | 江西理工大学 | Preparation method of copper-silver alloy wire |
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| CN115478185A (en) * | 2022-09-26 | 2022-12-16 | 江苏亨通电力智网科技有限公司 | Copper-tin alloy superfine wire and preparation method thereof |
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