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CN103757671A - Electroplating solution and electroplating method for electrocoppering surface of low-carbon steel plate in alkaline manner - Google Patents

Electroplating solution and electroplating method for electrocoppering surface of low-carbon steel plate in alkaline manner Download PDF

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CN103757671A
CN103757671A CN201410003876.1A CN201410003876A CN103757671A CN 103757671 A CN103757671 A CN 103757671A CN 201410003876 A CN201410003876 A CN 201410003876A CN 103757671 A CN103757671 A CN 103757671A
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electroplating
solution
steel plate
carbon steel
beaker
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钟庆东
顾帅帅
牟童
纪丹
勒霞文
周琼宇
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SHANGHAI UNIVERSITY
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SHANGHAI UNIVERSITY
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Abstract

本发明提出了一种在低碳钢板表面碱性电镀铜的电镀溶液和电镀方法，本发明采用镀液的基本配方为：一水合柠檬酸70~120g?L-1，酒石酸钠20~40g?L-1，柠檬酸三钠8~13g?L-1，Cu2(OH)2CO3 20~30g?L-1，CuSO4·5H2O8~12g?L-1，(NH4)2SO45~10g?L-1，NaHCO310~20g?L-1，NaOH10~20g?L-1，甲基苯骈三氮唑2~10mg?L-1。用快速直流电沉积和脉冲电镀法进行快速电镀，并观察和测试了其力学和电化学性能。结果表明，本处理方法能极大的提高低碳钢板的耐腐蚀性能和力学性能。The present invention proposes an electroplating solution and an electroplating method for alkaline electroplating copper on the surface of a low-carbon steel plate. The basic formula of the plating solution used in the present invention is: citric acid monohydrate 70~120g?L -1 , sodium tartrate 20~40g? L -1 , trisodium citrate 8~13g?L -1 , Cu 2 (OH) 2 CO 3 20~30g?L -1 , CuSO 4 ·5H 2 O8~12g?L -1 , (NH 4 ) 2 SO 4 5~10g?L -1 , NaHCO 3 10~20g?L -1 , NaOH 10~20g?L -1 , tolyltriazole 2~10mg?L -1 . Fast electroplating was performed by fast direct current electrodeposition and pulse electroplating, and its mechanical and electrochemical properties were observed and tested. The results show that this treatment method can greatly improve the corrosion resistance and mechanical properties of the low carbon steel plate.

Description

A kind of electroplating solution and electro-plating method in the electro-coppering of mild steel plate surface alkalinty
Technical field
The present invention relates to a kind of electroplating solution and electro-plating method in the electro-coppering of mild steel plate surface alkalinty, be specifically applicable to the coating surface metal of mild steel plate, belong to the coating technology field of metallic surface.
Background technology
Copper coating is a kind of quality softness, has the coating of good ductility, electroconductibility and thermal conductivity.Process for copper is divided into cyanide copper plating technique and the large class of cyanide-free copper electroplating technique two.Copper plate crystallization that cyanide copper plating technique obtains is careful, porosity is little, but cyanide copper plating process contains hypertoxic CN -, in whole technology controlling and process and maintenance process, there is huge potential safety hazard, therefore, research and development cyanide-free copper electroplating technique becomes trend of the times.
China carries out cyanideless electro-plating technological development the history of three more than ten years, in the seventies in last century, has once started a climax, has also obtained some achievements, as has developed HEDP copper facing etc.Adopt alkaline copper plating technique, because it can directly directly plate on steel part or foundry goods, can obtain the copper coating that luminance brightness is high, bonding force good, porosity is low, and current efficiency is high.
Pulse plating: make to electroplate loop and periodically switch on and off, or the electro-plating method of a certain waveform pulse that superposes again on fixing direct current.Compared with direct current electrode position, pulse plating also has many advantages, as reduced the porosity of settled layer, improves coating luminance brightness, electric conductivity and corrosion resistance nature, elimination of hydrogen embrittlement etc.
Direct current flash plate: remaining a kind of electrochemical process in principle, be a kind of redox processes of not carrying out in plating coating bath, and electroplating process carries out in need plating workpiece surface part, and sedimentation velocity is very fast, can save electroplating time.
Common are pyrophosphate copper plating technique, this technique dispersive ability is good, and corrodibility is little, nontoxicity, and the additive that matching property is good can obtain the careful coating of crystallization, but for steel part, direct copper plating can not get the good copper plate of bonding force; EDTA copper facing is convenient to obtain the coating of good bonding strength, but deposition is slow and EDTA and the stronger complexing of most metal, and complexation constant difference is little, at EDTA, is the formula of easy exploiting plating alloy not on copper plating bath basis.So we need the electroplating bath solution without cyanogen copper plating rapidly and the electro-plating method of development of new.
Summary of the invention
The defect existing for prior art, the object of the present invention is to provide a kind of electroplating solution and electro-plating method in the electro-coppering of mild steel plate surface alkalinty, a kind of simple to operate, equipment requirements is loose, less energy-consumption, the good in economic efficiency method in the electro-coppering of mild steel plate surface alkalinty.
For achieving the above object, the present invention adopts following technical scheme:
At an electroplating solution for mild steel plate surface alkalinty electro-coppering, the composition of electroplating solution has:
Monohydrate potassium 70 ~ 120 gL -1,
Sodium tartrate 20 ~ 40 gL -1,
Trisodium citrate 8 ~ 13 gL -1,
Cu 2(OH) 2CO 3 20~30 g·L -1，
CuSO 4·5H 2O 8~12 g·L -1，
(NH 4) 2SO 4 5~10 g·L -1，
NaHCO 3 10~20 g·L -1，
NaOH 10~20 g·L -1，
Tolyltriazole 2 ~ 10 mgL -1.
In a method for mild steel plate surface alkalinty electro-coppering, comprise following technological process and step:
A. with electronic scales, by above-mentioned formula, take monohydrate potassium, sodium tartrate and trisodium citrate and dissolve in a beaker, take Cu 2(OH) 2cO 3and CuSO 45H 2o is dissolved in another beaker, takes afterwards NaHCO again 3be dissolved in the 3rd beaker, merge first two solution, and stir, slowly add NaHCO 3solution, makes electroplating solution constant temperature at 25 ℃ afterwards, makes volume be not more than 3/4ths of beaker nominal volume, after standing 2 hours, with magnetic stirrer electroplating solution weighing (NH 4) 2sO 4, NaOH and tolyltriazole add in electroplating solution, the basic plating solution that secure ph is 9 ~ 10;
B. the preparation of coating: anticathode matrix, mild steel plate carries out the pre-treatment such as oil removing, rust cleaning and surface active, and concrete operations are: mild steel plate is immersed in except being heated to 50～60 ℃ in oil solution, after 5～10 minutes, takes out; After oil removing completely, the sulphuric acid soln of putting into 5wt% activates 30 seconds, and taking-up is selected 1-10 A/dm after cleaning with distilled water 2current density, carry out direct current electrode position; Or 10-20A/dm 2current density, the pulsed current that dutycycle is 60% ~ 80% carries out pulse plating; Deposit after 5-10 minute and to take out, after cleaning with distilled water and with cold wind, dry, can make light, the good and good copper coating of solidity to corrosion of bonding force.
Compared with prior art, the present invention has following outstanding substantive distinguishing features and significant advantage:
1) operating process is simple, and experiment condition easily reaches; 2) can adopt larger current density, direct current electrode position speed is fast, saves time; 3) surface of pulsed electrical copper facing has very high hardness, luminance brightness and erosion resistance; 4) electroplate liquid formulation is creative, additive add effectively refinement coating crystal grain, improved the intensity of coating, hardness and bonding force, further improved the performance of coating.
The present invention hot research fields such as mild steel plate surface quick electrodeposition and pulse plating of combining closely, and the additive of actively seeking to improve the complexing agent of current density and improving corrosion resistance coating, make the copper facing of mild steel plate surface electrical can adapt to the performance requriements of production and industrial circle.
Embodiment
After now specific embodiments of the invention being described in.
embodiment 1
In the present embodiment, with pure distilled water preparation 500ml plating solution, the composition of plating solution has: monohydrate potassium 70 gL -1, sodium tartrate 40gL -1, trisodium citrate 8 gL -1, Cu 2(OH) 2cO 320gL -1, CuSO 45H 2o 10gL -1, (NH 4) 2sO 410 gL -1, NaHCO 320 gL -1, NaOH 10 gL -1, tolyltriazole 2 mgL -1.
With electronic scales, take according to quantity monohydrate potassium, sodium tartrate and trisodium citrate and dissolve in a beaker, take Cu 2(OH) 2cO 3and CuSO 45H 2o is dissolved in another beaker, takes afterwards NaHCO again 3be dissolved in the 3rd beaker, merge first two solution, and stir, slowly add NaHCO 3solution, makes plating solution constant temperature at 25 ℃ afterwards, makes volume be not more than 3/4ths of beaker nominal volume.After standing 2 hours, with magnetic stirrer plating solution weighing (NH 4) 2sO 4, NaOH and tolyltriazole add in plating solution, the alkali plating solution that secure ph is 9.
Anticathode matrix (mild steel plate) carries out the pre-treatment such as oil removing, rust cleaning and surface active, and concrete operations are: the mild steel plate of 10mm × 10mm × 1.5mm is immersed in except being heated to 60 ℃ in oil solution, after 10 minutes, takes out; After oil removing completely, the sulphuric acid soln of putting into 5wt% activates 30 seconds, and taking-up is selected 5A/dm after cleaning with distilled water 2current density carry out direct current electrode position; Deposit after 5 minutes and to take out, after cleaning with distilled water and with cold wind, dry, can make light, the copper coating that smooth and bonding force is good.
Coating light after direct current electrode position, has good bonding force, and coating is approximately 20 μ m, and current impedance is 800 Ω/cm 2, microhardness is 150HV.
embodiment 2
In the present embodiment, with pure distilled water preparation 500ml plating solution, the composition of plating solution has: monohydrate potassium 100 gL -1, sodium tartrate 30gL -1, trisodium citrate 8gL -1, Cu 2(OH) 2cO 330gL -1, CuSO 45H 2o 10gL -1, (NH 4) 2sO 410gL -1, NaHCO 320 g L -1, NaOH 15 gL -1, tolyltriazole 2 mgL -1.
With electronic scales, take according to quantity monohydrate potassium, sodium tartrate and trisodium citrate and dissolve in a beaker, take Cu 2(OH) 2cO 3and CuSO 45H 2o is dissolved in another beaker, takes afterwards NaHCO again 3be dissolved in the 3rd beaker, merge first two solution, and stir, slowly add NaHCO 3solution, makes plating solution constant temperature at 25 ℃ afterwards, makes volume be not more than 3/4ths of beaker nominal volume.After standing 2 hours, with magnetic stirrer plating solution weighing (NH 4) 2sO 4, NaOH and tolyltriazole add in plating solution, the alkali plating solution that secure ph is 9.
Anticathode matrix (mild steel plate) carries out the pre-treatment such as oil removing, rust cleaning and surface active, and concrete operations are: the mild steel plate of 10mm × 10mm × 1.5mm is immersed in except being heated to 60 ℃ in oil solution, after 10 minutes, takes out; After oil removing completely, the sulphuric acid soln of putting into 5wt% activates 30 seconds, and taking-up is selected 8A/dm after cleaning with distilled water 2current density carry out direct current electrode position; Deposit after 5 minutes and to take out, after cleaning with distilled water and with cold wind, dry, can make light, the copper coating that smooth and bonding force is good.
Coating light after plating, has good bonding force, and coating is approximately 40 μ m, and current impedance is 1200 Ω/cm 2, microhardness is 180HV.
embodiment 3
In the present embodiment, with pure distilled water preparation 500ml plating solution, the composition of plating solution has: monohydrate potassium 120 gL -1, sodium tartrate 20gL -1, trisodium citrate 10gL -1, Cu 2(OH) 2cO 330gL -1, CuSO 45H 2o 10gL -1, (NH 4) 2sO 420 gL -1, NaHCO 310 gL -1, NaOH 20 gL -1, tolyltriazole 5 mgL -1.
With electronic scales, take according to quantity monohydrate potassium, sodium tartrate and trisodium citrate and dissolve in a beaker, take Cu 2(OH) 2cO 3and CuSO 45H 2o is dissolved in another beaker, takes afterwards NaHCO again 3be dissolved in the 3rd beaker, merge first two solution, and stir, slowly add NaHCO 3solution, makes plating solution constant temperature at 25 ℃ afterwards, makes volume be not more than 3/4ths of beaker nominal volume.After standing 2 hours, with magnetic stirrer plating solution weighing (NH 4) 2sO 4, NaOH and tolyltriazole add in plating solution, the alkali plating solution that secure ph is 10.
Anticathode matrix (mild steel plate) carries out the pre-treatment such as oil removing, rust cleaning and surface active, and concrete operations are: the mild steel plate of 10mm × 10mm × 1.5mm is immersed in except being heated to 60 ℃ in oil solution, after 10 minutes, takes out; After oil removing completely, the sulphuric acid soln of putting into 5wt% activates 30 seconds, and taking-up is selected 8A/dm after cleaning with distilled water 2current density carry out direct current electrode position; Deposit after 5 minutes and to take out, after cleaning with distilled water and with cold wind, dry, can make light, the copper coating that smooth and bonding force is good.
Coating light after plating, has good bonding force, and coating is approximately 40 μ m, and current impedance is 1000 Ω/cm 2, microhardness is 160HV.
embodiment 4
In the present embodiment, with pure distilled water preparation 500ml plating solution, the composition of plating solution has: monohydrate potassium 120 gL -1, sodium tartrate 40gL -1, trisodium citrate 13 gL -1, Cu 2(OH) 2cO 320 gL -1, CuSO 45H 2o 8 gL -1, (NH 4) 2sO 420 gL -1, NaHCO 310 gL -1, NaOH 20 gL -1, tolyltriazole 5 mgL -1.
With electronic scales, take according to quantity monohydrate potassium, sodium tartrate and trisodium citrate and dissolve in a beaker, take Cu 2(OH) 2cO 3and CuSO 45H 2o is dissolved in another beaker, takes afterwards NaHCO again 3be dissolved in the 3rd beaker, merge first two solution, and stir, slowly add NaHCO 3solution, makes plating solution constant temperature at 25 ℃ afterwards, makes volume be not more than 3/4ths of beaker nominal volume.After standing 2 hours, with magnetic stirrer plating solution weighing (NH 4) 2sO 4, NaOH and tolyltriazole add in plating solution, the alkali plating solution that secure ph is 10.
Anticathode matrix (mild steel plate) carries out the pre-treatment such as oil removing, rust cleaning and surface active, and concrete operations are: the mild steel plate of 10mm × 10mm × 1.5mm is immersed in except being heated to 60 ℃ in oil solution, after 10 minutes, takes out; After oil removing completely, the sulphuric acid soln of putting into 5wt% activates 30 seconds, and taking-up is selected 10A/dm after cleaning with distilled water 2current density and dutycycle be 60% electric current carries out pulse plating; Deposit after 8 minutes and to take out, after cleaning with distilled water and with cold wind, dry, can make light, the copper coating that smooth and bonding force is good.
Coating light after pulse plating, has extraordinary bonding force, and coating is approximately 50 μ m, and current impedance is 1360 Ω/cm 2, microhardness is 200HV.
embodiment 5
In the present embodiment, with pure distilled water preparation 500ml plating solution, the composition of plating solution has: monohydrate potassium 90 gL -1, sodium tartrate 20gL -1, trisodium citrate 8 gL -1, Cu 2(OH) 2cO 320gL -1, CuSO 45H 2o 10gL -1, (NH 4) 2sO 410 gL -1, NaHCO 320 gL -1, NaOH 18 gL -1, tolyltriazole 5mgL -1.
With electronic scales, take according to quantity monohydrate potassium, sodium tartrate and trisodium citrate and dissolve in a beaker, take Cu 2(OH) 2cO 3and CuSO 45H 2o is dissolved in another beaker, takes afterwards NaHCO again 3be dissolved in the 3rd beaker, merge first two solution, and stir, slowly add NaHCO 3solution, makes plating solution constant temperature at 25 ℃ afterwards, makes volume be not more than 3/4ths of beaker nominal volume.After standing 2 hours, with magnetic stirrer plating solution weighing (NH 4) 2sO 4, NaOH and tolyltriazole add in plating solution, the alkali plating solution that secure ph is 10.
Anticathode matrix (mild steel plate) carries out the pre-treatment such as oil removing, rust cleaning and surface active, and concrete operations are: the mild steel plate of 10mm × 10mm × 1.5mm is immersed in except being heated to 60 ℃ in oil solution, after 10 minutes, takes out; After oil removing completely, the sulphuric acid soln of putting into 5wt% activates 30 seconds, and taking-up is selected 10A/dm after cleaning with distilled water 2current density and dutycycle be 60% electric current carries out pulse plating; Deposit after 8 minutes and to take out, after cleaning with distilled water and with cold wind, dry, can make light, the copper coating that smooth and bonding force is good.
Coating light after pulse plating, has extraordinary bonding force, and coating is approximately 60 μ m, and current impedance is 1600 Ω/cm 2, microhardness is 230HV.
Examples prove utilizes the technology of the present invention, in the shorter time, can obtain more satisfactory copper plate, has improved greatly the efficiency of electroplating.The obvious increase of the impedance of the mild steel plate copper coating layer of processing, the coating hardness that the technology of the present invention obtains is higher, and explanation can make the corrosion resistance nature of mild steel plate greatly improve through treatment process of the present invention.

Claims (2)

1.一种在低碳钢板表面碱性电镀铜的电镀溶液，其特征在于，电镀溶液的组成有： 1. an electroplating solution for alkaline electroplating copper on low carbon steel plate surface, it is characterized in that, the composition of electroplating solution has: 一水合柠檬酸 70~120 g•L-1， Citric acid monohydrate 70~120 g•L -1 , 酒石酸钠 20~40 g•L-1， Sodium tartrate 20~40 g•L -1 , 柠檬酸三钠 8~13 g•L-1， Trisodium citrate 8~13 g•L -1 , Cu2(OH)2CO3 20~30 g•L-1， Cu 2 (OH) 2 CO 3 20~30 g•L -1 , CuSO4·5H2O 8~12 g•L-1， CuSO 4 ·5H 2 O 8~12 g·L -1 , (NH4)2SO4 5~10 g•L-1， (NH 4 ) 2 SO 4 5~10 g•L -1 , NaHCO3 10~20 g•L-1， NaHCO 3 10~20 g•L -1 , NaOH 10~20 g•L-1， NaOH 10~20 g•L -1 , 甲基苯骈三氮唑 2~10 mg•L-1。 Tolyltriazole 2~10 mg•L -1 . 2.一种在低碳钢板表面碱性电镀铜的方法，其特征在于，包括如下工艺过程和步骤： 2. A method of alkaline electroplating copper on the surface of low carbon steel plate, characterized in that, comprising the following process and steps: A.用电子秤按上述配方称取一水合柠檬酸、酒石酸钠和柠檬酸三钠在一个烧杯中溶解，称取Cu2(OH)2CO3和CuSO4·5H2O溶解在另一个烧杯中，之后再称取NaHCO3溶解在第三个烧杯中，合并前两种溶液，并搅拌均匀，缓慢加入NaHCO3溶液，之后使电镀溶液恒温在25℃，使体积不大于烧杯额定体积的四分之三，静置2小时后，用磁力搅拌器搅拌电镀溶液并称量(NH4)2SO4，NaOH和甲基苯骈三氮唑加入电镀溶液中，配制pH值为9~10的碱性电镀溶液； A. Use an electronic scale to weigh citric acid monohydrate, sodium tartrate and trisodium citrate in one beaker according to the above formula, and dissolve Cu 2 (OH) 2 CO 3 and CuSO 4 5H 2 O in another beaker After that, weigh NaHCO 3 and dissolve it in the third beaker, combine the first two solutions and stir evenly, slowly add NaHCO 3 solution, and then keep the temperature of the electroplating solution at 25°C so that the volume is not greater than four times the rated volume of the beaker. After standing still for 2 hours, stir the electroplating solution with a magnetic stirrer and weigh (NH 4 ) 2 SO 4 , add NaOH and tolyltriazole into the electroplating solution to prepare a pH value of 9~10 Alkaline plating solution; B．镀层的制备：对阴极基体，即低碳钢板进行除油、除锈和表面活化等预处理，具体操作是：将低碳钢板浸在除油溶液中加热到50～60℃，5～10分钟后取出；除油完全后，放入5wt%的硫酸溶液中活化30秒，取出用蒸馏水洗净后，选择1-10 A/dm2的电流密度，进行直流电镀；或者10-20A/dm2的电流密度，占空比为60%~80%的脉冲电流进行脉冲电镀；沉积5-10分钟后取出，用蒸馏水清洗后并用冷风烘干，可制得光亮，结合力良好和耐蚀性较好的铜镀层。 B． Preparation of the coating: pre-treat the cathode substrate, that is, the low-carbon steel plate, such as degreasing, derusting and surface activation. The specific operation is: immerse the low-carbon steel plate in the degreasing solution and heat it to 50-60°C for 5-10 minutes Then take it out; after the oil is completely removed, put it into 5wt% sulfuric acid solution to activate for 30 seconds, take it out and wash it with distilled water, choose a current density of 1-10 A/dm 2 for DC electroplating; or 10-20A/dm 2 The current density is 60%~80% pulse current for pulse electroplating; take it out after 5-10 minutes of deposition, wash with distilled water and dry with cold air, you can get bright, good bonding force and good corrosion resistance Good copper plating.
CN201410003876.1A 2013-10-11 2014-01-06 Electroplating solution and electroplating method for electrocoppering surface of low-carbon steel plate in alkaline manner Pending CN103757671A (en)

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CN104087985A (en) * 2014-06-25 2014-10-08 安徽长青电子机械（集团）有限公司 Copper coating method of metal part
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CN106835212B (en) * 2017-03-29 2019-07-16 南京信息工程大学 A kind of electroplating solution for cyanide-free electroplating nanocrystalline copper and using method thereof
CN107227472A (en) * 2017-06-26 2017-10-03 江西理工大学 A kind of engineering super-hydrophobic coat of metal and preparation method thereof
CN108193239A (en) * 2017-12-27 2018-06-22 北京欧地安科技有限公司 A kind of copper-plated steel wire and its production method
CN108193239B (en) * 2017-12-27 2020-01-17 北京欧地安科技有限公司 Copper-plated steel wire and production method thereof
CN112410832A (en) * 2020-11-18 2021-02-26 中钢集团郑州金属制品研究院有限公司 Electrochemical copper plating process for steel wire

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Application publication date: 20140430