CN108359837B - A kind of preparation method of the high silver-bearing copper pole of high-purity anaerobic - Google Patents
A kind of preparation method of the high silver-bearing copper pole of high-purity anaerobic Download PDFInfo
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- CN108359837B CN108359837B CN201810220408.8A CN201810220408A CN108359837B CN 108359837 B CN108359837 B CN 108359837B CN 201810220408 A CN201810220408 A CN 201810220408A CN 108359837 B CN108359837 B CN 108359837B
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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
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/001—Continuous casting of metals, i.e. casting in indefinite lengths of specific alloys
- B22D11/004—Copper alloys
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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
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/14—Plants for continuous casting
- B22D11/145—Plants for continuous casting for upward casting
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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
- C22C1/02—Making non-ferrous alloys by melting
Abstract
The invention belongs to nonferrous metallurgy manufacturing technology fields, specifically disclose a kind of preparation method of high silver-bearing copper pole of high-purity anaerobic, the following steps are included: (1) ingredient: preparing the raw material of following weight percent, silver-colored 0.0085-0.2%, zirconium 0.015-0.05%, chromium 0.015-0.03%, remaining is copper；(2) by raw copper heated baking；(3) raw material is fused into solution in 1138-1550 DEG C；(3) draw main frequency furnace holding furnace and transitional storehouse surface covering graphite flakes on melting sources, melting furnace surface covers charcoal and carries out oxygen barrier processing；And carbon dioxide gas is injected on full furnace surface；(4) water for drawing main frequency furnace cooling water in adjusting, makes hydraulic pressure be maintained at 0.2-0.25mpa, and the temperature of cooling water is maintained at 50-55 DEG C.The high-purity high silver-bearing copper pole of anaerobic is produced using this method, simplifies procedure of processing, energy consumption and manufacturing cost substantially reduce, and the obtained product of production antioxygenic property, creep-resistant property, wear-resisting, resistance to heat etching, in terms of be greatly improved.
Description
Technical field
The invention belongs to nonferrous metallurgy manufacturing technology field more particularly to a kind of preparation sides of the high silver-bearing copper pole of high-purity anaerobic
Method.
Background technique
Phase modifier is the synchronous motor of idle running, by changing the size of its exciting current, can control it be from
Absorbing reactive power or output reactive power in system.Have higher requirement to its rotor coil in phase modifier, it is desirable that its
Wearability, intensity, hardness etc. have good mechanical performance.Silver-bearing copper pole is due to joined micro silver element and resistance to
The mechanical properties such as mill, intensity, hardness have obtained biggish reinforcement, and have still maintained higher conductivity, therefore argentiferous
Copper bar largely applies in Large Rotor.Although the addition of micro silver element improves the machine of copper bar to a certain extent
Tool performance, but since the silver-bearing copper pole is applied on the rotor coil of phase modifier, high temperature, silver-bearing copper can be generated during use
Bar is oxidized easily, and service life needs to be extended.
Existing silver-bearing copper pole manufacturing method adds silver-colored ingredient the following steps are included: 1) high-purity catholyte copper sheet and feed back；
2) smelting furnace founding copper ingot is used；3) sawing forms；4) gas furnace heats；5) 2000 tons of water seals are squeezed into blank；6) 400 type of Φ
Rolled by cold rolling machine；7) vehicle bottom type annealing furnace is annealed；8) pickling, pointing；9) 30 tons of cold-drawn machine cold drawings are at finished product.Existing silver-bearing copper
Bar procedure of processing is various, including the links such as extruding, cold rolling, annealing, pickling, squeezes, cold rolling step is easy to make the surface of product to become
Out-of-flatness is obtained, and generates stress deformation, is made annealing treatment, residual stress, stable dimensions are eliminated.In the process of annealing
In, product is easy to happen oxidation reaction, generates oxidized residual object etc. on the surface of product, increases the contact resistance of product, blocked up
Oxide skin(coating) can even prevent electric current to lead to the problem of current density excessive by or part, to generate splashing and table
Face scaling loss shortens the service life of material.In addition, existing production method production efficiency is low, and serious waste of resources, finished product
Rate is not also high.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of high-purity high silver-bearing copper pole of anaerobic, high production efficiency, manufactures
Cost substantially reduces, and the silver-bearing copper pole good mechanical property being prepared, and antioxygenic property is good, and surface is free of oxidized residual object.
In order to achieve the above object, base case of the invention are as follows: a kind of preparation method of high-purity high silver-bearing copper pole of anaerobic,
It is prepared using up-drawing method technique, comprising the following steps:
(1) ingredient: prepare the raw material of following weight percent, silver-colored 0.0085-0.2%, zirconium 0.015-0.05%, chromium
0.015-0.03%, remaining is copper；
(2) by raw copper heated baking ready for use；
(3) copper through overbaking in the silver of step (1), zirconium, chromium and step (2) is fused into 1138-1550 DEG C molten
Liquid, often plus other raw materials in step (1) are added in one block of copper, correspondence, it is ensured that the proportion of various raw materials meets the requirements；
(4) draw main frequency furnace holding furnace and transitional storehouse surface covering graphite flakes, melting furnace on fusing step (1) raw material
Surface covers charcoal and carries out oxygen barrier processing；And full furnace surface inject from the top down carbon dioxide gas carry out it is oxygen barrier again；
(5) water for drawing main frequency furnace cooling water in adjusting, is maintained at hydraulic pressure within the scope of 0.2-0.25mpa, cooling
The temperature of water is maintained within the scope of 50-55 DEG C；Draw main frequency furnace on described and Cu crystallizer is installed.
The beneficial effect of this base case is:
1. in order to make silver-bearing copper pole also have good inoxidizability while having excellent mechanical properties, applicant is carried out
Test repeatedly, applicant have found under study for action, exist although conventional element with antioxygenic property is added in the feed
The inoxidizability of silver-bearing copper pole is improved to a certain extent, but since the addition of these elements reduces the mechanicalness of silver-bearing copper pole
Can, the also biggish conductivity for reducing silver-bearing copper pole in part.By constantly testing and theory analysis, it is found by the applicant that
It joined micro zirconium, chromium in raw material, silver-bearing copper pole is obtained in mechanical properties such as wear-resisting, resistance to heat etching, intensity, hardness
Reinforce, antioxygenic property is greatly improved, and silver-bearing copper pole conductivity it is not too high will not be too low, can be fine
The actual requirement for meeting phase modifier, which can be good at applying on the rotor coil of phase modifier, service life
Effectively extend.
2. first being toasted to copper before melting copper, the moisture content in copper is removed in baking process, is avoided in following process mistake
Keep product oxidizable due to the presence of moisture content in journey, improves the quality of product.
3. melting copper and the control of Yin Shi temperature are higher than routine, then speed cooling in subsequent cooling procedure slows down；
And in cooling procedure, hydraulic pressure is smaller, and the water outlet of cooling water slows, and the initial temperature of cooling water is higher, further decreases
Cooling velocity, the cooling velocity by controlling silver-bearing copper pole make silver-bearing copper pole crystallization more evenly, and crystal grain is bigger, increases silver-bearing copper
The tensile strength and elongation percentage of bar.
4. preparing silver-bearing copper pole using this method, relative to existing production technology, does not need to be squeezed, anneal, acid
The procedure of processings such as wash, energy consumption and manufacturing cost substantially reduce, and product quality and yield rate greatly improve.
5. covering charcoal, graphite phosphorus sheet, it can be well isolated from contact of the silver-bearing copper solution with air, and inject carbon dioxide
Gas can be oxygen barrier again, and oxygen is further prevented to enter, even if micro oxygen is possible to penetrate into silver-bearing copper solution, with copper
It reacts and generates copper oxide, and graphite phosphorus sheet can be chemically reacted with copper oxide, reaction product P2O5It is volatilizable for gas
Evolution, therefore, the present patent application is compared with prior art, hardly oxygen-containing in silver-bearing copper solution, the product surface produced
There is no oxidized residual object.
Further, it is 99.99% silver ingot that the silver in step (1), which selects purity, and copper selects high-purity catholyte copper.It selects
Above-mentioned raw materials prepare silver-bearing copper pole, and obtained product purity is high, high-quality.
Further, the silver of selection test resistance rate at 20 DEG C is 1.765-1.898 μ Ω .cm.In production silver-bearing copper pole
The silver that resistivity is 1.765-1.898 μ Ω .cm is added in the process, the resistivity of silver-bearing copper pole can be adjusted, enable silver-bearing copper pole
Enough meet the requirement of phase modifier.
Further, copper and silver are fused into solution in 1280-1530 DEG C in the step (2).
Further, it during preparing the high silver-bearing copper pole of high-purity anaerobic using up-drawing method, sets and draws bar pitch as 6-7mm,
Drawing bar speed is 0.4-0.55m/min.By applicant's the study found that can guarantee copper by state modulator in above range
Liquid solidifies near bar quickly drawing, the crystals tissue tight of formation, uniformly.
Further, further include step (5) crystallization rod: when carrying out drawing bar, temperature control 1135-1550 DEG C range it
It is interior, draw bar speed and be maintained within the scope of 0.4-0.55m/min, draws bar and obtain finished product.The study found that it will by applicant's
State modulator has good mobility and castability, can obtain good crystallization in above range, the Kufil of melting
Tissue and crystalline quality, the product better mechanical property produced.
Specific embodiment
Below by specific embodiment, the present invention is described in further detail:
Embodiment 1
A kind of preparation method of the high silver-bearing copper pole of high-purity anaerobic, is prepared using up-drawing method technique, comprising the following steps:
(1) ingredient: prepare the raw material of following weight percent: silver 0.009%, zirconium 0.018%, chromium 0.015%, copper
99.958%, wherein it is 99.99% silver ingot that silver, which selects purity, silver test resistance rate at 20 DEG C is 1.784 μ Ω .cm, copper choosing
With high-purity catholyte copper；
(2) the high-purity catholyte copper of raw material ready for use is placed in draw and is toasted above main frequency furnace, it will be in cathode copper
Moisture bake；
(3) raw material of step (1) is fused into solution in 1288 DEG C, one row's cathode copper of every addition is corresponding that step is added
(1) other raw materials in, make the weight percent of each raw material meet the requirements；
(4) draw main frequency furnace holding furnace and transitional storehouse surface covering graphite flakes, melting furnace on fusing step (1) raw material
Surface covers charcoal and carries out oxygen barrier processing；And full furnace surface from the top down slowly injection carbon dioxide gas carry out again every
Oxygen；
(5) water for drawing main frequency furnace cooling water in adjusting, is maintained at hydraulic pressure within the scope of 0.2mpa, the temperature of cooling water
Degree is maintained at 50 DEG C；Draw main frequency furnace on described and Cu crystallizer is installed；
(6) it crystallizes rod: setting and draw bar pitch as 6mm, drawing bar speed is 0.42m/min；When carrying out drawing bar, temperature control
Within the scope of 1288 DEG C, draws bar speed and be maintained within the scope of 0.42m/min, draw bar and obtain finished product.
Embodiment 2
A kind of preparation method of the high silver-bearing copper pole of high-purity anaerobic, is prepared using up-drawing method technique, comprising the following steps:
(1) ingredient: prepare the raw material of following weight percent: silver 0.03%, zirconium 0.03%, chromium 0.022%, copper
99.918%, wherein it is 99.99% silver ingot that silver, which selects purity, silver test resistance rate at 20 DEG C is 1.821 μ Ω .cm, copper choosing
With high-purity catholyte copper；
(2) the high-purity catholyte copper of raw material ready for use is placed in draw and is toasted above main frequency furnace, it will be in cathode copper
Moisture bake；
(3) raw material of step (1) is fused into solution in 1350 DEG C, one row's cathode copper of every addition is corresponding that step is added
(1) other raw materials in, make the weight percent of each raw material meet the requirements；
(4) draw main frequency furnace holding furnace and transitional storehouse surface covering graphite flakes, melting furnace on fusing step (1) raw material
Surface covers charcoal and carries out oxygen barrier processing；And full furnace surface from the top down slowly injection carbon dioxide gas carry out again every
Oxygen；
(5) water for drawing main frequency furnace cooling water in adjusting, is maintained at hydraulic pressure within the scope of 0.22mpa, cooling water
Temperature is maintained at 55 DEG C；Draw main frequency furnace on described and Cu crystallizer is installed；
(6) it crystallizes rod: setting and draw bar pitch as 6mm, drawing bar speed is 0.48m/min；When carrying out drawing bar, temperature control
Within the scope of 1350 DEG C, draws bar speed and be maintained within the scope of 0.48m/min, draw bar and obtain finished product.
Embodiment 3
A kind of preparation method of the high silver-bearing copper pole of high-purity anaerobic, is prepared using up-drawing method technique, comprising the following steps:
(1) ingredient: prepare the raw material of following weight percent: silver 0.18%, zirconium 0.045%, chromium 0.029%, copper
99.746%, wherein it is 99.99% silver ingot that silver, which selects purity, silver test resistance rate at 20 DEG C is 1.848 μ Ω .cm, copper choosing
With high-purity catholyte copper；
(2) the high-purity catholyte copper of raw material ready for use is placed in draw and is toasted above main frequency furnace, it will be in cathode copper
Moisture bake；
(3) raw material of step (1) is fused into solution in 1460 DEG C, one row's cathode copper of every addition is corresponding that step is added
(1) other raw materials in, make the weight percent of each raw material meet the requirements；
(4) draw main frequency furnace holding furnace and transitional storehouse surface covering graphite flakes, melting furnace on fusing step (1) raw material
Surface covers charcoal and carries out oxygen barrier processing；And full furnace surface from the top down slowly injection carbon dioxide gas carry out again every
Oxygen；
(5) water for drawing main frequency furnace cooling water in adjusting, is maintained at hydraulic pressure within the scope of 0.22mpa, cooling water
Temperature is maintained at 55 DEG C；Draw main frequency furnace on described and Cu crystallizer is installed；
(6) it crystallizes rod: setting and draw bar pitch as 6.2mm, drawing bar speed is 0.54m/min；When carrying out drawing bar, temperature control
System is drawn bar speed and is maintained within the scope of 0.54m/min, draw bar and obtain finished product within the scope of 1460 DEG C.
Comparative example 1
Comparative example 1 the difference from embodiment 1 is that: (1) ingredient: prepare the raw material of following weight percent: silver
0.009%, copper 99.991%, wherein it is 99.99% silver ingot that silver, which selects purity, silver test resistance rate at 20 DEG C is 1.160 μ
Ω .cm, copper select high-purity catholyte copper.
Comparative example 2
Comparative example 2 the difference from embodiment 1 is that: (1) ingredient: prepare the raw material of following weight percent: silver
0.009%, zirconium 0.018%, copper 99.973%, wherein it is 99.99% silver ingot, silver test resistance at 20 DEG C that silver, which selects purity,
Rate is 1.784 μ Ω .cm, and copper selects high-purity catholyte copper.
Comparative example 3
Comparative example 3 the difference from embodiment 1 is that: (1) ingredient: prepare the raw material of following weight percent: silver
0.009%, chromium 0.015%, copper 99.976%, wherein it is 99.99% silver ingot, silver test resistance at 20 DEG C that silver, which selects purity,
Rate is 1.784 μ Ω .cm, and copper selects high-purity catholyte copper.
Comparative example 4
Comparative example 4 the difference from embodiment 1 is that: (1) ingredient: prepare the raw material of following weight percent: silver
0.009%, zirconium 0.008%, chromium 0.015%, copper 99.968%, wherein it is 99.99% silver ingot that silver, which selects purity, silver is at 20 DEG C
Lower test resistance rate is 1.784 μ Ω .cm, and copper selects high-purity catholyte copper.
Comparative example 5
Comparative example 5 the difference from embodiment 1 is that: (1) ingredient: prepare the raw material of following weight percent: silver
0.009%, zirconium 0.012%, chromium 0.015%, copper 99.964%, wherein it is 99.99% silver ingot that silver, which selects purity, silver is at 20 DEG C
Lower test resistance rate is 1.784 μ Ω .cm, and copper selects high-purity catholyte copper.
Comparative example 6
Comparative example 6 the difference from embodiment 1 is that: (1) ingredient: prepare the raw material of following weight percent: silver
0.009%, zirconium 0.062%, chromium 0.015%, copper 99.914%, wherein it is 99.99% silver ingot that silver, which selects purity, silver is at 20 DEG C
Lower test resistance rate is 1.784 μ Ω .cm, and copper selects high-purity catholyte copper.
Comparative example 7
Comparative example 7 the difference from embodiment 1 is that: (1) ingredient: prepare the raw material of following weight percent: silver
0.009%, zirconium 0.078%, chromium 0.015%, copper 99.898%, wherein it is 99.99% silver ingot that silver, which selects purity, silver is at 20 DEG C
Lower test resistance rate is 1.784 μ Ω .cm, and copper selects high-purity catholyte copper.
Comparative example 8
Comparative example 8 the difference from embodiment 1 is that: (1) ingredient: prepare the raw material of following weight percent: silver
0.009%, zirconium 0.018%, chromium 0.008%, copper 99.965%, wherein it is 99.99% silver ingot that silver, which selects purity, silver is at 20 DEG C
Lower test resistance rate is 1.784 μ Ω .cm, and copper selects high-purity catholyte copper.
Comparative example 9
Comparative example 9 the difference from embodiment 1 is that: (1) ingredient: prepare the raw material of following weight percent: silver
0.009%, zirconium 0.018%, chromium 0.012%, copper 99.961%, wherein it is 99.99% silver ingot that silver, which selects purity, silver is at 20 DEG C
Lower test resistance rate is 1.784 μ Ω .cm, and copper selects high-purity catholyte copper.
Comparative example 10
Comparative example 10 the difference from embodiment 1 is that: (1) ingredient: prepare the raw material of following weight percent: silver
0.009%, zirconium 0.018%, chromium 0.062%, copper 99.911%, wherein it is 99.99% silver ingot that silver, which selects purity, silver is at 20 DEG C
Lower test resistance rate is 1.784 μ Ω .cm, and copper selects high-purity catholyte copper.
Comparative example 11
Comparative example 11 the difference from embodiment 1 is that: (1) ingredient: prepare the raw material of following weight percent: silver
0.009%, zirconium 0.018%, chromium 0.078%, copper 99.895%, wherein it is 99.99% silver ingot that silver, which selects purity, silver is at 20 DEG C
Lower test resistance rate is 1.784 μ Ω .cm, and copper selects high-purity catholyte copper.
Comparative example 12
Comparative example 12 is the silver-bearing copper pole for phase modifier rotor coil bought in the market.
Table 1
Table 2: at 400 DEG C sample mass with oxidization time variation table
(explanation: the data of table 2 are sample increased quality after oxidation processes)
Table 1,2 data of table are that detection uses embodiment 1- embodiment 3, and comparative example 1- comparative example 12 produces obtained silver-bearing copper
The parameter that bar obtains.
Analyze conclusion:
1, it can be seen that addition quantitative zirconium and chromium by the experimental data of comparative analysis embodiment 1 and comparative example 1-3 to remove
It can reinforce outside the mechanical performance of silver-bearing copper pole, moreover it is possible to be effectively improved the inoxidizability of silver-bearing copper pole.
2, it can be seen that by the experimental data of comparative analysis embodiment 1-3, comparative example 4-7 and change containing for zirconium in raw material
Amount has large effect, the content of zirconium silver-bearing copper within the scope of 0.015-0.05% to mechanical performance, the inoxidizability of silver-bearing copper bar
Bar just obtains preferable comprehensive performance；Being analyzed simultaneously by data will also realize that, the mechanical performance of the additional amount of zirconium and silver-bearing copper pole,
Linear relationship is not present between inoxidizability.
3, it can be seen that by the experimental data of comparative analysis embodiment 1-3, comparative example 8-11 and change containing for chromium in raw material
Amount has large effect, the content of chromium silver-bearing copper within the scope of 0.015-0.03% to mechanical performance, the inoxidizability of silver-bearing copper bar
Bar just obtains preferable comprehensive performance；It will also realize that simultaneously by analysis data, the mechanical performance of the additional amount of chromium and silver-bearing copper pole,
Linear relationship is not present between inoxidizability.
4, the data of analysis comparative example 1-3 and comparative example 12 are it is found that the preparation method using this programme produces argentiferous
Copper bar has more superior mechanical performance, more good inoxidizability than silver-bearing copper pole in the market.
Claims (4)
1. a kind of preparation method of the high silver-bearing copper pole of high-purity anaerobic, it is characterised in that: it is prepared using up-drawing method technique, including
Following steps:
(1) ingredient: prepare the raw material of following weight percent, silver-colored 0.0085-0.2%, zirconium 0.015-0.05%, chromium 0.015-
0.03%, remaining is copper；
(2) by raw copper heated baking ready for use；
(3) copper through overbaking in the silver of step (1), zirconium, chromium and step (2) is fused into solution in 1138-1550 DEG C, often
Add one block of copper, the corresponding other raw materials being added in step (1), it is ensured that the proportion of various raw materials meets the requirements；
(4) draw main frequency furnace holding furnace and transitional storehouse surface covering graphite flakes, melting furnace surface on fusing step (1) raw material
It covers charcoal and carries out oxygen barrier processing；And full furnace surface inject from the top down carbon dioxide gas carry out it is oxygen barrier again；
(5) water for drawing main frequency furnace cooling water in adjusting, is maintained at hydraulic pressure within the scope of 0.2-0.25mpa, cooling water
Temperature is maintained within the scope of 50-55 DEG C；Draw main frequency furnace on described and Cu crystallizer is installed；
(6) crystallize rod: when carrying out drawing bar, temperature is controlled within the scope of 1135-1550 DEG C, is drawn bar speed and is maintained at 0.4-
Within the scope of 0.55m/min, draws bar and obtain finished product；During preparing the high silver-bearing copper pole of high-purity anaerobic using up-drawing method, if
Surely drawing bar pitch is 6-7mm.
2. a kind of preparation method of high-purity high silver-bearing copper pole of anaerobic according to claim 1, it is characterised in that: step (1)
In silver to select purity be 99.99% silver ingot, copper selects high-purity catholyte copper.
3. a kind of preparation method of high-purity high silver-bearing copper pole of anaerobic according to claim 2, it is characterised in that: the silver of selection
Test resistance rate is 1.765-1.898 μ Ω .cm at 20 DEG C.
4. a kind of preparation method of high-purity high silver-bearing copper pole of anaerobic according to claim 3, it is characterised in that: the step
(3) copper and silver are fused into solution in 1280-1530 DEG C in.
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| CN101474663B (en) * | 2009-01-16 | 2011-06-01 | 重庆鸽牌电工材料有限公司 | Preparation method of silver-bearing copper pole |
| CN102168180B (en) * | 2011-04-11 | 2013-05-08 | 中天合金技术有限公司 | Upcast method for producing high-purity bright copper rod |
| WO2014007259A1 (en) * | 2012-07-02 | 2014-01-09 | 古河電気工業株式会社 | Copper-alloy wire rod and manufacturing method therefor |
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| 连铸结晶器用Cr-Zr-Cu合金抗氧化性能分析;隋晓红等;《物理测试》;20071028;第25卷(第9期);第24-26页 |
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