CN102324276A - Production process of copper coated aluminum-magnesium bimetallic conductor - Google Patents
Production process of copper coated aluminum-magnesium bimetallic conductor Download PDFInfo
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- CN102324276A CN102324276A CN201110149485A CN201110149485A CN102324276A CN 102324276 A CN102324276 A CN 102324276A CN 201110149485 A CN201110149485 A CN 201110149485A CN 201110149485 A CN201110149485 A CN 201110149485A CN 102324276 A CN102324276 A CN 102324276A
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Abstract
The invention relates to the technical field of metal conductor processing, in particular to a production process of a copper coated aluminum-magnesium bimetallic conductor, solving the technical problems of unreasonable prior art and the like. The production process comprises the following steps of: A, surface preprocessing; B, zinc deposit preprocessing; C, cyanogens-free nickel preplating; D, silicate copper plating; and E, postprocessing. The production process of the copper coated aluminum-magnesium bimetallic conductor has the advantages that: 1, the surface activity of an aluminum-magnesium alloy is better regulated, operation quality in a subsequence electroplating process and stability in a drawing process are ensured; 2, the problem of broken wires of electroplating intermediate products in a subsequent drawing process is solved, yield of final products is increased; and 3, electroplating is carried out by adopting a pulse modulation power supply, a microstructure of electrocrystallization copper is improved, compactness of a copper coating is improved, and hydrogen evolution side reaction is inhibited.
Description
Technical field
The present invention relates to the plain conductor processing technique field, especially relate to a kind of aluminium in copper magnesium bimetallic conductor production technology.
Background technology
The development of wires and cables industry be unable to do without electric conducting materials such as copper, aluminium.Copper has good electric property, is traditional electric conducting material, and the electric wire copper consumption accounts for 60～70% of national copper consumption figure, but improving constantly of the scarcity of copper resource and the market price impels cable industry actively to seek substitute material.The aluminium in copper magnesium bimetallic conductor is a kind of bimetallic conductor that on the almag heart yearn, coats one deck certain thickness fine copper with one heart.Guaranteeing both to have had the excellent conductive capability of copper under the prerequisite of serviceability, having the characteristics such as light weight, softness of aluminium again, is the optimal material of instead of pure copper cash as conductor.The advantage of copper-clad aluminum conductor mainly shows as: 1. conduct electricity very well, its dc resistivity is 1.5 times of pure copper wire, and when resistance was identical, copper-clad aluminum conductor weight was about 1/2 of pure copper wire.Calculate according to " skin effect ", when the above high frequency of 5MHZ, resistivity is identical with pure copper wire.2. good weldability because the copper-clad aluminum conductor surface has coated one deck fine copper with one heart, therefore has with the same solderability of pure copper wire.3. light weight, its proportion is merely 30%～32% of pure copper wire, and under the situation that online footpath, quality equate, its length is 2.5 times of pure copper wire, greatly reduces production cost thus.4. because in light weight, the sag degree is little, is more suitable in physical blowing high frequency cable production technology, guarantees concentricity.5. bending property is better than pure copper wire, can reduce the impedance variations that causes because of bending radius is little.6. can overcome with aluminum pipe and make cable that outer conductor, pure copper wire make inner wire under the too big situation of variations in temperature, the phenomenon with connector " uncoupling " because the cable core that both linear expansion coefficient differences cause " is loosed core ".
Galvanoplastic are traditional bimetallic composite wire rod production technologies, because the aluminum-magnesium alloy wire surface very easily forms oxide-film, copper plate is of poor quality, and adhesion is not firm, can't satisfy the demand of wires and cables industry, can't form industrialization always.In recent years, along with the copper material price sharp rises, stepping up to study the method for practicing thrift the copper resource more in the world.The beginning of this century, Germany develops hydrochlorate electrocoppering new technology, and copperizing continuously on aluminum-magnesium alloy wire is then through drawing the skill of exchanging work to obtain the copper cladding aluminum conductor in required line footpath.This technology has solved low, the deficiency such as fine and close, in uneven thickness inadequately of the coating adhesion that common copper-plating technique exists, and the comparable mechanical coating method of copper material consumption descends 20%, energy consumption decline 25%, and electric property is more excellent.This technology reaches a standard at present basically, is beginning suitability for industrialized production.But what the hydrochlorate copper-plating method new technology of Germany adopted is full-automatic electromechanical integration production line, and its technical equipment is very expensive, and a production line price is up to more than 150 ten thousand, and production cost is also higher.
Tradition is electroplated in the manufactured aluminium in copper magnesium bimetallic conductor technology and is had significantly weak point; What have shows the production environment aspect, has adopted the cyanide pre-plating copper method in the coating bottoming technology behind the red cigarette of more nitrogen oxide, the heavy zinc and has produced serious cyanogen and pollute as having produced in the almag bar scale removal pre-treating technology.What have shows on the product inherent quality index, like the copper coating fault-layer-phenomenon that occurs on the aluminium substrate, the finished product composite wire hydrogen embrittlement fracture phenomenon that the cathode hydrogen evolution side reaction causes.What have also shows on the production run efficient, is provided with etc. like the walking speed of almag bar in the layout quantity of almag bar in the electrolysis tank, the continuous electroplating.Totally see, mainly contain following aspect technical problem in the present conventional electroplating technology: 2, copper, aluminium interfacial structure are difficult to control; 1, the environmental hazard that brings of technology such as cyanide preplating copper; 3, product hydrogen embrittlement problem; 4, the recycled problem that removes and handle the back plating bath of foreign metal ion in the treatment media.
Summary of the invention
The objective of the invention is provides a kind of easy to implement, low in the pollution of the environment, the aluminium in copper magnesium bimetallic conductor production technology that product quality is high to the problems referred to above.
For achieving the above object, the present invention has adopted following technical proposal: this aluminium in copper magnesium bimetallic conductor production technology is characterized in that this technology comprises the steps:
A, surface preparation: hydronalium is carried out the oil removing scale removal handle, thereby remove the hydronalium surface film oxide;
B, heavy zinc preliminary treatment: the hydronalium that will remove surface film oxide sink zinc to be handled, and makes the hydronalium surface form one deck densification and the uniform many intermediate metals of zinc-base;
C, non-cyanide pre-plating nickel: one deck nickel dam is electroplated through non-cyanide plating nickel mode in the hydronalium surface that has the many intermediate metals of zinc-base on the surface;
D, hydrochlorate copper facing: the hydronalium that will be coated with nickel dam carries out hydrochlorate copper facing, thereby forms fine and close oxygen-free copper layer on the surface;
E, reprocessing: the hydronalium that will be coated with the copper layer carries out reprocessing, thereby makes the aluminium in copper magnesium bimetallic conductor.
In above-mentioned aluminium in copper magnesium bimetallic conductor production technology, in above-mentioned steps A, adopt degreaser earlier to the hydronalium surface degreasing, remove the hydronalium surface film oxide with acid etching scale removal treatment fluid then.
In above-mentioned aluminium in copper magnesium bimetallic conductor production technology, in above-mentioned steps A, described acid etching scale removal treatment fluid comprises following component: concentration is 68% HNO
3Solution: 500-600ml/L; H
3PO
4: 300-350ml/L; Inorganic ammonium salt: 10-15g/L; Organic amino-contained compound 15-25g/L; Surfactant: 5-10g/L; Surplus is a water.
In above-mentioned aluminium in copper magnesium bimetallic conductor production technology, in above-mentioned step B, adopt the Zinc-based multi-element alloy deposit fluid to carry out at least once heavy zinc preliminary treatment, described Zinc-based multi-element alloy deposit fluid comprises following component: NaOH: 100-150g/L; Zinc oxide: 10-30g/L; Sodium potassium tartrate tetrahydrate: 8-10g/L; Nickel salt: 10-50g/L; Cobalt salt: 8-20g/L; Pink salt: 5-15g/L; Iron chloride: 2-3g/L; Surfactant: 1-5g/L; Surplus is a water.
In above-mentioned aluminium in copper magnesium bimetallic conductor production technology, in above-mentioned step D, in plating bath, add the high APES class liberation of hydrogen inhibitor of overpotential of hydrogen evolution.
In above-mentioned aluminium in copper magnesium bimetallic conductor production technology; In above-mentioned step D; When electroplating, adopt the pulse modulation power supply to electroplate; Promptly sometime the section in electrode will carry out the cathode electrodeposition under the higher current density, after a period of time, electrode will get into the reverse anodic solution stage.
In above-mentioned aluminium in copper magnesium bimetallic conductor production technology, in above-mentioned step e, reprocessing comprises surface passivation, oven dry, rolling and wire drawing.
Compared with prior art; The advantage of this aluminium in copper magnesium bimetallic conductor production technology is: 1, handle microstructure integrality in the gained superficial layer of back through the Zinc-based multi-element alloy deposit fluid; Even compact, Zinc-based multi-element alloy transition zone that conduction is good on the chemically active almag matrix of height, have been obtained; Adjust the surface activity of almag well, guaranteed the running quality and the stability of drawing group processing procedure of follow-up electroplating process.2, in plating bath, add the high APES class liberation of hydrogen inhibitor of overpotential of hydrogen evolution; Reduced the liberation of hydrogen side reaction in the copper ion cathodic electrodeposition process significantly; Significantly reduced the degree that copper cover aluminum is electroplated intermediate products generation hydrogen embrittlement; Solved and electroplated the fracture of wire phenomenon of intermediate products in follow-up drawing process, improved the rate of finished products of final products.3, select for use the pulse modulation power supply to electroplate, improved the microstructure of electrocrystallization copper, improved the packing of copper coating, suppressed the liberation of hydrogen side reaction.4, the acid etching scale removal treatment fluid of no fluorine ion; In prescription, add surfactant and contain amino organic nitrogen oxide inhibitor; Make the almag surface in acid etching, scale removal process, can effectively remove surface film oxide; The excessive corrosion that can effectively suppress matrix is again compared nitrogen oxides pollution thing amount and has been reduced more than 90% with traditional handicraft, improved the production operation environment widely.
Embodiment
This aluminium in copper magnesium bimetallic conductor production technology comprises the steps:
A, surface preparation: hydronalium is carried out the oil removing scale removal handle, thereby remove the hydronalium surface film oxide.Adopt degreaser to the hydronalium surface degreasing earlier, remove the hydronalium surface film oxide with acid etching scale removal treatment fluid then.Acid etching scale removal treatment fluid comprises following component: concentration is 68% HNO
3Solution: 500-600ml/L; H
3PO
4: 300-350ml/L; Inorganic ammonium salt: 10-15g/L; Organic amino-contained compound 15-25g/L; Surfactant: 5-10g/L; Surplus is a water.
B, heavy zinc preliminary treatment: the hydronalium that will remove surface film oxide sink zinc to be handled, and makes the hydronalium surface form one deck densification and the uniform many intermediate metals of zinc-base.Adopt the Zinc-based multi-element alloy deposit fluid to carry out at least once heavy zinc preliminary treatment, described Zinc-based multi-element alloy deposit fluid comprises following component: NaOH: 100-150g/L; Zinc oxide: 10-30g/L; Sodium potassium tartrate tetrahydrate: 8-10g/L; Nickel salt: 10-50g/L; Cobalt salt: 8-20g/L; Pink salt: 5-15g/L; Iron chloride: 2-3g/L; Surfactant: 1-5g/L; Surplus is a water.
C, non-cyanide pre-plating nickel: one deck nickel dam is electroplated through non-cyanide plating nickel mode in the hydronalium surface that has the many intermediate metals of zinc-base on the surface.
D, hydrochlorate copper facing: the hydronalium that will be coated with nickel dam carries out hydrochlorate copper facing, thereby forms fine and close oxygen-free copper layer on the surface.In plating bath, add the high APES class liberation of hydrogen inhibitor of overpotential of hydrogen evolution.When electroplating, adopt the pulse modulation power supply to electroplate, promptly electrode will carry out the cathode electrodeposition under the higher current density in section sometime, and after a period of time, electrode will get into the reverse anodic solution stage.
E, reprocessing: the hydronalium that will be coated with the copper layer carries out reprocessing, thereby makes the aluminium in copper magnesium bimetallic conductor.Reprocessing comprises surface passivation, oven dry, rolling and wire drawing.
In the steps A, do not contain the high concentration fluorine ion in the acid etching scale removal treatment fluid, add suitable surfactant, promoted the acid etching process.In addition, comprised the release that organic amino-contained compound can reduce nitrogen oxide significantly.Compare nitrogen oxides pollution thing amount with traditional handicraft and reduced more than 90%, improved the production operation environment widely.
Among the step B, the Zinc-based multi-element alloy deposit fluid can form zinc-base nickel, cobalt, tin, iron multicomponent alloy layer on the hydronalium surface.Heavy zinc is handled microstructure integrality in the gained superficial layer of back; Even compact, Zinc-based multi-element alloy transition zone that conduction is good on the chemically active almag matrix of height, have been obtained; Adjust the surface activity of almag well, guaranteed the running quality and the stability of drawing group processing procedure of follow-up electroplating process.Through chemical replacement at hydronalium surface deposition multiple zinc-base alloy; Improved the microstructure integrality of the zinc-containing alloy layer that displacement forms on the hydronalium greatly; Simultaneously also refinement separate out the size of kirsite crystal grain, improve and soak the adhesion between zinc alloy layer and almag matrix.This combines tight copper plate extremely important to aluminium, the magnesium surface formation at high chemical activity in the subsequent handling.In addition, add the stability that proper amount of surfactant can obviously be improved treatment fluid.The surfactant here is meant to have fixing hydrophilic and oleophilic group, aligns at the surface energy of solution, and the material that surface tension is significantly descended.The molecular structure of surfactant has amphipathic: an end is a hydrophilic radical, and the other end is the hydrophobic group; Hydrophilic radical often is the group of polarity, like carboxylic acid, sulfonic acid, sulfuric acid, amino or amido and salt thereof, and also hydroxyl, amide groups, ehter bond etc.; And the hydrophobic group is nonpolar hydrocarbon chain often, like 8 above hydrocarbon chains of carbon atom.Surfactant is divided into ionic surfactant and nonionic surface active agent etc.
Among the step C; For further improving the bond strength of Zinc-based multi-element alloy layer and copper plate; Pre-nickel plating on the Zinc-based multi-element alloy layer; Guarantee newly to separate out Zinc-based multi-element alloy layer that electrodeposited coating and original chemical replacement deposit and between good combination, brought into play the effect of nickel, cobalt composition in the Zinc-based multi-element alloy layer, significantly improved the Mechanics of Machinery and the electric property of coating.
Among the step D, in traditional hydrochlorate electro-coppering process, adopted higher current density, be generally 500A/m2 or higher for enhancing productivity.In the case; When the mass transfer in liquid phase of reaction mass copper ion in the electrolyte was under-supply, the liberation of hydrogen side reaction must aggravate, thereby caused that amount of hydrogen infiltration increases in the electro-coppering alclad product; And further cause the hydrogen embrittlement problem; The fracture of wire phenomenon promptly taking place in follow-up drawing process, have a strong impact on the quality and the rate of finished products of product, can't produce sometimes even at all.The hydrogen embrittlement problem is the quality problems of most important and necessary solution to galvanoplastic copper-clad aluminum conductor manufacturer.The method that the present invention adopts is that the source of cathode reaction dynamic analysis from the hydrochlorate electroplating process addresses.According to principle of electrochemical reaction, solve having its source in of hydrogen embrittlement problem and suppress the liberation of hydrogen side reaction in the electrochemical cathode course of reaction.The present invention adopts linear potential scanning and electrochemical AC impedance achievement in research; Tested the inhibition effect of more than 20 additive, therefrom filtered out and have a good inhibiting APES class additive copper liberation of hydrogen side reaction in the salt cathodic electrodeposition process.Through in plating bath, adding a certain amount of APES class additive, the liberation of hydrogen side reaction of success in having suppressed the cathode electrodeposition process solved the amount of hydrogen infiltration in the electro-coppering alclad product preferably, thus solution hydrogen embrittlement problem.
The conventional current mode that adopts in the present domestic electro-coppering alclad production is the conventional dc power supply; The applicant electroplates on the basis of test at the employing conventional dc power supply of long period; Find that traditional direct current mode is subject to the mass transport affects of reaction mass and produces the concentration polarization effect; And then influencing the surface quality of coating, coating crystal grain is thick, loose porous as producing, not enough even compact etc.For solving this technical barrier, the applicant finds to adopt modulation power source pulse plating technology, can improve the packing of copper coating.Can know that from electroplating basic theories the technological factor that influences coating compactness mainly comprises: (1) bath element; (2) cathode-current density; (3) concentration of reaction mass and mass transfer in liquid phase situation in the electrolyte; (4) current system.In Electrochemical Engineering, current density indicates the speed of electrochemical reaction.In galvanoplastic manufactured copper alclad production, be the higher current density of general employing of enhancing productivity, but the raising of current density must need the good mass transfer in liquid phase of reaction mass to guarantee.If mass transfer in liquid phase can not get guaranteeing when improving current density, will cause the electro-deposition grain coarsening, coating is fine and close inadequately, and adhesion variation between coating and the matrix, the more dangerous generation that will aggravate evolving hydrogen reaction greatly, and then the hydrogen embrittlement of generation electroplated product.For smooth solution can guarantee production efficiency, can improve quality of coating again, the electroplating technology with the modulating pulse power supply has been proposed to the applicant's novelty.The modulating pulse power supply is a kind of polarity of periodicity adjustment electric current, the extraordinary electric current of amplitude, and its parameter comprises pulsewidth, duty ratio.The notion of pulse modulation power supply is used in copper electrolyzing refining and boost battery charge technology, but in the copper cover aluminum galvanoplastic are produced, does not adopt as yet.Analyze theoretically, adopt the pulse modulation power technology, electrode will carry out the cathode electrodeposition under the higher current density in section sometime; But after a period of time; Electrode will get into the reverse anodic solution stage, through the reverse dissolving in this stage, both can make positive half cycle electro-deposition separate out bad crystal grain dissolving again takes place; But also can alleviate the concentration of copper ion in the electrode surface liquid layer, eliminate the concentration polarization effect.And, through this technology, can eliminate the liberation of hydrogen side reaction.
The technology and the performance index of the aluminium in copper magnesium bimetallic conductor that processes through the present invention are following:
(1) outward appearance: on the evenly continuous metallized aluminum magnesium alloy heart yearn of copper layer, the smooth surface rounding must not have defectives such as indenture, crackle, dew aluminium and obvious rust staining;
(2) nominal diameter: 0.1～2.77mm (also can produce the aluminium in copper magnesium line of other sizes) by customer requirements; Diameter is less than the aluminium in copper magnesium line of 0.3mm, and deviation is no more than+/-0.003mm; Diameter is greater than the aluminium in copper magnesium line of 0.3mm, and deviation is no more than 1%.
(3) resistivity:＜=0.029 (mm
2/ m, 20 ℃)
(4) tensile strength and percentage elongation
(5) copper layer thickness :=＞3.5% (line footpath), be used for the CCAM copper layer thickness of high-frequency signal transmission, also need skin depth greater than signal;
(6) density:＜=3.32 (g/cm3)
(7) copper layer density: the sample of intercepting suitable length, with its interval clamping and tension, reverse 3 circles along same direction 15 times of nominal diameters, and then turn-back 3 circles.Any destructiveness, successional crackle should not appear in the copper layer.
(8) copper aluminium adhesiveness: sample is carried out alternating bending, and until sample fracture, the copper aluminium on the fracture should flush, and both are very close to each other.
Specific embodiment described herein only is that the present invention's spirit is illustrated.Person of ordinary skill in the field of the present invention can make various modifications or replenishes or adopt similar mode to substitute described specific embodiment, but can't depart from spirit of the present invention or surmount the defined scope of appended claims.
Although this paper has used term morely, do not get rid of the possibility of using other term.Using these terms only is in order to describe and explain essence of the present invention more easily; It all is contrary with spirit of the present invention being construed to any additional restriction to them.
Claims (7)
1. an aluminium in copper magnesium bimetallic conductor production technology is characterized in that this technology comprises the steps:
A, surface preparation: hydronalium is carried out the oil removing scale removal handle, thereby remove the hydronalium surface film oxide;
B, heavy zinc preliminary treatment: the hydronalium that will remove surface film oxide sink zinc to be handled, and makes the hydronalium surface form one deck densification and the uniform many intermediate metals of zinc-base;
C, non-cyanide pre-plating nickel: one deck nickel dam is electroplated through non-cyanide plating nickel mode in the hydronalium surface that has the many intermediate metals of zinc-base on the surface;
D, hydrochlorate copper facing: the hydronalium that will be coated with nickel dam carries out hydrochlorate copper facing, thereby forms fine and close oxygen-free copper layer on the surface;
E, reprocessing: the hydronalium that will be coated with the copper layer carries out reprocessing, thereby makes the aluminium in copper magnesium bimetallic conductor.
2. aluminium in copper magnesium bimetallic conductor production technology according to claim 1 is characterized in that, in above-mentioned steps A, adopts degreaser to the hydronalium surface degreasing earlier, removes the hydronalium surface film oxide with acid etching scale removal treatment fluid then.
3. aluminium in copper magnesium bimetallic conductor production technology according to claim 2 is characterized in that, in above-mentioned steps A, described acid etching scale removal treatment fluid comprises following component: concentration is 68% HNO
3Solution: 500-600ml/L; H
3PO
4: 300-350ml/L; Inorganic ammonium salt: 10-15g/L; Organic amino-contained compound 15-25g/L; Surfactant: 5-10g/L; Surplus is a water.
4. aluminium in copper magnesium bimetallic conductor production technology according to claim 1; It is characterized in that; In above-mentioned step B; Adopt the Zinc-based multi-element alloy deposit fluid to carry out at least once heavy zinc preliminary treatment, described Zinc-based multi-element alloy deposit fluid comprises following component: NaOH: 100-150g/L; Zinc oxide: 10-30g/L; Sodium potassium tartrate tetrahydrate: 8-10g/L; Nickel salt: 10-50g/L; Cobalt salt: 8-20g/L; Pink salt: 5-15g/L; Iron chloride: 2-3g/L; Surfactant: 1-5g/L; Surplus is a water.
5. according to claim 1 or 2 or 3 or 4 described aluminium in copper magnesium bimetallic conductor production technologies, it is characterized in that, in above-mentioned step D, in plating bath, add the high APES class liberation of hydrogen inhibitor of overpotential of hydrogen evolution.
6. according to claim 1 or 2 or 3 or 4 described aluminium in copper magnesium bimetallic conductor production technologies; It is characterized in that; In above-mentioned step D, when electroplating, adopt the pulse modulation power supply to electroplate, promptly electrode will carry out the cathode electrodeposition under the higher current density in section sometime; After a period of time, electrode will get into the reverse anodic solution stage.
7. according to claim 1 or 2 or 3 or 4 described aluminium in copper magnesium bimetallic conductor production technologies, it is characterized in that in above-mentioned step e, reprocessing comprises surface passivation, oven dry, rolling and wire drawing.
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| CN201110149485.7A CN102324276B (en) | 2011-06-02 | 2011-06-02 | Production process of copper coated aluminum-magnesium bimetallic conductor |
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| CN201110149485.7A CN102324276B (en) | 2011-06-02 | 2011-06-02 | Production process of copper coated aluminum-magnesium bimetallic conductor |
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| CN105793932A (en) * | 2013-12-02 | 2016-07-20 | 株式会社藤仓 | High-frequency electrical wire and coil |
| CN108221018A (en) * | 2017-12-28 | 2018-06-29 | 中宥(平原)科技有限公司 | A kind of high-efficiency copper based on secondary heavy zinc covers aluminium technique |
| CN114045476A (en) * | 2021-11-11 | 2022-02-15 | 重庆大学 | Copper-magnesium composite material and preparation method and application thereof |
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| CN114045476B (en) * | 2021-11-11 | 2023-10-20 | 重庆大学 | Copper-magnesium composite material and preparation method and application thereof |
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| CN102324276B (en) | 2017-02-22 |
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