CN110125209B - Production method for manufacturing copper wire - Google Patents
Production method for manufacturing copper wire Download PDFInfo
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- CN110125209B CN110125209B CN201810125964.7A CN201810125964A CN110125209B CN 110125209 B CN110125209 B CN 110125209B CN 201810125964 A CN201810125964 A CN 201810125964A CN 110125209 B CN110125209 B CN 110125209B
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- copper
- wire
- electrolytic copper
- copper wire
- manufacturing
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 245
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 58
- 229910052802 copper Inorganic materials 0.000 claims abstract description 173
- 239000010949 copper Substances 0.000 claims abstract description 173
- 230000007547 defect Effects 0.000 claims abstract description 61
- 238000010438 heat treatment Methods 0.000 claims abstract description 45
- 238000005491 wire drawing Methods 0.000 claims abstract description 32
- 238000005498 polishing Methods 0.000 claims abstract description 30
- 239000002994 raw material Substances 0.000 claims abstract description 22
- 238000000576 coating method Methods 0.000 claims abstract description 21
- 238000002791 soaking Methods 0.000 claims abstract description 12
- 238000005520 cutting process Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims description 38
- 238000001816 cooling Methods 0.000 claims description 32
- 239000010702 perfluoropolyether Substances 0.000 claims description 31
- 238000001125 extrusion Methods 0.000 claims description 30
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 21
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims description 21
- 239000011248 coating agent Substances 0.000 claims description 20
- 238000000280 densification Methods 0.000 claims description 20
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 20
- 230000010355 oscillation Effects 0.000 claims description 20
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 20
- -1 polydimethylsiloxane Polymers 0.000 claims description 20
- 238000007599 discharging Methods 0.000 claims description 10
- 238000007731 hot pressing Methods 0.000 claims description 10
- 239000003921 oil Substances 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 10
- 238000003825 pressing Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 230000032798 delamination Effects 0.000 claims description 6
- 229920005989 resin Polymers 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 10
- 239000010410 layer Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 238000005096 rolling process Methods 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000012797 qualification Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000010583 slow cooling Methods 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C37/00—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
- B21C37/04—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of bars or wire
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C9/00—Cooling, heating or lubricating drawing material
- B21C9/02—Selection of compositions therefor
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Metal Extraction Processes (AREA)
- Electrical Discharge Machining, Electrochemical Machining, And Combined Machining (AREA)
Abstract
The invention provides a production method for manufacturing copper wires, which comprises the steps of taking an electrolytic copper plate without a layering defect as a raw material, cutting the electrolytic copper plate into copper strips, processing the copper strips into copper rods, manufacturing round copper wires, polishing, phosphating coatings, soaking in a wire drawing protective solution, carrying out heat treatment, and finally drawing the copper wires by a wire drawing machine.
Description
Technical Field
The invention relates to the technical field of electric wires, in particular to a production method for manufacturing a copper wire.
Background
Copper (4N copper) with a purity of 99.99% or more belongs to the high-purity copper of the heroic sense, and ultra-high-purity copper (5N-7N) can be broadly called high-purity copper. High-purity copper wires made on the basis of generalized high-purity copper have very broad application prospects in electronic and electrical products as high-end electronic materials, for example: high-definition television signal wires, high-quality sound box wires, special enameled wires for electric automobile motors, targets for vacuum evaporation, copper strips for solar photovoltaics and the like. Compared with the conventional copper, the high-purity copper wire has higher purity and fewer crystal lattice defects and impurities, so that higher conductivity, better heat dissipation and better flexibility are endowed, and the characteristics of the high-purity copper wire, the low energy consumption and the high safety of the high-purity copper wire provide fundamental guarantee for high fidelity, low energy consumption and high safety of products.
However, the current high-purity copper wire has high production cost, and particularly, the product percent of pass of the copper wire with smaller diameter is low, so that the current market demand cannot be met. In addition, copper has poorer extensibility than gold, and the extensibility is generally improved by doping gold, which undoubtedly increases the production cost.
Disclosure of Invention
The invention aims to provide a production method for manufacturing a copper wire, which has excellent extensibility and high product qualification rate.
In order to achieve the purpose, the invention is realized by the following scheme:
a production method for manufacturing a copper wire comprises the following specific steps:
(1) taking an electrolytic copper plate without a layering defect as a raw material, cutting the electrolytic copper plate into copper strips, processing the copper strips into copper rods with circular sections, and then manufacturing a disc-shaped copper wire for later use;
(2) preparing a drawing protection solution: dissolving polyethylene glycol 400 in absolute ethyl alcohol, adding polyvinyl butyral, and fully stirring until the polyvinyl butyral is completely dissolved to obtain a first solution; heating perfluoropolyether to 70-80 ℃, adding the first solution and polydimethylsiloxane, and carrying out ultrasonic oscillation for 20-30 minutes to obtain the perfluoropolyether resin;
(3) and (2) polishing the wire rod of the wire rod obtained in the step (1), phosphating a coating, soaking in the wire drawing protection solution obtained in the step (2), performing ultrasonic oscillation treatment for 2-3 hours, taking out, performing heating-first and cooling-second heat treatment, and finally drawing by using a wire drawing machine to obtain the copper wire.
Preferably, in the step (1), the electrolytic copper plate is sorted to sort out the electrolytic copper plate without delamination defect and the electrolytic copper plate with delamination defect, the electrolytic copper plate is directly used as a raw material, and the former is subjected to tissue densification treatment to eliminate the delamination defect.
Further preferably, the specific method of the tissue densification treatment is as follows: and (3) placing the electrolytic copper plate with the layering defect in a vacuum hot-pressing sintering furnace, applying pressure of 30-40 MPa to the front surface and the back surface of the electrolytic copper plate, preserving heat for 20-30 minutes at 900-1000 ℃ under a vacuum condition, naturally cooling to below 60 ℃, and discharging.
Preferably, in the step (1), the copper bar is repeatedly subjected to swaging or swaging to form the copper rod with a circular cross section.
Preferably, in the step (1), after the copper rods are subjected to surface oxide layer removal, oil removal and deburring treatment, the copper rods are firmly welded into a whole in an extrusion cavity of a continuous extruder through continuous feeding in the extrusion cavity of the continuous extruder, and the disc-shaped copper wire rod is obtained at an extrusion die outlet of the extruder.
Preferably, in the step (2), the mass ratio of the perfluoropolyether to the polydimethylsiloxane to the polyvinyl butyral to the polyethylene glycol 400 to the absolute ethyl alcohol is 1: 0.5-0.6: 0.1-0.2: 0.3-0.4: 2 to 3.
Preferably, in the step (3), the disc-shaped copper wire is polished by a polishing machine.
Preferably, in the step (3), the process conditions of the phosphating coating are as follows: the phosphating temperature is 60-70 ℃, the phosphating time is 20-30 minutes, the total acidity is 50-60 points, and the free acidity is 5-8 points.
Preferably, in the step (3), the specific method of the heat treatment is: raising the temperature to 400-450 ℃ at a speed of 5-8 ℃/min, then preserving the heat for 2-3 hours, then reducing the temperature to 200-300 ℃ at a speed of 2-4 ℃/min, preserving the heat for 50-80 minutes, and naturally cooling.
The invention has the beneficial effects that:
1. the invention uses the electrolytic copper plate without the layering defect as the raw material, cuts the electrolytic copper plate into copper strips, processes the copper strips into copper rods, then produces the disc copper wire, polishes, coats, uses the wiredrawing protective solution to soak, heat treats, and finally draws the copper wire by the wiredrawing machine, and the invention has the advantages of excellent extensibility and high product qualification rate.
2. Disc circle copper wire rod reduces roughness through the polishing, helps the formation of bonderizing coating, the bonderizing membrane of formation is porous structure, wire drawing protection liquid soaking treatment can promote each component of wire drawing protection liquid fully to fill porous structure in, through the heat treatment of follow-up earlier cooling after rising temperature, can promote the abundant integration of wire drawing protection liquid and bonderizing membrane, to the surface formation protective layer of disc circle copper wire rod, avoid the wire drawing in-process fracture to appear, improve the product percent of pass, improve the extensibility simultaneously.
3. The wire drawing protection solution is prepared from perfluoropolyether, polydimethylsiloxane, polyethylene glycol 400, polyvinyl butyral and absolute ethyl alcohol, and a lubricating component is added, so that the wire drawing protection solution can effectively protect a coiled copper wire and prevent processing damage.
4. The heat treatment of first heating and then cooling is carried out by paying attention to rapid heating and slow cooling, and the protection effect is influenced by too slow heating or too fast cooling.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A production method for manufacturing a copper wire comprises the following specific steps:
(1) taking an electrolytic copper plate without a layering defect as a raw material, cutting the electrolytic copper plate into copper strips, processing the copper strips into copper rods with circular sections, and then manufacturing a disc-shaped copper wire for later use;
(2) preparing a drawing protection solution: dissolving polyethylene glycol 400 in absolute ethyl alcohol, adding polyvinyl butyral, and fully stirring until the polyvinyl butyral is completely dissolved to obtain a first solution; heating perfluoropolyether to 70 ℃, adding the first solution and polydimethylsiloxane, and carrying out ultrasonic oscillation for 20 minutes to obtain the perfluoropolyether;
(3) and (2) polishing the wire rod of the wire rod obtained in the step (1), phosphating a coating, soaking in the wire drawing protection solution obtained in the step (2), performing ultrasonic oscillation treatment for 2 hours, taking out, performing heating-first and cooling-second heat treatment, and finally drawing by using a wire drawing machine to obtain the copper wire.
In the step (1), the electrolytic copper plates are sorted, the electrolytic copper plates without the layering defect and with the layering defect are sorted, the electrolytic copper plates with the layering defect are directly used as raw materials, and the electrolytic copper plates are subjected to tissue densification treatment to eliminate the layering defect. The specific method of the tissue densification treatment comprises the following steps: and (3) placing the electrolytic copper plate with the layering defect in a vacuum hot-pressing sintering furnace, applying pressure of 30MPa to the front surface and the back surface of the electrolytic copper plate, preserving heat for 20 minutes at 900 ℃ under a vacuum condition, naturally cooling to below 60 ℃, and discharging.
In the step (1), the copper bar is repeatedly subjected to shape rolling or rotary swaging processing to manufacture the copper bar with the circular section.
In the step (1), after the surface of the copper rod is subjected to oxide layer removal, oil removal and deburring treatment, the copper rod is firmly welded into a whole in an extrusion cavity of a continuous extruder by continuously feeding materials into the extrusion cavity of the continuous extruder, and a disc-shaped copper wire rod is obtained at an extrusion die outlet of the extruder.
In the step (2), the mass ratio of the perfluoropolyether, the polydimethylsiloxane, the polyvinyl butyral, the polyethylene glycol 400 and the absolute ethyl alcohol is 1: 0.5: 0.1: 0.3: 2.
and (3) polishing the disc-shaped copper wire by using a polishing machine.
In the step (3), the process conditions of the phosphating coating are as follows: the phosphorization temperature is 60 ℃, the phosphorization time is 20 minutes, the total acidity is 50 points, and the free acidity is 5 points.
In the step (3), the specific method of the heat treatment is as follows: raising the temperature to 400 ℃ at the speed of 5 ℃/minute, then preserving the heat for 2 hours, then reducing the temperature to 200 ℃ at the speed of 2 ℃/minute, preserving the heat for 50 minutes, and naturally cooling.
Example 2
A production method for manufacturing a copper wire comprises the following specific steps:
(1) taking an electrolytic copper plate without a layering defect as a raw material, cutting the electrolytic copper plate into copper strips, processing the copper strips into copper rods with circular sections, and then manufacturing a disc-shaped copper wire for later use;
(2) preparing a drawing protection solution: dissolving polyethylene glycol 400 in absolute ethyl alcohol, adding polyvinyl butyral, and fully stirring until the polyvinyl butyral is completely dissolved to obtain a first solution; heating perfluoropolyether to 80 ℃, adding the first solution and polydimethylsiloxane, and carrying out ultrasonic oscillation for 30 minutes to obtain the perfluoropolyether;
(3) and (2) polishing the wire rod of the wire rod obtained in the step (1), phosphating a coating, soaking in the wire drawing protection solution obtained in the step (2), performing ultrasonic oscillation treatment for 3 hours, taking out, performing heating-first and cooling-second heat treatment, and finally drawing by using a wire drawing machine to obtain the copper wire.
In the step (1), the electrolytic copper plates are sorted, the electrolytic copper plates without the layering defect and with the layering defect are sorted, the electrolytic copper plates with the layering defect are directly used as raw materials, and the electrolytic copper plates are subjected to tissue densification treatment to eliminate the layering defect. The specific method of the tissue densification treatment comprises the following steps: and (3) placing the electrolytic copper plate with the layering defect in a vacuum hot-pressing sintering furnace, applying 40MPa pressure to the front surface and the back surface of the electrolytic copper plate, preserving the heat for 30 minutes at 1000 ℃ under the vacuum condition, naturally cooling to below 60 ℃, and discharging.
In the step (1), the copper bar is repeatedly subjected to shape rolling or rotary swaging processing to manufacture the copper bar with the circular section.
In the step (1), after the surface of the copper rod is subjected to oxide layer removal, oil removal and deburring treatment, the copper rod is firmly welded into a whole in an extrusion cavity of a continuous extruder by continuously feeding materials into the extrusion cavity of the continuous extruder, and a disc-shaped copper wire rod is obtained at an extrusion die outlet of the extruder.
In the step (2), the mass ratio of the perfluoropolyether, the polydimethylsiloxane, the polyvinyl butyral, the polyethylene glycol 400 and the absolute ethyl alcohol is 1: 0.6: 0.2: 0.4: 3.
And (3) polishing the disc-shaped copper wire by using a polishing machine.
In the step (3), the process conditions of the phosphating coating are as follows: the phosphating temperature is 70 ℃, the phosphating time is 30 minutes, the total acidity is 60 points, and the free acidity is 8 points.
In the step (3), the specific method of the heat treatment is as follows: heating to 450 ℃ at the speed of 8 ℃/min, preserving heat for 3 hours, then cooling to 300 ℃ at the speed of 4 ℃/min, preserving heat for 80 minutes, and naturally cooling.
Example 3
A production method for manufacturing a copper wire comprises the following specific steps:
(1) taking an electrolytic copper plate without a layering defect as a raw material, cutting the electrolytic copper plate into copper strips, processing the copper strips into copper rods with circular sections, and then manufacturing a disc-shaped copper wire for later use;
(2) preparing a drawing protection solution: dissolving polyethylene glycol 400 in absolute ethyl alcohol, adding polyvinyl butyral, and fully stirring until the polyvinyl butyral is completely dissolved to obtain a first solution; heating perfluoropolyether to 70 ℃, adding the first solution and polydimethylsiloxane, and carrying out ultrasonic oscillation for 30 minutes to obtain the perfluoropolyether;
(3) and (2) polishing the wire rod of the wire rod obtained in the step (1), phosphating a coating, soaking in the wire drawing protection solution obtained in the step (2), performing ultrasonic oscillation treatment for 2 hours, taking out, performing heating-first and cooling-second heat treatment, and finally drawing by using a wire drawing machine to obtain the copper wire.
In the step (1), the electrolytic copper plates are sorted, the electrolytic copper plates without the layering defect and with the layering defect are sorted, the electrolytic copper plates with the layering defect are directly used as raw materials, and the electrolytic copper plates are subjected to tissue densification treatment to eliminate the layering defect. The specific method of the tissue densification treatment comprises the following steps: and (3) placing the electrolytic copper plate with the layering defect in a vacuum hot-pressing sintering furnace, applying pressure of 40MPa to the front surface and the back surface of the electrolytic copper plate, preserving heat for 30 minutes at 900 ℃ under a vacuum condition, naturally cooling to below 60 ℃, and discharging.
In the step (1), the copper bar is repeatedly subjected to shape rolling or rotary swaging processing to manufacture the copper bar with the circular section.
In the step (1), after the surface of the copper rod is subjected to oxide layer removal, oil removal and deburring treatment, the copper rod is firmly welded into a whole in an extrusion cavity of a continuous extruder by continuously feeding materials into the extrusion cavity of the continuous extruder, and a disc-shaped copper wire rod is obtained at an extrusion die outlet of the extruder.
In the step (2), the mass ratio of the perfluoropolyether, the polydimethylsiloxane, the polyvinyl butyral, the polyethylene glycol 400 and the absolute ethyl alcohol is 1: 0.5: 0.2: 0.3: 3.
And (3) polishing the disc-shaped copper wire by using a polishing machine.
In the step (3), the process conditions of the phosphating coating are as follows: the phosphorization temperature is 60 ℃, the phosphorization time is 30 minutes, the total acidity is 50 points, and the free acidity is 8 points.
In the step (3), the specific method of the heat treatment is as follows: heating to 450 deg.C at 5 deg.C/min, holding for 2 hr, cooling to 200 deg.C at 4 deg.C/min, holding for 80 min, and naturally cooling.
Example 4
A production method for manufacturing a copper wire comprises the following specific steps:
(1) taking an electrolytic copper plate without a layering defect as a raw material, cutting the electrolytic copper plate into copper strips, processing the copper strips into copper rods with circular sections, and then manufacturing a disc-shaped copper wire for later use;
(2) preparing a drawing protection solution: dissolving polyethylene glycol 400 in absolute ethyl alcohol, adding polyvinyl butyral, and fully stirring until the polyvinyl butyral is completely dissolved to obtain a first solution; heating perfluoropolyether to 80 ℃, adding the first solution and polydimethylsiloxane, and carrying out ultrasonic oscillation for 20 minutes to obtain the perfluoropolyether;
(3) and (2) polishing the wire rod of the wire rod obtained in the step (1), phosphating a coating, soaking in the wire drawing protection solution obtained in the step (2), performing ultrasonic oscillation treatment for 3 hours, taking out, performing heating-first and cooling-second heat treatment, and finally drawing by using a wire drawing machine to obtain the copper wire.
In the step (1), the electrolytic copper plates are sorted, the electrolytic copper plates without the layering defect and with the layering defect are sorted, the electrolytic copper plates with the layering defect are directly used as raw materials, and the electrolytic copper plates are subjected to tissue densification treatment to eliminate the layering defect. The specific method of the tissue densification treatment comprises the following steps: and (3) placing the electrolytic copper plate with the layering defect in a vacuum hot-pressing sintering furnace, applying pressure of 30MPa to the front surface and the back surface of the electrolytic copper plate, preserving heat for 20 minutes at 1000 ℃ under a vacuum condition, naturally cooling to below 60 ℃, and discharging.
In the step (1), the copper bar is repeatedly subjected to shape rolling or rotary swaging processing to manufacture the copper bar with the circular section.
In the step (1), after the surface of the copper rod is subjected to oxide layer removal, oil removal and deburring treatment, the copper rod is firmly welded into a whole in an extrusion cavity of a continuous extruder by continuously feeding materials into the extrusion cavity of the continuous extruder, and a disc-shaped copper wire rod is obtained at an extrusion die outlet of the extruder.
In the step (2), the mass ratio of the perfluoropolyether, the polydimethylsiloxane, the polyvinyl butyral, the polyethylene glycol 400 and the absolute ethyl alcohol is 1: 0.6: 0.1: 0.4: 2.
and (3) polishing the disc-shaped copper wire by using a polishing machine.
In the step (3), the process conditions of the phosphating coating are as follows: the phosphating temperature is 70 ℃, the phosphating time is 20 minutes, the total acidity is 60 points, and the free acidity is 5 points.
In the step (3), the specific method of the heat treatment is as follows: heating to 400 ℃ at the speed of 8 ℃/min, then preserving heat for 3 hours, then cooling to 300 ℃ at the speed of 2 ℃/min, preserving heat for 50 minutes, and naturally cooling.
Example 5
A production method for manufacturing a copper wire comprises the following specific steps:
(1) taking an electrolytic copper plate without a layering defect as a raw material, cutting the electrolytic copper plate into copper strips, processing the copper strips into copper rods with circular sections, and then manufacturing a disc-shaped copper wire for later use;
(2) preparing a drawing protection solution: dissolving polyethylene glycol 400 in absolute ethyl alcohol, adding polyvinyl butyral, and fully stirring until the polyvinyl butyral is completely dissolved to obtain a first solution; heating perfluoropolyether to 75 ℃, adding the first solution and polydimethylsiloxane, and carrying out ultrasonic oscillation for 25 minutes to obtain the perfluoropolyether;
(3) and (2) polishing the wire rod of the wire rod obtained in the step (1), phosphating a coating, soaking in the wire drawing protection solution obtained in the step (2), performing ultrasonic oscillation treatment for 2 hours, taking out, performing heating-first and cooling-second heat treatment, and finally drawing by using a wire drawing machine to obtain the copper wire.
In the step (1), the electrolytic copper plates are sorted, the electrolytic copper plates without the layering defect and with the layering defect are sorted, the electrolytic copper plates with the layering defect are directly used as raw materials, and the electrolytic copper plates are subjected to tissue densification treatment to eliminate the layering defect. The specific method of the tissue densification treatment comprises the following steps: and (3) placing the electrolytic copper plate with the layering defect in a vacuum hot-pressing sintering furnace, applying pressure of 35MPa to the front surface and the back surface of the electrolytic copper plate, preserving heat for 25 minutes at 950 ℃ under a vacuum condition, naturally cooling to below 60 ℃, and discharging.
In the step (1), the copper bar is repeatedly subjected to shape rolling or rotary swaging processing to manufacture the copper bar with the circular section.
In the step (1), after the surface of the copper rod is subjected to oxide layer removal, oil removal and deburring treatment, the copper rod is firmly welded into a whole in an extrusion cavity of a continuous extruder by continuously feeding materials into the extrusion cavity of the continuous extruder, and a disc-shaped copper wire rod is obtained at an extrusion die outlet of the extruder.
In the step (2), the mass ratio of the perfluoropolyether, the polydimethylsiloxane, the polyvinyl butyral, the polyethylene glycol 400 and the absolute ethyl alcohol is 1: 0.55: 0.15: 0.35: 2.5.
and (3) polishing the disc-shaped copper wire by using a polishing machine.
In the step (3), the process conditions of the phosphating coating are as follows: the phosphorization temperature is 65 ℃, the phosphorization time is 25 minutes, the total acidity is 50 points, and the free acidity is 6 points.
In the step (3), the specific method of the heat treatment is as follows: heating to 420 ℃ at the speed of 6 ℃/min, then preserving heat for 2.5 hours, then cooling to 250 ℃ at the speed of 3 ℃/min, preserving heat for 70 minutes, and naturally cooling.
Comparative example 1
A production method for manufacturing a copper wire comprises the following specific steps:
(1) taking an electrolytic copper plate without a layering defect as a raw material, cutting the electrolytic copper plate into copper strips, processing the copper strips into copper rods with circular sections, and then manufacturing a disc-shaped copper wire for later use;
(2) preparing a drawing protection solution: dissolving polyethylene glycol 400 in absolute ethyl alcohol to obtain a first solution; heating perfluoropolyether to 75 ℃, adding the first solution and polydimethylsiloxane, and carrying out ultrasonic oscillation for 25 minutes to obtain the perfluoropolyether;
(3) and (2) polishing the wire rod of the wire rod obtained in the step (1), phosphating a coating, soaking in the wire drawing protection solution obtained in the step (2), performing ultrasonic oscillation treatment for 2 hours, taking out, performing heating-first and cooling-second heat treatment, and finally drawing by using a wire drawing machine to obtain the copper wire.
In the step (1), the electrolytic copper plates are sorted, the electrolytic copper plates without the layering defect and with the layering defect are sorted, the electrolytic copper plates with the layering defect are directly used as raw materials, and the electrolytic copper plates are subjected to tissue densification treatment to eliminate the layering defect. The specific method of the tissue densification treatment comprises the following steps: and (3) placing the electrolytic copper plate with the layering defect in a vacuum hot-pressing sintering furnace, applying pressure of 35MPa to the front surface and the back surface of the electrolytic copper plate, preserving heat for 25 minutes at 950 ℃ under a vacuum condition, naturally cooling to below 60 ℃, and discharging.
In the step (1), the copper bar is repeatedly subjected to shape rolling or rotary swaging processing to manufacture the copper bar with the circular section.
In the step (1), after the surface of the copper rod is subjected to oxide layer removal, oil removal and deburring treatment, the copper rod is firmly welded into a whole in an extrusion cavity of a continuous extruder by continuously feeding materials into the extrusion cavity of the continuous extruder, and a disc-shaped copper wire rod is obtained at an extrusion die outlet of the extruder.
In the step (2), the mass ratio of the perfluoropolyether, the polydimethylsiloxane, the polyethylene glycol 400 and the absolute ethyl alcohol is 1: 0.55: 0.35: 2.5.
and (3) polishing the disc-shaped copper wire by using a polishing machine.
In the step (3), the process conditions of the phosphating coating are as follows: the phosphorization temperature is 65 ℃, the phosphorization time is 25 minutes, the total acidity is 50 points, and the free acidity is 6 points.
In the step (3), the specific method of the heat treatment is as follows: heating to 420 ℃ at the speed of 6 ℃/min, then preserving heat for 2.5 hours, then cooling to 250 ℃ at the speed of 3 ℃/min, preserving heat for 70 minutes, and naturally cooling.
Comparative example 2
A production method for manufacturing a copper wire comprises the following specific steps:
(1) taking an electrolytic copper plate without a layering defect as a raw material, cutting the electrolytic copper plate into copper strips, processing the copper strips into copper rods with circular sections, and then manufacturing a disc-shaped copper wire for later use;
(2) preparing a drawing protection solution: dissolving polyethylene glycol 400 in absolute ethyl alcohol, adding polyvinyl butyral, and fully stirring until the polyvinyl butyral is completely dissolved to obtain a first solution; heating perfluoropolyether to 75 ℃, adding the first solution, and performing ultrasonic oscillation for 25 minutes to obtain the perfluoropolyether;
(3) and (2) polishing the wire rod of the wire rod obtained in the step (1), phosphating a coating, soaking in the wire drawing protection solution obtained in the step (2), performing ultrasonic oscillation treatment for 2 hours, taking out, performing heating-first and cooling-second heat treatment, and finally drawing by using a wire drawing machine to obtain the copper wire.
In the step (1), the electrolytic copper plates are sorted, the electrolytic copper plates without the layering defect and with the layering defect are sorted, the electrolytic copper plates with the layering defect are directly used as raw materials, and the electrolytic copper plates are subjected to tissue densification treatment to eliminate the layering defect. The specific method of the tissue densification treatment comprises the following steps: and (3) placing the electrolytic copper plate with the layering defect in a vacuum hot-pressing sintering furnace, applying pressure of 35MPa to the front surface and the back surface of the electrolytic copper plate, preserving heat for 25 minutes at 950 ℃ under a vacuum condition, naturally cooling to below 60 ℃, and discharging.
In the step (1), the copper bar is repeatedly subjected to shape rolling or rotary swaging processing to manufacture the copper bar with the circular section.
In the step (1), after the surface of the copper rod is subjected to oxide layer removal, oil removal and deburring treatment, the copper rod is firmly welded into a whole in an extrusion cavity of a continuous extruder by continuously feeding materials into the extrusion cavity of the continuous extruder, and a disc-shaped copper wire rod is obtained at an extrusion die outlet of the extruder.
In the step (2), the mass ratio of the perfluoropolyether to the polyvinyl butyral to the polyethylene glycol 400 to the absolute ethyl alcohol is 1: 0.15: 0.35: 2.5.
and (3) polishing the disc-shaped copper wire by using a polishing machine.
In the step (3), the process conditions of the phosphating coating are as follows: the phosphorization temperature is 65 ℃, the phosphorization time is 25 minutes, the total acidity is 50 points, and the free acidity is 6 points.
In the step (3), the specific method of the heat treatment is as follows: heating to 420 ℃ at the speed of 6 ℃/min, then preserving heat for 2.5 hours, then cooling to 250 ℃ at the speed of 3 ℃/min, preserving heat for 70 minutes, and naturally cooling.
Comparative example 3
A production method for manufacturing a copper wire comprises the following specific steps:
(1) taking an electrolytic copper plate without a layering defect as a raw material, cutting the electrolytic copper plate into copper strips, processing the copper strips into copper rods with circular sections, and then manufacturing a disc-shaped copper wire for later use;
(2) preparing a drawing protection solution: dissolving polyethylene glycol 400 in absolute ethyl alcohol, adding polyvinyl butyral, and fully stirring until the polyvinyl butyral is completely dissolved to obtain a first solution; heating perfluoropolyether to 75 ℃, adding the first solution and polydimethylsiloxane, and carrying out ultrasonic oscillation for 25 minutes to obtain the perfluoropolyether;
(3) polishing the wire rod of the wire rod obtained in the step (1), soaking the wire rod in the wire drawing protection solution obtained in the step (2), performing ultrasonic oscillation treatment for 2 hours, taking out the wire rod, performing heating treatment and cooling heat treatment, and finally drawing the wire rod by using a wire drawing machine to obtain the copper wire.
In the step (1), the electrolytic copper plates are sorted, the electrolytic copper plates without the layering defect and with the layering defect are sorted, the electrolytic copper plates with the layering defect are directly used as raw materials, and the electrolytic copper plates are subjected to tissue densification treatment to eliminate the layering defect. The specific method of the tissue densification treatment comprises the following steps: and (3) placing the electrolytic copper plate with the layering defect in a vacuum hot-pressing sintering furnace, applying pressure of 35MPa to the front surface and the back surface of the electrolytic copper plate, preserving heat for 25 minutes at 950 ℃ under a vacuum condition, naturally cooling to below 60 ℃, and discharging.
In the step (1), the copper bar is repeatedly subjected to shape rolling or rotary swaging processing to manufacture the copper bar with the circular section.
In the step (1), after the surface of the copper rod is subjected to oxide layer removal, oil removal and deburring treatment, the copper rod is firmly welded into a whole in an extrusion cavity of a continuous extruder by continuously feeding materials into the extrusion cavity of the continuous extruder, and a disc-shaped copper wire rod is obtained at an extrusion die outlet of the extruder.
In the step (2), the mass ratio of the perfluoropolyether, the polydimethylsiloxane, the polyvinyl butyral, the polyethylene glycol 400 and the absolute ethyl alcohol is 1: 0.55: 0.15: 0.35: 2.5.
and (3) polishing the disc-shaped copper wire by using a polishing machine.
In the step (3), the specific method of the heat treatment is as follows: heating to 420 ℃ at the speed of 6 ℃/min, then preserving heat for 2.5 hours, then cooling to 250 ℃ at the speed of 3 ℃/min, preserving heat for 70 minutes, and naturally cooling.
Test examples
The yield of copper wire (15 μm) produced by the production methods of examples 1 to 5 and comparative examples 1 to 3 was examined (the resistivity of pure copper at 25 ℃ C. was 0.0172 μ Ω. m, and the measured resistivity was not more than 1% above or below, and was regarded as being acceptable), and the mechanical properties of the copper wire (average value of multiple lots) were measured, and the results are shown in Table 1.
TABLE 1 comparison of percent of pass and mechanical Properties of copper wire
| Percent pass (%) | Elongation (%) | Breaking load (g) | |
| Example 1 | ≥99.8 | 18.3 | 22.4 |
| Example 2 | ≥99.8 | 18.4 | 22.4 |
| Example 3 | ≥99.8 | 18.5 | 22.5 |
| Example 4 | ≥99.8 | 18.5 | 22.6 |
| Example 5 | ≥99.8 | 18.5 | 22.8 |
| Comparative example 1 | 92.3 | 9.2 | 14.3 |
| Comparative example 2 | 91.8 | 9.1 | 14.2 |
| Comparative example 3 | 94.1 | 11.3 | 16.5 |
As can be seen from Table 1, the copper wires of examples 1 to 5 had good elongation, good mechanical properties, and high product yield. The polyvinyl butyral in the wire drawing protection solution is omitted in the comparative example 1, the polydimethylsiloxane in the wire drawing protection solution is omitted in the comparative example 2, the phosphating coating treatment is not carried out in the comparative example 3, the product percent of pass is low, and the elongation rate is obviously poor.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (7)
1. A production method for manufacturing a copper wire is characterized by comprising the following specific steps:
(1) taking an electrolytic copper plate without a layering defect as a raw material, cutting the electrolytic copper plate into copper strips, processing the copper strips into copper rods with circular sections, and then manufacturing a disc-shaped copper wire for later use;
(2) preparing a drawing protection solution: dissolving polyethylene glycol 400 in absolute ethyl alcohol, adding polyvinyl butyral, and fully stirring until the polyvinyl butyral is completely dissolved to obtain a first solution; heating perfluoropolyether to 70-80 ℃, adding the first solution and polydimethylsiloxane, and carrying out ultrasonic oscillation for 20-30 minutes to obtain the perfluoropolyether resin;
the mass ratio of the perfluoropolyether to the polydimethylsiloxane to the polyvinyl butyral to the polyethylene glycol 400 to the absolute ethyl alcohol is 1: 0.5-0.6: 0.1-0.2: 0.3-0.4: 2-3;
(3) polishing the wire rod of the wire rod obtained in the step (1), phosphorizing a coating, soaking the wire rod of the wire rod in the wire drawing protection solution obtained in the step (2), performing ultrasonic oscillation treatment for 2-3 hours, taking out the wire rod, performing heating and cooling heat treatment, and finally drawing the wire rod by using a wire drawing machine to obtain a copper wire;
the process conditions of the phosphating coating are as follows: the phosphating temperature is 60-70 ℃, the phosphating time is 20-30 minutes, the total acidity is 50-60 points, and the free acidity is 5-8 points.
2. The method as claimed in claim 1, wherein the electrolytic copper sheets are sorted in step (1) to sort out the electrolytic copper sheets having no delamination defect as a raw material and having a delamination defect, and the former is subjected to a structure densification treatment to eliminate the delamination defect.
3. The method for manufacturing copper wire according to claim 2, wherein the specific method of the structure densification process is: and (3) placing the electrolytic copper plate with the layering defect in a vacuum hot-pressing sintering furnace, applying pressure of 30-40 MPa to the front surface and the back surface of the electrolytic copper plate, preserving heat for 20-30 minutes at 900-1000 ℃ under a vacuum condition, naturally cooling to below 60 ℃, and discharging.
4. The method for manufacturing copper wire according to claim 1, wherein in the step (1), the copper bar is repeatedly subjected to the swaging process to manufacture the copper bar with a circular cross section.
5. The production method of copper wire according to any one of claims 1 to 4, wherein in step (1), the copper rod is subjected to surface oxide layer removal, oil removal and deburring treatment, and then is subjected to continuous and uninterrupted feeding into an extrusion cavity of a continuous extruder, so that the copper rods are firmly welded into a whole in the extrusion cavity, and a coiled copper wire is obtained at the outlet of an extrusion die of the extruder.
6. The method for manufacturing copper wire according to claim 1, wherein in the step (3), the disc-shaped copper wire is polished by a polishing machine.
7. The method for manufacturing copper wire according to claim 1, wherein in step (3), the heat treatment is performed by the following specific method: raising the temperature to 400-450 ℃ at a speed of 5-8 ℃/min, then preserving the heat for 2-3 hours, then reducing the temperature to 200-300 ℃ at a speed of 2-4 ℃/min, preserving the heat for 50-80 minutes, and naturally cooling.
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