CN106676313A - Preparation method of high-intensity and high-conductivity Cu-Nb alloy billet - Google Patents
Preparation method of high-intensity and high-conductivity Cu-Nb alloy billet Download PDFInfo
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- CN106676313A CN106676313A CN201611237171.1A CN201611237171A CN106676313A CN 106676313 A CN106676313 A CN 106676313A CN 201611237171 A CN201611237171 A CN 201611237171A CN 106676313 A CN106676313 A CN 106676313A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D17/00—Pressure die casting or injection die casting, i.e. casting in which the metal is forced into a mould under high pressure
- B22D17/007—Semi-solid pressure die casting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D27/00—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
- B22D27/04—Influencing the temperature of the metal, e.g. by heating or cooling the mould
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/12—Making non-ferrous alloys by processing in a semi-solid state, e.g. holding the alloy in the solid-liquid phase
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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
Abstract
The invention discloses a preparation method of a high-intensity and high-conductivity Cu-Nb alloy billet, and belongs to the technical field of preparation of copper microcomposites. The high-intensity and high-conductivity Cu-Nb alloy is Cu-Nb binary alloy; 80-98wt% of pure copper ingot, 1-17wt% of pure niobium ingot, and 1-3wt% of pure niobium powder are used as the raw materials; a solid-liquid double-phase solidifying and semi-solid casting combined technology is adopted; the pure niobium powder is added to an alloy melt, and an Nb-enriched solid solution can be formed in the rapid solidifying process; the Nb-enriched solid solution is treated through drawing and rolling technologies to prepare the Cu-Nb alloy billet of which the micro structure is refined to the nanometer level, so that the foundation is provided for the micro structure refining technology. The tensile strength of the Cu-Nb alloy billet is 1300-1700MPa; the conductivity is more than 75% IACS; the grain size is 1-30 microns. Therefore, the preparation efficiency of an alloy wire and a thin belt material can be greatly improved. The application field of such material is greatly expanded.
Description
Technical field
The invention belongs to copper microcomposite preparing technical field.More particularly to a kind of high-strength high-conductivity Cu-
The preparation method of Nb alloy blanks.
Background technology
High-strength highly-conductive acid bronze alloy is the structure function material that a class has excellent comprehensive performance, be widely used in electric power,
The industrial circles such as electronics, metallurgy, machinery.The development of modern science and technology proposes one to the combination property of conductive copper-based material
The requirement of Lie Genggao：Large-scale integrated circuit lead frame requires that the tensile strength of material is higher than 600MPa, and conductivity is higher than
80%IACS, with electric railway at a high speed, heavily loaded direction develop, the intensity of contact line/aerial line is proposed higher
Require, require contact line tensile strength higher than 530MPa, conductivity more than 78%IACS when train speed per hour is 350km/h
(International Annealed Copper Standard International Annealed Copper Standards), builds the pulsed magnetic of a 100T
, it is desirable to the intensity of coil method is higher than 1500MPa, and conductivity is higher than 60%IACS.Therefore, high-intensity high-conductivity copper based alloy
Material becomes one of study hotspot in recent years.
Copper microcomposite with Cu-Nb, Cu-Ag as representative has higher conductivity and tensile strength, by magnet
Expert is unanimously considered the conductor material for most possibly realizing 100T impulse magnetic fields.Cu-Nb microcosmic prepared by clustered drawing
Intensity level of the superhigh intensity that composite is obtained significantly larger than as obtained by mixing principle is calculated, and the solid solution due to Nb in Cu
Degree is extremely low, and the elastic performance of Cu and Nb is sufficiently close to, so being also possible to obtain high electric conductivity and toughness, therefore Cu-Nb microcosmic
Composite will become the research emphasis of impulse magnetic field conductor material.
, used as high-intensity magnetic field application material, (high-intensity magnetic field, superhigh temperature are heavily stressed for its harsh applied environment for Cu-Nb composites
Deng) require that material has the good combination of the performances such as intensity and conductive and heat-conductive.Existing research shows, receives when organizational structure reaches
Meter ruler cun, Cu-Nb composites can obtain high strength ＆ high electric-conduction.But further reduce size, due to Interface Motion deformation
Mechanism is started, and material is likely to occur ruckbildung, now the heat stability faced blocks material at Cu-Nb interfaces is weaker, intensity
Also may decline.It is also imperfect to the reinforcing of this whole process and the understanding of softening mechanism at present.Therefore improve under nanoscale
The stability at Cu-Nb interfaces, it is that following Cu-Nb composites research field is urgently to be resolved hurrily to analyse in depth research material strengthening mechanism
One of problem.In practical application area, certain domestic high power pulse laboratory comes into operation and breaches 90T high-intensity magnetic fields high point,
But yet suffer from some technical bottlenecks at present to need further research and solve.For example, still cannot realize quantitatively, production
Cycle is long, and drawing process radial force difference causes Nb fibrosclerosiss degree uneven first-class.Prepare to solve Cu-Nb alloy materials
The technical problem that field is present, the invention discloses a kind of method for directly preparing fine grain Cu-Nb alloy blank, can be by drawing
The technique such as pull out, roll and more efficiently preparing Cu-Nb alloy wires or band that microstructure thinning causes Nano grade.
The content of the invention
It is an object of the invention to provide a kind of preparation method of high-strength high-conductivity Cu-Nb alloy blanks, its feature
It is that the high-strength high-conductivity Cu-Nb alloys are Cu-Nb bianry alloys, its main component is：Cu elements are 80-
98wt%, Nb element is 2-20wt%；Semi-solid casting technology is combined using the solidification of solid-liquid two-phase, and pure niobium powder is added
Alloy melt, forms the solid solution of richness Nb in rapid solidification, and by drawing, that rolling mill practice prepares microscopic structure is thin
The Cu-Nb alloy blanks of change cause Nano grade, its tensile strength 1300-1700MPa, conductivity is higher than 75%IACS, the alloy
The crystallite dimension of blank is 1-30 μm, can greatly improve the preparation efficiency of this alloy wire, thin-band material.
A kind of concrete technology step of the preparation method of high-strength high-conductivity Cu-Nb alloy blanks includes：
(1) melting of alloy and solid-liquid mix：With fine copper ingot, pure niobium ingot, pure niobium powder as raw material, it is into being grouped into
Fine copper ingot is 80-98wt%, and pure niobium ingot is 1-17wt%, and pure niobium powder is 1-3wt%；The particle diameter of wherein pure niobium powder is
0.5-30 μm, and remove its oxide on surface through reduction treatment；First, by fine copper ingot and pure niobium ingot mixing post-heating extremely
1300-1700 DEG C so as to be fused into alloy melt, after insulation 10min, melt liquid level is protected using argon, and by pure niobium powder
End adds alloy melt；
(2) Melt Stirring：1-5min is sufficiently stirred for alloy melt using mechanical agitation mode, while by alloy melt temperature
Degree is reduced to 1200-1600 DEG C and is incubated 10-15min, makes alloy melt rapid partially solidified and forms semisolid mixing
Tissue；
(3) quick cooling：The melt cast of above-mentioned semisolid line and staff control is prepared in the mould using circulating water
Into ingot casting, room temperature is cooled to the speed of 100-200 DEG C/min, obtains high-strength high-conductivity Cu-Nb alloy blanks.
The invention has the beneficial effects as follows the present invention combines semi-solid casting technology using the solidification of solid-liquid two-phase, close in Cu-Nb
Fine copper powder is added in golden melt, and stirring forms microstructure of semisolid, notable refining alloy as-cast microstructure, and make Nb
It is that the microstructure thinning technique during deformation after unloading is laid a good foundation more in solid solution and Cu matrixes.Can directly make
For the tiny big specification Cu-Nb alloy blank of crystallite dimension is gone out, Cu-Nb alloy wires, band etc. can be on the one hand greatly improved
The working (machining) efficiency of product, additionally it is possible to prepare the Cu-Nb alloy material products of more specifications, its tensile strength 1300-
1700MPa, conductivity is higher than 75%IACS, and the application of this material has been expanded significantly.
Specific embodiment
The present invention provides a kind of preparation method of high-strength high-conductivity Cu-Nb alloy blanks, and the high intensity height is led
Electrical property Cu-Nb alloys are Cu-Nb bianry alloys, and its main component is：Cu elements are 80-98wt%, and Nb elements are 2-
20wt%；Semi-solid casting technology is combined using the solidification of solid-liquid two-phase, and pure niobium powder is added into alloy melt, quick
The solid solution of richness Nb is formed in process of setting, and microstructure thinning is prepared by drawing, rolling mill practice and cause Nano grade
Cu-Nb alloy blanks, its tensile strength 1300-1700MPa, conductivity is higher than 75%IACS, the crystallite dimension of the alloy blank
For 1-30 μm, the preparation efficiency of this alloy wire, thin-band material can be greatly improved.Embodiment is set forth below to be explained.
Embodiment 1：Cu-2Nb alloys
Cu-2Nb alloys are prepared, is comprised the steps：
(1) melting of alloy and solid-liquid mix：With fine copper ingot, pure niobium ingot, pure niobium powder as raw material, it is according to fine copper ingot
98wt%, pure niobium ingot is 1wt% and pure niobium powder is 1% dispensing, wherein the particle diameter of described pure niobium powder is 30 μm, and
And remove its oxide on surface through reduction treatment.First, melt it to 1300 DEG C fine copper ingot and pure niobium ingot mixing post-heating
Chemical conversion alloy melt, after insulation 10min, using argon melt liquid level is protected, and pure niobium powder is added into alloy melt；
(2) Melt Stirring：5min is sufficiently stirred for alloy melt using mechanical agitation mode, while by alloy melt temperature
It is reduced to 1200 DEG C and is incubated 15min, makes alloy melt rapid partially solidified and form semisolid line and staff control；
(3) quick cooling：The melt cast of above-mentioned semisolid line and staff control is prepared in the mould using circulating water
Into ingot casting, room temperature is cooled to the speed of 190 DEG C/min, obtains Cu-2Nb alloys；Its microscopic structure its average crystal grain diameter is
30 μm, its tensile strength 1300-1700MPa, conductivity is higher than 75%IACS.
Embodiment 2：Cu-5Nb alloys
Cu-5Nb alloys are prepared, is comprised the steps：
(1) melting of alloy and solid-liquid mix：With fine copper ingot, pure niobium ingot, pure niobium powder as raw material, it is according to fine copper ingot
95wt%, pure niobium ingot is 4wt%, and pure niobium powder is 1wt% dispensings, wherein the particle diameter of described pure niobium powder is 10 μm,
And remove its oxide on surface through reduction treatment.First, fine copper ingot and pure niobium ingot mixing post-heating are made into it to 1400 DEG C
Alloy melt is fused into, after insulation 10min, melt liquid level is protected using argon, and pure niobium powder is added into alloy melt.
(2) Melt Stirring：Subsequently, immediately 1-5min is sufficiently stirred for alloy melt using mechanical agitation mode, while will
Alloy melt temperature is reduced to 1350 DEG C and is incubated 15min, makes alloy melt rapid partially solidified and form semisolid to mix
It is charge-coupled to knit.
(3) quick cooling：The melt cast of above-mentioned semisolid line and staff control is prepared in the mould using circulating water
Into ingot casting, room temperature is cooled to the speed of 100-200 DEG C/min, obtains Cu-5Nb alloys；Its average crystal grain of its microscopic structure is straight
Footpath is 15 μm, its tensile strength 1300-1700MPa, and conductivity is higher than 75%IACS.
Embodiment 3：Cu-10Nb alloys
Cu-10Nb alloys are prepared, is comprised the steps：
(1) melting of alloy and solid-liquid mix：With fine copper ingot, pure niobium ingot, pure niobium powder as raw material, it is according to fine copper ingot
90wt%, pure niobium ingot is 7wt%, and pure niobium powder is 3wt% dispensings, wherein the particle diameter of described pure niobium powder is 5 μm, and
And remove its oxide on surface through reduction treatment.First, melt it to 1450 DEG C fine copper ingot and pure niobium ingot mixing post-heating
Chemical conversion alloy melt, after insulation 10min, using argon melt liquid level is protected, and pure niobium powder is added into alloy melt；
(2) Melt Stirring：Subsequently, immediately 5min is sufficiently stirred for alloy melt using mechanical agitation mode, while will close
Golden melt temperature is reduced to 1400 DEG C and is incubated 15min, makes alloy melt rapid partially solidified and forms semisolid mixing
Tissue；
(3) quick cooling：The melt cast of above-mentioned semisolid line and staff control is prepared in the mould using circulating water
Into ingot casting, room temperature is cooled to the speed of 200 DEG C/min, obtains Cu-5Nb alloys；Its microscopic structure its average crystal grain diameter is
10 μm, its tensile strength 1300-1700MPa, conductivity is higher than 75%IACS.
Embodiment 4：Cu-15Nb alloys
Cu-15Nb alloys are prepared, is comprised the steps：
(1) melting of alloy and solid-liquid mix：With fine copper ingot, pure niobium ingot, pure niobium powder as raw material, it is according to fine copper ingot
85wt%, pure niobium ingot is 12.5wt%, and pure niobium powder is 2.5wt% dispensings, wherein the particle diameter of described pure niobium powder is 2
μm, and remove its oxide on surface through reduction treatment.First, fine copper ingot and pure niobium ingot mixing post-heating are made to 1600 DEG C
It is fused into alloy melt, after insulation 10min, using argon melt liquid level is protected, and pure niobium powder is added into alloy melt.
(2) Melt Stirring：Subsequently, immediately 5min is sufficiently stirred for alloy melt using mechanical agitation mode, while will close
Golden melt temperature is reduced to 1500 DEG C and is incubated 10min, makes alloy melt rapid partially solidified and forms semisolid mixing
Tissue.
(3) quick cooling：The melt cast of above-mentioned semisolid line and staff control is prepared in the mould using circulating water
Into ingot casting, room temperature is cooled to the speed of 180 DEG C/min, obtains Cu-15Nb alloys；Its microscopic structure its average crystal grain diameter is
20 μm, its tensile strength 1300-1700MPa, conductivity is higher than 75%IACS.
Embodiment 5：Cu-20Nb alloys
Cu-20Nb alloys are prepared, is comprised the steps：
(1) melting of alloy and solid-liquid mix：With fine copper ingot, pure niobium ingot, pure niobium powder as raw material, it is according to fine copper ingot
80wt%, pure niobium ingot is 17wt%, and pure niobium powder is 3wt% dispensings, wherein the particle diameter of described fine copper powder is 1 μm,
And remove its oxide on surface through reduction treatment.First, fine copper ingot and pure niobium ingot mixing post-heating are made into it to 1700 DEG C
Alloy melt is fused into, after insulation 10min, melt liquid level is protected using argon, and pure niobium powder is added into alloy melt.
(2) Melt Stirring：Subsequently, immediately 5min is sufficiently stirred for alloy melt using mechanical agitation mode, while will close
Golden melt temperature is reduced to 1600 DEG C and is incubated 13min, makes alloy melt rapid partially solidified and forms semisolid mixing
Tissue.
(3) quick cooling：The melt cast of above-mentioned semisolid line and staff control is prepared in the mould using circulating water
Into ingot casting, room temperature is cooled to the speed of 200 DEG C/min, obtains Cu-20Nb alloys；Its microscopic structure its average crystal grain diameter is
25 μm, its tensile strength 1300-1700MPa, conductivity is higher than 75%IACS.
Claims (4)
1. a kind of preparation method of high-strength high-conductivity Cu-Nb alloy blanks, it is characterised in that the high-strength high conductivity
Performance Cu-Nb alloy is Cu-Nb bianry alloys, and its main component is：Cu elements are 80-98wt%, and Nb elements are 2-20wt%；
Semi-solid casting technology is combined using the solidification of solid-liquid two-phase, and pure niobium powder is added into alloy melt, in rapid solidification
The solid solution of richness Nb is formed, and the Cu-Nb alloy preforms that microstructure thinning causes Nano grade are prepared by drawing, rolling mill practice
Material, its tensile strength 1300-1700MPa, conductivity is higher than 75%IACS, and the crystallite dimension of the alloy blank is 1-30 μm, energy
Enough greatly improve the preparation efficiency of this alloy wire, thin-band material.
2. a kind of preparation method of high-strength high-conductivity Cu-Nb alloy blanks according to claim 1, its feature exists
In step of preparation process includes：
(1) melting of alloy and solid-liquid mix：With fine copper ingot, pure niobium ingot, pure niobium powder as raw material, it is into being grouped into fine copper
Ingot is 80-98wt%, and pure niobium ingot is 1-17wt%, and pure niobium powder is 1-3wt%；The particle diameter of wherein pure niobium powder is 0.5-
30 μm, and remove its oxide on surface through reduction treatment；First, by fine copper ingot and pure niobium ingot mixing post-heating to 1300-
1700 DEG C so as to be fused into alloy melt, after insulation 10min, melt liquid level is protected using argon, and pure niobium powder is added
Alloy melt；
(2) Melt Stirring：1-5min is sufficiently stirred for alloy melt using mechanical agitation mode, while alloy melt temperature is dropped
As little as 1200-1600 DEG C and 10-15min is incubated, makes alloy melt rapid partially solidified and form semisolid line and staff control；
(3) quick cooling：The melt cast of above-mentioned semisolid line and staff control is prepared into casting in the mould using circulating water
Ingot, with the speed of 100-200 DEG C/min room temperature is cooled to, and obtains high-strength high-conductivity Cu-Nb alloy blanks.
3. a kind of preparation method of high-strength high-conductivity Cu-Nb alloy blanks, it is characterised in that specifically prepare Cu-10Nb
Alloy comprises the steps：
(1) melting of alloy and solid-liquid mix：With fine copper ingot, pure niobium ingot, pure niobium powder as raw material, it is according to fine copper ingot
90wt%, pure niobium ingot is 7wt%, and pure niobium powder is 3wt% dispensings, wherein the particle diameter of described pure niobium powder is 5 μm, and
And remove its oxide on surface through reduction treatment.First, melt it to 1450 DEG C fine copper ingot and pure niobium ingot mixing post-heating
Chemical conversion alloy melt, after insulation 10min, using argon melt liquid level is protected, and pure niobium powder is added into alloy melt；
(2) Melt Stirring：Subsequently, immediately 5min is sufficiently stirred for alloy melt using mechanical agitation mode, while alloy is melted
Temperature reduction is to 1400 DEG C and is incubated 15min, makes alloy melt rapid partially solidified and forms semisolid line and staff control；
(3) quick cooling：The melt cast of above-mentioned semisolid line and staff control is prepared into casting in the mould using circulating water
Ingot, with the speed of 200 DEG C/min room temperature is cooled to, and obtains Cu-5Nb alloys；Its average crystal grain diameter of its microscopic structure is 10 μm,
Its tensile strength 1300-1700MPa, conductivity is higher than 75%IACS.
4. a kind of preparation method of high-strength high-conductivity Cu-Nb alloy blanks, it is characterised in that specifically prepare Cu-15Nb
Alloy comprises the steps：
(1) melting of alloy and solid-liquid mix：With fine copper ingot, pure niobium ingot, pure niobium powder as raw material, it is according to fine copper ingot
85wt%, pure niobium ingot is 12.5wt%, and pure niobium powder is 2.5wt% dispensings, wherein the particle diameter of described pure niobium powder is 2
μm, and remove its oxide on surface through reduction treatment.First, fine copper ingot and pure niobium ingot mixing post-heating are made to 1600 DEG C
It is fused into alloy melt, after insulation 10min, using argon melt liquid level is protected, and pure niobium powder is added into alloy melt；
(2) Melt Stirring：Subsequently, immediately 5min is sufficiently stirred for alloy melt using mechanical agitation mode, while alloy is melted
Temperature reduction is to 1500 DEG C and is incubated 10min, makes alloy melt rapid partially solidified and forms semisolid line and staff control；
(3) quick cooling：The melt cast of above-mentioned semisolid line and staff control is prepared into casting in the mould using circulating water
Ingot, with the speed of 180 DEG C/min room temperature is cooled to, and obtains Cu-15Nb alloys；Its average crystal grain diameter of its microscopic structure is 20 μ
M, its tensile strength 1300-1700MPa, conductivity is higher than 75%IACS.
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| CN111041250A (en) * | 2019-11-27 | 2020-04-21 | 江苏科技大学 | Preparation method of copper-niobium superconducting composite material |
| CN112007949A (en) * | 2020-08-27 | 2020-12-01 | 西北有色金属研究院 | Preparation method of reinforced Cu-Nb composite wire |
| CN113528883A (en) * | 2021-07-13 | 2021-10-22 | 上海理工大学 | Copper-niobium alloy for medical biopsy puncture needle |
| CN113969364A (en) * | 2021-09-10 | 2022-01-25 | 中南大学 | High-strength high-conductivity copper-niobium alloy and preparation method thereof |
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Effective date of registration: 20191115 Address after: 101407 Beijing city Huairou District Yanqi Economic Development Zone Branch Hing Street No. 11 Patentee after: Research Institute of engineering and Technology Co., Ltd. Address before: 100088 Beijing city Xicheng District Xinjiekou Avenue No. 2 Patentee before: General Research Institute for Nonferrous Metals |