CN107557601A - A kind of preparation method of high-strength highly-conductive copper wire - Google Patents
A kind of preparation method of high-strength highly-conductive copper wire Download PDFInfo
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- CN107557601A CN107557601A CN201710840503.3A CN201710840503A CN107557601A CN 107557601 A CN107557601 A CN 107557601A CN 201710840503 A CN201710840503 A CN 201710840503A CN 107557601 A CN107557601 A CN 107557601A
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Abstract
The invention discloses a kind of preparation method of high-strength highly-conductive copper wire, the technique carries out high temperature roll milling to cathode copper, high-temperature pressurizing, addition antioxidant obtain compound copper liquid, high-strength highly-conductive copper wire are obtained using techniques such as vacuum casting, forged, sub-cooled wire drawing, annealing, cleaning, dryings.The high-strength highly-conductive copper wire being prepared, its copper wire quality is light, intensity is big, electric conductivity is high, has preferable application prospect.
Description
Technical field
The present invention relates to this copper wire material used technical field, is related specifically to a kind of preparation method of high-strength highly-conductive copper wire.
Background technology
Ultramicro-fine brass wires are widely used in household electrical appliance, microelectronics, IT product, such as micro machine, relay, small-sized transformation
Device, inductance, oscillator coil, voice coil etc..It is general to require ultramicro-fine brass wires conductance height, single line length exceed 5000m with
On, the problems such as easily broken string in process due to ultramicro-fine brass wires, general lumber recovery is low, and the current country can only produce
Low-and-medium-grade products, line footpath is thicker, and in more than 0.05mm, single line length is within 3 kms.The production of ultramicro-fine brass wires is prepared at present
Technique mainly has following three kinds：1st, continuous casting and rolling low oxygen copper bar-rolling-drawing-annealing-drawing；2nd, up-casting oxygen-free copper rod-roll
System-drawing-annealing-drawing；3rd, continuous directional solidification-rolling-drawing-annealing-drawing.
Find that these three techniques have shortcoming by production practices：The first technique uses continuous casting and rolling low oxygen copper bar,
Its copper bar oxygen content is higher, typically in 200ppm~400ppm；Casting and rolling process need to pass through holding furnace, chute, centre simultaneously
Bag transhipment copper liquid, relatively easily causes the peeling of refractory material, and hot rolling process need to cause coming off for irony by roll, this
To copper bar outside can be brought to be mingled with.And be rolled into hot rolling on skin with subscale thing, to be caused to the wire drawing of hypoxemia bar unfavorable
Influence.Second of technique uses up-casting oxygen-free copper rod as as-cast structure, without hot-working is passed through in production process, above draws anaerobic
Copper bar easily produces stomata, shrinkage porosite, and rough surface, and broken string is easily produced in follow-up drawing process.The third technique
Using directional solidification technique, columnar single crystal is combined with follow-up plastic working, production efficiency is relatively low, and energy consumption is larger etc. be present
Shortcoming.
The characteristics of ultra-fine copper wire is due to its softness, good conductivity, application is more and more extensive, meanwhile, it is widely applied to super
Thin copper wire proposes higher and higher requirement, and the particularly yield to ultra-fine copper wire and the life-span proposes higher requirement.It is ultra-fine
In the production technology of copper wire, the annealing process of ultra-fine copper wire is always an important side for restricting ultra-fine copper wire yield and quality
Face.At present, ultra-fine copper wire annealing of the prior art, can only carry out single annealing, because the diameter of ultra-fine copper wire only has
0.03mm-0.07mm；Copper wire will be broken using excessive power traction such as in annealing process, it is necessary to after copper wire is connected
It could continue to produce, so causing ultra-fine copper wire process velocity and production capacity to be restricted；Meanwhile the annealing used in the prior art
The ultra-fine copper wire oxidation resistance of technology production is weak, can only use to half a year and just be oxidized, it is necessary to change.The present invention passes through copper
Process modification prepared by silk, optimization copper wire wire-drawing process make copper wire diameter and it is thin on the premise of keep high performance electric conductivity and
Intensity, there is fabulous application prospect.
The content of the invention
In order to solve the above technical problems, the present invention provides a kind of preparation method of high-strength highly-conductive copper wire, the technique is to electrolysis
Copper carries out high temperature roll milling, high-temperature pressurizing, and addition antioxidant is obtained compound copper liquid, pulled out using vacuum casting, forged, sub-cooled
The techniques such as silk, annealing, cleaning, drying obtain high-strength highly-conductive copper wire.The high-strength highly-conductive copper wire being prepared, its copper wire quality are light, strong
Degree is big, electric conductivity is high, has preferable application prospect.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of preparation method of high-strength highly-conductive copper wire, comprises the following steps：
(1) cathode copper being added in high-temperature roller furnace, is warming up to 1200-1260 DEG C, insulation fusing is complete, obtains copper liquid,
Inert gas is passed through into copper liquid, while adds antioxidant, then is warming up to 1500-1520 DEG C, electromagnetic agitation 30-45min is quiet
Purchase use；
(2) copper liquid of step (1) is subjected to vacuum bottom pour mold casting, after ingot casting cooling, removes casting pressing port, carry out ingot casting table
Face is cleaned, and is then placed in resistance-heated furnace and is heated, 950-965 DEG C of heating-up temperature, soaking time 60-90min, is carried out after taking-up
Hot forging, until alloy size reaches preset value；
(3) wire drawing is carried out to the copper alloy of step (2), silk material is entered wire-drawing die using sub-cooled at wire-drawing die both ends
It is preceding and for equal fast cooling between -110 DEG C to -196 DEG C, low temperature wire drawing process is performed repeatedly until institute after wire-drawing die
The silk material size needed；
(4) copper wire obtained step (3) carries out thermal annealing, and wherein thermal annealing temperatures are 350-400 DEG C, and the time is about
15-25 minutes；
(5) spend ionized water to the annealing copper wire of step (4) to be cleaned three times, then 65 DEG C of drying, get product.
Preferably, the antioxidant in the step (1) be selected from three (2.4- di-tert-butyl-phenyls) phosphite esters, four (β-
(3,5- di-tert-butyl-hydroxy phenyl) propionic ester) pentaerythritol ester, β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid is just
One or more in octadecanol ester.
Preferably, the inert gas in the step (1) is nitrogen.
Preferably, the vacuum pressure in the step (2) is 2*10-2-3*10-2Pa。
Preferably, surface cleaning is specific in the step (2) is carried out using 6% SDS solution.
Compared with prior art, its advantage is the present invention：
(1) preparation method of high-strength highly-conductive copper wire of the invention carries out high temperature roll milling, high-temperature pressurizing to cathode copper, and addition resists
Oxidant obtains compound copper liquid, is obtained using techniques such as vacuum casting, forged, sub-cooled wire drawing, annealing, cleaning, dryings high-strength
Height leads copper wire.The high-strength highly-conductive copper wire being prepared, its copper wire quality is light, intensity is big, electric conductivity is high, has preferably application
Prospect.
(2) high-strength highly-conductive copper wire raw material of the invention be easy to get, technique it is simple, used suitable for heavy industrialization, practicality
By force.
Embodiment
The technical scheme of invention is described in detail with reference to specific embodiment.
Embodiment 1
(1) cathode copper is added in high-temperature roller furnace, is warming up to 1200 DEG C, insulation fusing is complete, copper liquid is obtained, to copper liquid
In be passed through nitrogen gas, while add three (2.4- di-tert-butyl-phenyls) phosphite esters, then be warming up to 1500 DEG C, electromagnetic agitation
30min, stand for standby use；
(2) copper liquid of step (1) is subjected to vacuum bottom pour mold casting, wherein vacuum pressure is 2*10-2Pa, after ingot casting cooling,
Remove casting pressing port, ingot casting surface cleaning is carried out using 6% SDS solution, is then placed in resistance-heated furnace and heats, heat
950 DEG C, soaking time 60min of temperature, hot forging is carried out after taking-up, until alloy size reaches preset value；
(3) wire drawing is carried out to the copper alloy of step (2), silk material is entered wire-drawing die using sub-cooled at wire-drawing die both ends
It is preceding and for equal fast cooling to -110 DEG C, low temperature wire drawing process is performed repeatedly until required silk material chi after wire-drawing die
It is very little；
(4) copper wire obtained step (3) carries out thermal annealing, and wherein thermal annealing temperatures are 350-400 DEG C, and the time is about
15 minutes；
(5) spend ionized water to the annealing copper wire of step (4) to be cleaned three times, then 65 DEG C of drying, get product.
The performance test results of obtained high-strength highly-conductive copper wire are as shown in table 1.
Embodiment 2
(1) cathode copper is added in high-temperature roller furnace, is warming up to 1220 DEG C, insulation fusing is complete, copper liquid is obtained, to copper liquid
In be passed through nitrogen gas, while add four (β-(3,5- di-tert-butyl-hydroxy phenyl) propionic ester) pentaerythritol esters, then heat up
To 1505 DEG C, electromagnetic agitation 35min, stand for standby use；
(2) copper liquid of step (1) is subjected to vacuum bottom pour mold casting, wherein vacuum pressure is 2.2*10-2Pa, treat that ingot casting cools down
Afterwards, remove casting pressing port, ingot casting surface cleaning carried out using 6% SDS solution, is then placed in resistance-heated furnace and heats,
955 DEG C, soaking time 70min of heating-up temperature, hot forging is carried out after taking-up, until alloy size reaches preset value；
(3) wire drawing is carried out to the copper alloy of step (2), silk material is entered wire-drawing die using sub-cooled at wire-drawing die both ends
It is preceding and for equal fast cooling to -130 DEG C, low temperature wire drawing process is performed repeatedly until required silk material chi after wire-drawing die
It is very little；
(4) copper wire for obtaining step (3) carries out thermal annealing, and wherein thermal annealing temperatures are 370 DEG C, and the time is about 18 points
Clock；
(5) spend ionized water to the annealing copper wire of step (4) to be cleaned three times, then 65 DEG C of drying, get product.
The performance test results of obtained high-strength highly-conductive copper wire are as shown in table 1.
Embodiment 3
(1) cathode copper is added in high-temperature roller furnace, is warming up to 1250 DEG C, insulation fusing is complete, copper liquid is obtained, to copper liquid
In be passed through nitrogen gas, while add β-positive octadecanol ester of (3,5- di-tert-butyl-hydroxy phenyl) propionic acid, then be warming up to
1515 DEG C, electromagnetic agitation 40min, stand for standby use；
(2) copper liquid of step (1) is subjected to vacuum bottom pour mold casting, wherein vacuum pressure is 2.6*10-2Pa, treat that ingot casting cools down
Afterwards, remove casting pressing port, ingot casting surface cleaning carried out using 6% SDS solution, is then placed in resistance-heated furnace and heats,
960 DEG C, soaking time 80min of heating-up temperature, hot forging is carried out after taking-up, until alloy size reaches preset value；
(3) wire drawing is carried out to the copper alloy of step (2), silk material is entered wire-drawing die using sub-cooled at wire-drawing die both ends
It is preceding and for equal fast cooling to -180 DEG C, low temperature wire drawing process is performed repeatedly until required silk material chi after wire-drawing die
It is very little；
(4) copper wire for obtaining step (3) carries out thermal annealing, and wherein thermal annealing temperatures are 390 DEG C, and the time is about 20 points
Clock；
(5) spend ionized water to the annealing copper wire of step (4) to be cleaned three times, then 65 DEG C of drying, get product.
The performance test results of obtained high-strength highly-conductive copper wire are as shown in table 1.
Embodiment 4
(1) cathode copper is added in high-temperature roller furnace, is warming up to 1260 DEG C, insulation fusing is complete, copper liquid is obtained, to copper liquid
In be passed through nitrogen gas, while add four (β-(3,5- di-tert-butyl-hydroxy phenyl) propionic ester) pentaerythritol esters, then heat up
To 1520 DEG C, electromagnetic agitation 45min, stand for standby use；
(2) copper liquid of step (1) is subjected to vacuum bottom pour mold casting, wherein vacuum pressure is 3*10-2Pa, after ingot casting cooling,
Remove casting pressing port, ingot casting surface cleaning is carried out using 6% SDS solution, is then placed in resistance-heated furnace and heats, heat
965 DEG C, soaking time 90min of temperature, hot forging is carried out after taking-up, until alloy size reaches preset value；
(3) wire drawing is carried out to the copper alloy of step (2), silk material is entered wire-drawing die using sub-cooled at wire-drawing die both ends
It is preceding and for equal fast cooling to -196 DEG C, low temperature wire drawing process is performed repeatedly until required silk material chi after wire-drawing die
It is very little；
(4) copper wire for obtaining step (3) carries out thermal annealing, and wherein thermal annealing temperatures are 400 DEG C, and the time is about 25 points
Clock；
(5) spend ionized water to the annealing copper wire of step (4) to be cleaned three times, then 65 DEG C of drying, get product.
The performance test results of obtained high-strength highly-conductive copper wire are as shown in table 1.
Comparative example 1
(1) cathode copper is added in high-temperature roller furnace, is warming up to 1200 DEG C, insulation fusing is complete, copper liquid is obtained, to copper liquid
In be passed through nitrogen gas, while add three (2.4- di-tert-butyl-phenyls) phosphite esters, then be warming up to 1500 DEG C, electromagnetic agitation
30min, stand for standby use；
(2) copper liquid of step (1) is subjected to vacuum bottom pour mold casting, wherein vacuum pressure is 2*10-2Pa, after ingot casting cooling,
Remove casting pressing port, be then placed in resistance-heated furnace and heat, 950 DEG C, soaking time 60min of heating-up temperature, carried out after taking-up
Hot forging, until alloy size reaches preset value；
(3) wire drawing is carried out to the copper alloy of step (2), silk material is entered wire-drawing die using sub-cooled at wire-drawing die both ends
It is preceding and for equal fast cooling to -110 DEG C, low temperature wire drawing process is performed repeatedly until required silk material chi after wire-drawing die
It is very little；
(4) copper wire obtained step (3) carries out thermal annealing, and wherein thermal annealing temperatures are 350-400 DEG C, and the time is about
15 minutes；
(5) spend ionized water to the annealing copper wire of step (4) to be cleaned three times, then 65 DEG C of drying, get product.
The performance test results of obtained high-strength highly-conductive copper wire are as shown in table 1.
Comparative example 2
(1) cathode copper is added in high-temperature roller furnace, is warming up to 1260 DEG C, insulation fusing is complete, obtains copper liquid, adds simultaneously
Enter four (β-(3,5- di-tert-butyl-hydroxy phenyl) propionic ester) pentaerythritol esters, then be warming up to 1520 DEG C, electromagnetic agitation
45min, stand for standby use；
(2) copper liquid of step (1) is subjected to vacuum bottom pour mold casting, wherein vacuum pressure is 3*10-2Pa, after ingot casting cooling,
Remove casting pressing port, ingot casting surface cleaning is carried out using 6% SDS solution, is then placed in resistance-heated furnace and heats, heat
965 DEG C, soaking time 90min of temperature, hot forging is carried out after taking-up, until alloy size reaches preset value；
(3) wire drawing is carried out to the copper alloy of step (2), silk material is entered wire-drawing die using sub-cooled at wire-drawing die both ends
It is preceding and for equal fast cooling to -196 DEG C, low temperature wire drawing process is performed repeatedly until required silk material chi after wire-drawing die
It is very little；
(4) copper wire for obtaining step (3) carries out thermal annealing, and wherein thermal annealing temperatures are 400 DEG C, and the time is about 25 points
Clock；
(5) to 65 DEG C of drying of annealing copper wire of step (4), get product.
The performance test results of obtained high-strength highly-conductive copper wire are as shown in table 1.
Embodiment 1-4 and comparative example 1-2 obtained high-strength highly-conductive copper wire is subjected to resistivity, blowout current, ball respectively
Hardness and anti-this several performance tests of intensity of drawing.
Table 1
The preparation method of the high-strength highly-conductive copper wire of the present invention carries out high temperature roll milling to cathode copper, high-temperature pressurizing, adds antioxygen
Agent obtains compound copper liquid, and high-strength height is obtained using techniques such as vacuum casting, forged, sub-cooled wire drawing, annealing, cleaning, dryings
Lead copper wire.The high-strength highly-conductive copper wire being prepared, its copper wire quality is light, intensity is big, electric conductivity is high, before having preferably application
Scape.The high-strength highly-conductive copper wire raw material of the present invention is easy to get, technique is simple, is used suitable for heavy industrialization, practical.
Embodiments of the invention are the foregoing is only, are not intended to limit the scope of the invention, it is every to utilize this hair
The equivalent structure or equivalent flow conversion that bright description is made, or directly or indirectly it is used in other related technology necks
Domain, it is included within the scope of the present invention.
Claims (5)
1. a kind of preparation method of high-strength highly-conductive copper wire, it is characterised in that comprise the following steps：
(1) cathode copper is added in high-temperature roller furnace, is warming up to 1200-1260 DEG C, insulation fusing is complete, copper liquid is obtained, to copper
Inert gas is passed through in liquid, while adds antioxidant, then is warming up to 1500-1520 DEG C, electromagnetic agitation 30-45min, is stood standby
With；
(2) copper liquid of step (1) is subjected to vacuum bottom pour mold casting, after ingot casting cooling, removes casting pressing port, it is clear to carry out ingot casting surface
It is clean, it is then placed in resistance-heated furnace and heats, 950-965 DEG C of heating-up temperature, soaking time 60-90min, heat is carried out after taking-up
Forging, until alloy size reaches preset value；
(3) copper alloy of step (2) is carried out it is hot candied, made at wire-drawing die both ends using sub-cooled silk material enter before wire-drawing die and
To between -110 DEG C to -196 DEG C, low temperature wire drawing process is performed repeatedly until required equal fast cooling after wire-drawing die
Silk material size；
(4) copper wire for obtaining step (3) carries out thermal annealing, and wherein thermal annealing temperatures are 350-400 DEG C, and the time is about 15-
25 minutes；
(5) spend ionized water to the annealing copper wire of step (4) to be cleaned three times, then 65 DEG C of drying, get product.
2. the preparation method of high-strength highly-conductive copper wire according to claim 1, it is characterised in that anti-in the step (1)
Oxidant is selected from three (2.4- di-tert-butyl-phenyls) phosphite esters, four (β-(3,5- di-tert-butyl-hydroxy phenyl) propionic ester)
One or more in pentaerythritol ester, β-positive octadecanol ester of (3,5- di-tert-butyl-hydroxy phenyls) propionic acid.
3. the preparation method of high-strength highly-conductive copper wire according to claim 1, it is characterised in that lazy in the step (1)
Property gas is nitrogen.
4. the preparation method of high-strength highly-conductive copper wire according to claim 1, it is characterised in that true in the step (2)
Pneumatics is 2*10 by force-2-3*10-2Pa。
5. the preparation method of high-strength highly-conductive copper wire according to claim 1, it is characterised in that surface in the step (2)
Cleaning is specific to be carried out using 6% SDS solution.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109355527A (en) * | 2018-11-14 | 2019-02-19 | 世纪电缆有限公司 | A kind of preparation method of high-strength highly-conductive copper wire |
| CN113976656A (en) * | 2021-10-26 | 2022-01-28 | 江西云泰铜业有限公司 | Preparation method of high-strength bending-resistant copper wire |
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| CN104561642A (en) * | 2014-12-23 | 2015-04-29 | 中国兵器科学研究院宁波分院 | Ultrathin high-conductivity Cr-Zr-Cu wire and preparation method thereof |
| CN105177344A (en) * | 2015-07-30 | 2015-12-23 | 张连仲 | Cu-Fe alloy wire and preparing method thereof |
| CN105568193A (en) * | 2016-01-12 | 2016-05-11 | 天津理工大学 | Method for machining high-strength copper wire |
| CN106269970A (en) * | 2016-08-10 | 2017-01-04 | 安徽晋源铜业有限公司 | A kind of preparation technology of high-strength highly-conductive micro-wire |
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2017
- 2017-09-18 CN CN201710840503.3A patent/CN107557601A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104561642A (en) * | 2014-12-23 | 2015-04-29 | 中国兵器科学研究院宁波分院 | Ultrathin high-conductivity Cr-Zr-Cu wire and preparation method thereof |
| CN105177344A (en) * | 2015-07-30 | 2015-12-23 | 张连仲 | Cu-Fe alloy wire and preparing method thereof |
| CN105568193A (en) * | 2016-01-12 | 2016-05-11 | 天津理工大学 | Method for machining high-strength copper wire |
| CN106269970A (en) * | 2016-08-10 | 2017-01-04 | 安徽晋源铜业有限公司 | A kind of preparation technology of high-strength highly-conductive micro-wire |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109355527A (en) * | 2018-11-14 | 2019-02-19 | 世纪电缆有限公司 | A kind of preparation method of high-strength highly-conductive copper wire |
| CN113976656A (en) * | 2021-10-26 | 2022-01-28 | 江西云泰铜业有限公司 | Preparation method of high-strength bending-resistant copper wire |
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Application publication date: 20180109 |