CN104630512B - Dispersion type copper-bismuth-tin immiscible alloy composite wire rod and preparation method thereof - Google Patents
Dispersion type copper-bismuth-tin immiscible alloy composite wire rod and preparation method thereof Download PDFInfo
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- CN104630512B CN104630512B CN201310553970.XA CN201310553970A CN104630512B CN 104630512 B CN104630512 B CN 104630512B CN 201310553970 A CN201310553970 A CN 201310553970A CN 104630512 B CN104630512 B CN 104630512B
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 76
- 239000000956 alloy Substances 0.000 title claims abstract description 76
- 239000002131 composite material Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000006185 dispersion Substances 0.000 title claims abstract description 6
- ZWFRZGJUJSOHGL-UHFFFAOYSA-N [Bi].[Cu].[Sn] Chemical compound [Bi].[Cu].[Sn] ZWFRZGJUJSOHGL-UHFFFAOYSA-N 0.000 title abstract description 5
- 238000007711 solidification Methods 0.000 claims abstract description 46
- 230000008023 solidification Effects 0.000 claims abstract description 46
- 229910016338 Bi—Sn Inorganic materials 0.000 claims abstract description 33
- 230000000694 effects Effects 0.000 claims abstract description 23
- 239000011159 matrix material Substances 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 15
- 229910052718 tin Inorganic materials 0.000 claims abstract description 15
- 229910052802 copper Inorganic materials 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims description 18
- 239000010949 copper Substances 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 15
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 9
- QAAXRTPGRLVPFH-UHFFFAOYSA-N [Bi].[Cu] Chemical compound [Bi].[Cu] QAAXRTPGRLVPFH-UHFFFAOYSA-N 0.000 claims description 9
- 229910052593 corundum Inorganic materials 0.000 claims description 3
- 239000010431 corundum Substances 0.000 claims description 3
- 229910001152 Bi alloy Inorganic materials 0.000 claims description 2
- 229910052797 bismuth Inorganic materials 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims description 2
- 229910001128 Sn alloy Inorganic materials 0.000 abstract description 17
- 230000006911 nucleation Effects 0.000 abstract description 13
- 238000010899 nucleation Methods 0.000 abstract description 13
- 238000005204 segregation Methods 0.000 abstract description 3
- 239000012071 phase Substances 0.000 abstract 4
- 239000007791 liquid phase Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 230000008018 melting Effects 0.000 description 6
- 238000002844 melting Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 238000000354 decomposition reaction Methods 0.000 description 4
- 230000006798 recombination Effects 0.000 description 4
- 238000005215 recombination Methods 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000015271 coagulation Effects 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005275 alloying Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000013517 stratification Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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Abstract
The present invention discloses a dispersion type copper-bismuth-tin immiscible alloy composite wire rod and a preparation method thereof, and belongs to the technical field of alloy composite materials and preparation thereof. The dispersion type copper-bismuth-tin immiscible alloy composite wire rod is characterized in that a Cu-Bi-Sn immiscible alloy is adopted as a raw material, and a continuous solidification technology under a pulse current effect is adopted to prepare the copper-bismuth-tin immiscible alloy composite wire rod with the dispersed phase uniformly distributed in the matrix, wherein the solidification rate is 8-20 mm/s. According to the present invention, the continuous solidification technology under the pulse current effect is adopted, the nucleation rate of the rich (Cu, Sn) phase (hereinafter referred as: dispersed phase) during the liquid-liquid phase change process of the (10-15)wt% Cu-(75-80)wt% Bi-10wt% Sn alloy is increased, the phase segregation is inhibited, and the dispersion type Cu-Bi-Sn alloy composite material is prepared.
Description
Technical field
The invention belongs to alloy wire preparing technical field is and in particular to a kind of diffusion-type Cu-Bi-Sn immiscible alloy is multiple
Zygonema material and preparation method thereof.
Background technology
Cu-Bi-Sn immiscible alloy composite wire has a wide range of applications in fields such as welding, catalysis and machineries.
It is very necessary for therefore developing a kind of diffusion-type copper bismuth tin alloy composite wire and its technology of preparing, has great market price
Value.But there is liquid-liquid decomposition process during the cooling of such alloy melt, easily form gravity segregation when solidifying in gravitational field tight
The tissue of weight, its preparation and application is restricted.
Content of the invention
It is an object of the invention to provide a kind of diffusion-type copper bismuth stannum immiscible alloy composite wire and preparation method thereof, carry
Go out by suitably choosing alloying component and crystallizer inner lining material, carry out continuous solidification under pulse current effect, make alloy
During liquid-liquid decomposition, the nucleation rate of disperse phase drop increases, and weakens and eliminate the phase segregation phenomenon in process of setting, obtains more
Dephasing is uniformly distributed in the copper bismuth stannum immiscible alloy composite wire of matrix.
The technical scheme is that：
A kind of preparation method of diffusion-type copper bismuth stannum immiscible alloy composite wire, the method is miscible with Cu-Bi-Sn difficulty
Alloy is raw material, prepares disperse phase using the continuous solidification technology under pulse current effect and is uniformly distributed in the copper bismuth in matrix
Stannum immiscible alloy composite wire；Wherein：Setting rate is 8-20mm/s.
Continuous solidification technology under the described effect using pulse current refers to：In preparation process, alloy melt is applied along knot
The pulse current of brilliant device axial direction, the inner lining material of adopted continuous solidification its crystallizer of device is corundum simultaneously, crystallizer
Internal diameter 5-15mm.The peak current density of described pulse current is（1～3）×104A/cm2, pulse width is 4～6 μ s, pulse
Frequency is 20～50Hz.
In the chemical composition of described Cu-Bi-Sn alloy raw material：Cu (10-15) wt%, Sn10wt%, Bi are surplus.
The preparation method of diffusion-type Cu-Bi-Sn alloy composite wire of the present invention specifically includes following steps：
1）Described Cu-Bi-Sn immiscible alloy raw material is heated fusing, forms uniform alloy melt；
2）Under pulse current effect, continuous solidification is carried out to alloy melt, obtain diffusion-type Cu-Bi-Sn alloy recombination line
Material.
In the diffusion-type Cu-Bi-Sn alloy composite wire being obtained using said method, rich（Cu, Sn）Phase particle dispersion
It is distributed in rich Bi alloy substrate.
The principle of the present invention is as follows：
During the lower solidification of pulse current effect, rich during Cu-Bi-Sn immiscible alloy liquid-liquid decomposition（Cu, Sn）Phase drop
Nucleation rate increases, mean radiuss reduce, and drop is equal along the Stokes movement velocity of crystallizer axial direction and Marangoni movement velocity
Reduce, promote the acquisition of diffusion-type Cu-Bi-Sn immiscible alloy composite wire.
Brief description
Fig. 1 is the continuous solidification device with impulse current generator.
In figure：1- wire；2- graphite electrode；3- crucible；4- resistive heater；5- alloy melt；6- pulse generating units；
7- crystallizer；8- water cooler；9- alloy bar；10- conduction slide plate；11- lifting rod.
Fig. 2 is not apply during pulse current 15wt%Cu-75wt%Bi-10wt%Sn alloy with 10mm/s speed continuous solidification
Tissue afterwards.
Fig. 3 be apply pulse current when 15wt%Cu-75wt%Bi-10wt%Sn alloy with 10mm/s speed continuous solidification after
Tissue（Peak current density is：30000A/cm2, pulse frequency is 50Hz, and pulse width is 6 μ s）.
Fig. 4 is not apply after during pulse current, 10wt%Cu-80wt%Bi-10wt%Sn alloy is with 8mm/s speed continuous solidification
Tissue.
Fig. 5 be apply pulse current when 10wt%Cu-80wt%Bi-10wt%Sn alloy with 8mm/s speed continuous solidification after
Tissue（Peak current density is：20000A/cm2, pulse frequency is 50Hz, and pulse width is 6 μ s）.
Fig. 6 is not apply during pulse current 10wt%Cu-80wt%Bi-10wt%Sn alloy with 10mm/s speed continuous solidification
The tissue of sample afterwards.
Fig. 7 be apply pulse current when 10wt%Cu-80wt%Bi-10wt%Sn alloy with 10mm/s speed continuous solidification after
Tissue（Peak current density is：10000A/cm2, pulse frequency is 50Hz, and pulse width is 6 μ s）.
Fig. 8 be apply pulse current when 10wt%Cu-80wt%Bi-10wt%Sn alloy with 10mm/s speed continuous solidification after
The tissue of sample（Peak current density is：30000A/cm2, pulse frequency is 50Hz, and pulse width is 4 μ s）.
Fig. 9 be apply pulse current when 10wt%Cu-80wt%Bi-10wt%Sn alloy with 10mm/s speed continuous solidification after
The tissue of sample（Peak current density is：30000A/cm2, pulse frequency is 50Hz, and pulse width is 6 μ s）.
Figure 10 for peak current density is：30000A/cm2, pulse width is 6 μ s, when pulse frequency is 20Hz, 10wt%
Cu-80wt%Bi-10wt%Sn alloy is with the tissue of sample after 10mm/s speed continuous solidification.
Specific embodiment
Research shows, under the conditions of continuous solidification, Cu-Bi-Sn immiscible alloy is rich during liquid-liquid decomposition（Cu,
Sn）Drop nucleation rate is relatively low, typically results in that disperse phase drop is thick, the formation of skewness or even two phase stratification tissue, such as
Shown in Fig. 2, Fig. 4 and Fig. 6.
When melt is passed to the pulse current along crystallizer axial direction, disperse phase drop nucleation rate increases, and can be formed
Diffusion-type composite wire.Accordingly, the present invention passes through from Cu-Bi-Sn immiscible alloy, using continuous under pulse current effect
Solidification technology, is prepared for diffusion-type composite wire, as shown in Fig. 3, Fig. 5, Fig. 7, Fig. 8 and Fig. 9.
Coagulation system used in following examples is as shown in figure 1, this device is on the basis of conventional continuous solidification device
Increase pulse generating units 6 so as to pulse current can be applied to alloy melt 5, the liner of crystallizer 7 adopts corundum simultaneously
Material, crystallizer 7 internal diameter 5-15mm.Concrete structure is：This coagulation system includes crucible 3 for fusing metal, is used for solidifying
The crystallizer 7 of alloy melt 5 and pulse generating units 6；Wherein：By resistive heater 4, described crucible 3 is heated, pass through
Water cooler 8 cools down to described crystallizer 7, so that alloy melt 5 solidifies, water cooler 8 lower section setting traction alloy bar（Wire rod）9
Lifting rod 11.Described pulse generating units 6 one outfan connects one end of graphite electrode 2, described graphite by wire 1
The other end of electrode 2 stretches in the alloy melt 5 in crucible 3.Its another outfan of described pulse generating units 6 passes through conduction
Slide plate 10 is connected with alloy bar 9, thus realizing applying pulse current to alloy melt 5.
Embodiment 1
From 15wt%Cu-75wt%Bi-10wt%Sn alloy, using the continuous solidification device under pulse current effect, with firm
The beautiful inner lining material for crystallizer, setting rate is 10mm/s, is 30000A/cm2 by the peak current density of melt, pulse
Frequency is 50Hz, and pulse width is 6 μ s.Prepare diffusion-type Cu-Bi-Sn alloy composite wire, its a diameter of 8mm.
Its preparation process is as follows：
With resistance furnace melting Cu-Bi-Sn alloy, obtain homogeneous melt by being incubated in 1173K, stirring after 40 minutes；Make
Melt is in pulse current（Peak current density is 30000A/cm2, and pulse frequency is 50Hz, and pulse width is 6 μ s）Connect under effect
Continuous solidification.
As shown in figure 3, in figure white phase is rich Bi matrix, black phase is richness to the present embodiment gained alloy composite wire（Cu,
Sn）Phase.In process of setting, pulse current promotes disperse phase drop nucleation rate to increase, and in solidified structure, disperse phase size is tiny and equal
Even distribution.
Comparative example 1
Difference from Example 1 is：Pulse current is not applied to alloy melt.Gained Cu-Bi-Sn alloy recombination line
Material tissue is as shown in Figure 2.In Fig. 2, white phase is rich Bi matrix, and black phase is richness（Cu, Sn）Phase, disperse phase liquid in process of setting
Drip nucleation rate relatively low, in solidified structure disperse phase size is thick and uneven distribution.
Experiment shows, in embodiment 1 solidification sample, disperse phase particle size is thin during pulse current compared with not applying in comparative example 1
Little, and uniform particle is distributed in matrix.
Embodiment 2
From 10wt%Cu-80wt%Bi-10wt%Sn alloy, using the continuous solidification device under pulse current effect, with firm
The beautiful inner lining material for crystallizer, setting rate is 8mm/s, is 20000A/cm2 by the peak current density of melt, pulse
Frequency is 50Hz, and pulse width is 6 μ s.Prepare diffusion-type Cu-Bi-Sn alloy composite wire, its a diameter of 8mm.
Its preparation process is as follows：
With resistance furnace melting Cu-Bi-Sn alloy, obtain homogeneous melt by being incubated in 1173K, stirring after 40 minutes；Make
Melt is in pulse current（Peak current density is 20000A/cm2, and pulse frequency is 50Hz, and pulse width is 6 μ s）Connect under effect
Continuous solidification.
As shown in figure 5, in figure white phase is rich Bi matrix, black phase is richness to the present embodiment gained alloy composite wire（Cu,
Sn）Phase.In process of setting, pulse current promotes disperse phase drop nucleation rate to increase, and alloy assumes diffusion-type solidified structure.
Comparative example 2
Difference from Example 2 is：Pulse current is not applied to alloy melt.Gained Cu-Bi-Sn alloy recombination line
Material is organized as shown in figure 4, white phase is rich Bi matrix in Fig. 4, and black phase is richness（Cu, Sn）Phase, alloy assumes two-phase laminated flow and coagulates
Gu tissue.
Experiment shows, in embodiment 2 solidification sample, disperse phase particle size is thin during pulse current compared with not applying in comparative example 2
Little, and uniform particle is distributed in matrix.
Embodiment 3
From 10wt%Cu-80wt%Bi-10wt%Sn alloy, using the continuous solidification device under pulse current effect, with firm
The beautiful inner lining material for crystallizer, setting rate is 10mm/s, is 10000A/cm2 by the peak current density of melt, pulse
Frequency is 50Hz, and pulse width is 6 μ s.Prepare diffusion-type Cu-Bi-Sn alloy composite wire, its a diameter of 8mm.
Its preparation process is as follows：
With resistance furnace melting Cu-Bi-Sn alloy, obtain homogeneous melt by being incubated in 1173K, stirring after 40 minutes；Make
Melt is in pulse current（Peak current density is 10000A/cm2, and pulse frequency is 50Hz, and pulse width is 6 μ s）Connect under effect
Continuous solidification.
As shown in fig. 7, in figure white phase is rich Bi matrix, black phase is richness to the present embodiment gained alloy composite wire（Cu,
Sn）Phase.In process of setting, pulse current promotes disperse phase drop nucleation rate to increase, disperse phase particle size in Solidification Structure
Tiny and be uniformly distributed in matrix.
Comparative example 3
Difference from Example 3 is：Pulse current is not applied to alloy melt.Gained Cu-Bi-Sn alloy recombination line
Material is organized as shown in fig. 6, white phase is rich Bi matrix in Fig. 6, and black phase is richness（Cu, Sn）Phase.Disperse phase liquid in process of setting
Drip nucleation rate relatively low, in Solidification Structure disperse phase size is more thick and skewness in the base.
Experiment shows, in embodiment 3 solidification sample, disperse phase particle size is thin during pulse current compared with not applying in comparative example 3
Little, and uniform particle is distributed in matrix.
Embodiment 4
From 10wt%Cu-80wt%Bi-10wt%Sn alloy, using the continuous solidification device under pulse current effect, with firm
The beautiful inner lining material for crystallizer, setting rate is 10mm/s, is 30000A/cm2 by the peak current density of melt, pulse
Frequency is 50Hz, and pulse width is 4 μ s.Prepare diffusion-type Cu-Bi-Sn alloy composite wire, its a diameter of 8mm.
Its preparation process is as follows：
With resistance furnace melting Cu-Bi-Sn alloy, obtain homogeneous melt by being incubated in 1173K, stirring after 40 minutes；Make
Melt is in pulse current（Peak current density is 30000A/cm2, and pulse frequency is 50Hz, and pulse width is 4 μ s）Connect under effect
Continuous solidification.
As shown in figure 8, in figure white phase is rich Bi matrix, black phase is richness to the present embodiment gained alloy composite wire（Cu,
Sn）Phase.In process of setting, pulse current leads to disperse phase drop nucleation rate to increase, disperse phase particle size in Solidification Structure
Tiny and be uniformly distributed with matrix in.
Experiment shows, in sample disperse phase particle size do not apply (Fig. 6) during pulse current tiny, uniform particle be distributed
In matrix.
Embodiment 5
From 10wt%Cu-80wt%Bi-10wt%Sn alloy, using the continuous solidification device under pulse current effect, with firm
The beautiful inner lining material for crystallizer, setting rate is 10mm/s, is 30000A/cm2 by the peak current density of melt, pulse
Frequency is 50Hz, and pulse width is 6 μ s.Prepare diffusion-type Cu-Bi-Sn alloy composite wire, its a diameter of 8mm.
Its preparation process is as follows：
With resistance furnace melting Cu-Bi-Sn alloy, obtain homogeneous melt by being incubated in 1173K, stirring after 40 minutes；Make
Melt is in pulse current（Peak current density is 30000A/cm2, and pulse frequency is 50Hz, and pulse width is 6 μ s）Connect under effect
Continuous solidification.
As shown in figure 9, in figure white phase is rich Bi matrix, black phase is richness to the present embodiment gained alloy composite wire（Cu,
Sn）Phase.In process of setting, pulse current leads to disperse phase drop nucleation rate to increase, disperse phase particle size in Solidification Structure
Tiny and be uniformly distributed with matrix in.
Experiment shows, in sample disperse phase particle size do not apply (Fig. 6) during pulse current more tiny, uniform particle
It is distributed in matrix.
Embodiment 6
From 10wt%Cu-80wt%Bi-10wt%Sn alloy, using the continuous solidification device under pulse current effect, with firm
The beautiful inner lining material for crystallizer, setting rate is 10mm/s, is 30000A/cm2 by the peak current density of melt, pulse
Frequency is 20Hz, and pulse width is 6 μ s.Prepare diffusion-type Cu-Bi-Sn alloy composite wire, its a diameter of 8mm.
Its preparation process is as follows：
With resistance furnace melting Cu-Bi-Sn alloy, obtain homogeneous melt by being incubated in 1173K, stirring after 40 minutes；Make
Melt is in pulse current（Peak current density is 30000A/cm2, and pulse frequency is 20Hz, and pulse width is 6 μ s）Connect under effect
Continuous solidification.
As shown in Figure 10, in figure white phase is rich Bi matrix to the present embodiment gained alloy composite wire, and black phase is richness
（Cu, Sn）Phase.In process of setting, pulse current leads to disperse phase drop nucleation rate to increase, disperse phase particle in Solidification Structure
Size tiny and be uniformly distributed with matrix in.
Experiment shows, in sample disperse phase particle size do not apply (Fig. 6) during pulse current tiny, uniform particle be distributed
In matrix.
Claims (3)
1. a kind of preparation method of diffusion-type copper bismuth stannum immiscible alloy composite wire it is characterised in that：The method is with Cu-
Bi-Sn immiscible alloy is raw material, prepares disperse phase using the continuous solidification technology under pulse current effect and is uniformly distributed in
Copper bismuth stannum immiscible alloy composite wire in matrix；Wherein：Setting rate is 8-20mm/s；Weight percentage, institute
State in the chemical composition of Cu-Bi-Sn immiscible alloy raw material：Cu is 10-15%, and Sn is 10%, Bi is surplus；
Continuous solidification technology under the described effect using pulse current refers in preparation process, alloy melt be applied along crystallizer
The pulse current of axial direction, the inner lining material of adopted continuous solidification its crystallizer of device is corundum simultaneously, crystallizer internal diameter
5-15mm；
The peak current density of described pulse current is (1～3) × 104A/cm2, pulse width is 4～6 μ s, and pulse frequency is 20
～50Hz.
2. diffusion-type copper bismuth stannum immiscible alloy composite wire according to claim 1 preparation method it is characterised in that：
The preparation method of described composite wire specifically includes following steps：
1) described Cu-Bi-Sn immiscible alloy raw material is heated fusing, form uniform alloy melt；
2) under pulse current effect, continuous solidification is carried out to alloy melt, obtain diffusion-type Cu-Bi-Sn alloy composite wire.
3. a kind of diffusion-type copper bismuth stannum immiscible alloy composite wire of utilization claim 1 methods described preparation, its feature exists
In：In described composite wire, rich (Cu, Sn) phase particle dispersion is distributed in rich Bi alloy substrate.
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| CN114178499A (en) * | 2021-11-18 | 2022-03-15 | 上海大学 | Continuous preparation method and device for homogeneous immiscible alloy material |
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| CN101348875A (en) * | 2008-06-04 | 2009-01-21 | 厦门市及时雨焊料有限公司 | Tin, bismuth and copper type low temperature lead-free solder alloy |
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