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 PDFInfo
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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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Abstract
The invention provides an electroplating solution and electroplating method for electrocoppering the surface of a low-carbon steel plate in an alkaline manner. A basic formula of the electroplating solution comprises the following substances: 70-120g/L of citric acid monohydrate, 20-40g/L of sodium tartrate, 8-13g/L of trisodium citrate, 20-30g/L of Cu2(OH)2CO3, 8-12g/L of CuSO4.5H2O, 5-10g/L of (NH4)2SO4, 10-20g/L of NaHCO3, 10-20g/L of NaOH and 2-10mg/L of tolyltriazole. Quick electroplating is carried out by using quick direct current electrodeposition and pulse plating methods, and mechanical and electrochemical performances of the low-carbon steel plate are observed and tested. The results show that the corrosion resistance and mechanical performances of the low-carbon steel plate can be greatly improved by adopting the treatment method.
Description
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. at an electroplating solution for mild steel plate surface alkalinty electro-coppering, it is characterized in that, 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.
2. in a method for mild steel plate surface alkalinty electro-coppering, it is characterized in that, 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.
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|---|---|---|---|
| CN201410003876.1A CN103757671A (en) | 2013-10-11 | 2014-01-06 | Electroplating solution and electroplating method for electrocoppering surface of low-carbon steel plate in alkaline manner |
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|---|---|---|---|
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| CN201310480042 | 2013-10-11 | ||
| CN201410003876.1A CN103757671A (en) | 2013-10-11 | 2014-01-06 | Electroplating solution and electroplating method for electrocoppering surface of low-carbon steel plate in alkaline manner |
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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 |
| CN105734630A (en) * | 2016-03-08 | 2016-07-06 | 上海大学 | Method of preparing copper-zinc-copper composite coating with high corrosion resistance on surface of low-carbon steel |
| CN106835212A (en) * | 2017-03-29 | 2017-06-13 | 南京信息工程大学 | A kind of cyanideless electro-plating nanocrystalline copper electroplate liquid and its application method |
| 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 |
| 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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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105734630A (en) * | 2016-03-08 | 2016-07-06 | 上海大学 | Method of preparing copper-zinc-copper composite coating with high corrosion resistance on surface of low-carbon steel |
| CN105734630B (en) * | 2016-03-08 | 2018-08-17 | 上海大学 | The method that the copper zinc-copper composite deposite of highly corrosion resistant is prepared in surface of low-carbon steel |
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| CN106835212B (en) * | 2017-03-29 | 2019-07-16 | 南京信息工程大学 | A kind of cyanideless electro-plating nanocrystalline copper electroplate liquid and its application method |
| 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 |