CN101260551B - Non-cyanide silver electroplating method - Google Patents
Non-cyanide silver electroplating method Download PDFInfo
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- CN101260551B CN101260551B CN2008100110059A CN200810011005A CN101260551B CN 101260551 B CN101260551 B CN 101260551B CN 2008100110059 A CN2008100110059 A CN 2008100110059A CN 200810011005 A CN200810011005 A CN 200810011005A CN 101260551 B CN101260551 B CN 101260551B
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- solution
- nickel layer
- plating
- silver
- electroplating
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Links
- 238000009713 electroplating Methods 0.000 title claims abstract description 29
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 21
- 239000004332 silver Substances 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 15
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 68
- 238000007747 plating Methods 0.000 claims abstract description 37
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 34
- 239000000463 material Substances 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 4
- PVNIIMVLHYAWGP-UHFFFAOYSA-N Niacin Chemical compound OC(=O)C1=CC=CN=C1 PVNIIMVLHYAWGP-UHFFFAOYSA-N 0.000 claims description 34
- 230000004913 activation Effects 0.000 claims description 26
- 229960003512 nicotinic acid Drugs 0.000 claims description 17
- 235000001968 nicotinic acid Nutrition 0.000 claims description 17
- 239000011664 nicotinic acid Substances 0.000 claims description 17
- 101710134784 Agnoprotein Proteins 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 10
- LFAGQMCIGQNPJG-UHFFFAOYSA-N silver cyanide Chemical compound [Ag+].N#[C-] LFAGQMCIGQNPJG-UHFFFAOYSA-N 0.000 claims description 10
- 238000003672 processing method Methods 0.000 claims description 7
- 238000011010 flushing procedure Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 230000005611 electricity Effects 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims description 2
- VXHVELPLHCCGQL-UHFFFAOYSA-N pyridine-3-carboxylic acid;silver Chemical compound [Ag].OC(=O)C1=CC=CN=C1 VXHVELPLHCCGQL-UHFFFAOYSA-N 0.000 abstract 1
- 239000011248 coating agent Substances 0.000 description 18
- 238000000576 coating method Methods 0.000 description 18
- 239000003795 chemical substances by application Substances 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 229910017053 inorganic salt Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 239000003115 supporting electrolyte Substances 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- 208000006558 Dental Calculus Diseases 0.000 description 1
- 241000080590 Niso Species 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 238000005282 brightening Methods 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- RWPGFSMJFRPDDP-UHFFFAOYSA-L potassium metabisulfite Chemical compound [K+].[K+].[O-]S(=O)S([O-])(=O)=O RWPGFSMJFRPDDP-UHFFFAOYSA-L 0.000 description 1
- 235000010263 potassium metabisulphite Nutrition 0.000 description 1
- 125000000561 purinyl group Chemical class N1=C(N=C2N=CNC2=C1)* 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- PODWXQQNRWNDGD-UHFFFAOYSA-L sodium thiosulfate pentahydrate Chemical compound O.O.O.O.O.[Na+].[Na+].[O-]S([S-])(=O)=O PODWXQQNRWNDGD-UHFFFAOYSA-L 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
Landscapes
- Electroplating And Plating Baths Therefor (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
The invention relates to a method for cyanides-free silver electroplating, wherein, firstly, the surface of base materials is plated with nickel; secondly, a nickel layer is electrically activated in acid solution; thirdly, after chemical silver electroplating, double-pulse silver electroplating is performed in a nicotinic acid silver electroplating system. After processed by adoption of the method, the surface of the base materials obtains a compact silver plating layer with good binding force.
Description
Technical field
The present invention relates to electroplating technology, be specifically related to the method for non-cyanide silver electroplating.
Background technology
Electrosilvering is widely used in electron device, semi-conductor, instrument, decoration and other functional silver-plated fields.At present, electrosilvering is still silver-plated based on the prussiate system both at home and abroad.Because the prussiate environmental pollution is serious, along with the continuous enhancing of people's environmental consciousness, having cyanogen to electroplate will be eliminated gradually.Existing patent documentation discloses the processing method of non-cyanide silver coating in the prior art, and relevant patent is as follows:
Patent 200510023573 relates to a kind of non-cyanide silver coating processing method, and it is the non-cyanide silver coating processing method under magnetic field and pulsed current effect.This method comprises following technological process and step: plating piece electrochemical deoiling, chemistry remove embroidery, bright nickel plating, activation treatment, soak silver, pulse silver-coating, Passivation Treatment, drying, finally make silver-plated finished product.Activation treatment adopts chemical process, and the complexing agent that soaks silver-colored solution is a thiocarbamide, and the prescription of pulse plating silvering solution is: Silver Nitrate 50-60g/L, Sulfothiorine 250-350g/L, potassium pyrosulfite 90-110g/L, vitriolate of tartar 20-30g/L, boric acid 25-35g/L, brightening agent 5ml/L.
Patent 200710009207 relates to a kind of non-cyanide silver coating plating bath, the mass concentration that it is characterized in that each component of composition of raw materials of described electroplate liquid is: the inorganic salt or the organic salt 1-200g/L that contain silver, purine class coordination agent 1-800g/L, supporting electrolyte 1-200g/L, plating bath pH regulator agent 0-550g/L and electroplating additive system.
Patent 200710009208 relates to a kind of silver plated non-cyanogen type electroplating solution that is used for, the mass concentration that it is characterized in that each component of composition of raw materials of described electroplate liquid is: the inorganic salt or the organic salt 1-200g/L that contain silver, miazines coordination agent 1-800g/L, supporting electrolyte 1-200g/L, plating bath pH regulator agent 0-550g/L and electroplating additive system.
Summary of the invention
The object of the present invention is to provide a kind of method of non-cyanide silver electroplating, to obtain good, the fine and close silvered film of bonding force.For achieving the above object, the technical solution used in the present invention is: a kind of method of non-cyanide silver electroplating, comprise: with substrate material surface nickel plating, nickel layer activation treatment, electrosilvering on nickel layer, the nickel layer activation treatment is with nickel layer electric activation treatment in acid solution, the electrosilvering method be included on the nickel layer chemical silvering and in nicotinic acid electrosilvering system double-pulse plating silver, it is characterized in that the method for described electricity activation nickel layer is: the body material of plating nickel on surface is put into H is housed
2SO
4In the electric activated bath of solution, H
2SO
4Solution is every liter of H
2SO
4The H that contains the 80-250 milliliter in the solution
2SO
4, H
2SO
4Concentration is 98%, and solution temperature remains on 4-8 ℃, and electric activatory cathode current density is 1-2.5A/dm
2, electric soak time is 1-5min, the activation back is taken out clean with flushing with clean water; Described chemical silvering processing method is: the body material after the nickel layer activation is put into Na is housed
2SO
3And AgNO
3In the plating tank of mixing solutions, Na in every liter of mixing solutions in the plating tank
2SO
3Content is 100-200g, AgNO
3Content is 0.8-1.5g, and solution temperature keeps 12-25 ℃, and electroplating time is 5-60s; Described in nicotinic acid electrosilvering system the processing method of double-pulse plating silver be: the nicotinic acid plating silver solution is by nicotinic acid: 80-150g/L, AgNO
3: 20-55g/L, K
2CO
3: 60-100g/L, KOH:40-65g/L, NH
4AC:60-80g/L, NH
3H
2O:15-40ml/L forms, and the electroplating solution temperature remains on 12-25 ℃, and the forward pulsewidth of Double-pulse Plating Power Source is 2ms, and dutycycle is 20%, and the working hour is 100ms; Oppositely pulsewidth is 1ms, and dutycycle is 10%, and the working hour is 10ms, electroplating time 0.5-6h.
The present invention has following advantage:
1. guaranteed bonding force by electrochemical activation, non-cyanide silver coating is applied, thereby farthest reduced pollution environment.
2. the use of Double-pulse Plating Power Source when improving corrosion resistance, also can effectively reduce thickness of coating, saves cost.
Embodiment
Embodiment 1
Electrosilvering on the stainless steel.Stainless model is 316L.Remove the oxide film on surface, dipping 30min makes surface active, 12 ℃ of acid solution temperature in 100ml/L hydrochloric acid (d=1.19).Electronickelling is adopted at NiSO
47H
2O:270g/L, NiCl
27H
2O:50g/L, H
3BO
3: carry out in the plating bath of 35g/L, electroplating technology is: electroplating temperature: 20 ℃, and electroplating time: 3min, cathodic current: 2.0A/dm
2The electrochemical activation nickel layer carries out in electric activated bath, the material after the nickel plating is put into H is housed
2SO
4In the electric activated bath of solution, H
2SO
4Solution is every liter of H
2SO
4Contain 100 milliliters H in the solution
2SO
4, H
2SO
4Concentration is 98%, and solution temperature remains on 8 ℃, and electric activatory cathode current density is 1.5A/dm
2, electric soak time is 5min, the activation back is taken out clean with flushing with clean water.Carry out chemical silvering again, the material after the nickel layer activation is put into Na is housed
2SO
3And AgNO
3In the coating bath of mixing solutions, Na in every liter of mixing solutions in the coating bath
2SO
3Content is 150g, AgNO
3Content is 0.8g, and solution temperature keeps 25 ℃, and the silver-plated time is 5s.Double-pulse plating silver in nicotinic acid electrosilvering system at last, the nicotinic acid plating silver solution is by nicotinic acid: 100g/L, AgNO
3: 35g/L, K
2CO
3: 80g/L, KOH:55g/L, NH
4AC:70g/L, NH
3H
2O:30ml/L forms, and the electroplating solution temperature remains on 25 ℃, electroplating time 3h, and the forward pulsewidth of Double-pulse Plating Power Source is 2ms, and dutycycle is 20%, and the working hour is 100ms; Oppositely pulsewidth is 1ms, and dutycycle is 10%, and the working hour is 10ms.
Embodiment 2
Electrosilvering on copper.At first, adopt usual way on copper, to electroplate one deck nickel, electrochemical activation nickel layer then, the electrochemical activation nickel layer carries out in electric activated bath, the copper after the nickel plating is put into H is housed
2SO
4In the electric activated bath of solution, H
2SO
4Solution is every liter of H
2SO
4Contain 250 milliliters H in the solution
2SO
4, H
2SO
4Concentration is 98%, and solution temperature remains on 4 ℃, and electric activatory cathode current density is 1.0A/dm
2, electric soak time is 1min, the activation back is taken out clean with flushing with clean water.Carry out chemical silvering again, the copper after the nickel layer activation is put into Na is housed
2SO
3And AgNO
3In the coating bath of mixing solutions, Na in every liter of mixing solutions in the coating bath
2SO
3Content is 100g, AgNO
3Content is 1g, and solution temperature keeps 20 ℃, and the silver-plated time is 30s.Double-pulse plating silver in nicotinic acid electrosilvering system at last, the nicotinic acid plating silver solution is by nicotinic acid: 150g/L, AgNO
3: 55g/L, K
2CO
3: 100g/L, KOH:65g/L, NH
4AC:80g/L, NH
3H
2O:40ml/L forms, and the electroplating solution temperature remains on 20 ℃, electroplating time 0.5h, and the forward pulsewidth of Double-pulse Plating Power Source is 2ms, and dutycycle is 20%, and the working hour is 100ms; Oppositely pulsewidth is 1ms, and dutycycle is 10%, and the working hour is 10ms.
Embodiment 3
Electrosilvering on pure titanium.Adopt usual method on pure titanium, to electroplate one deck nickel, electrochemical activation nickel layer then, the electrochemical activation nickel layer carries out in electric activated bath, the titanium after the nickel plating is put into H is housed
2SO
4In the electric activated bath of solution, H
2SO
4Solution is every liter of H
2SO
4Contain 80 milliliters H in the solution
2SO
4, H
2SO
4Concentration is 98%, and solution temperature remains on 6 ℃, and electric activatory cathode current density is 2.5A/dm
2, electric soak time is 3min, the activation back is taken out clean with flushing with clean water.Carry out chemical silvering again, the titanium after the nickel layer activation is put into Na is housed
2SO
3And AgNO
3In the coating bath of mixing solutions, Na in every liter of mixing solutions in the coating bath
2SO
3Content is 200g, AgNO
3Content is 1.5g, and solution temperature keeps 12 ℃, and the silver-plated time is 60s.Double-pulse plating silver in nicotinic acid electrosilvering system at last, the nicotinic acid plating silver solution is by nicotinic acid: 80g/L, AgNO
3: 20g/L, K
2CO
3: 60g/L, KOH:40g/L, NH
4AC:60g/L, NH
3H
2O:15ml/L forms, and the electroplating solution temperature remains on 12 ℃, electroplating time 6h, and the forward pulsewidth of Double-pulse Plating Power Source is 2ms, and dutycycle is 20%, and the working hour is 100ms; Oppositely pulsewidth is 1ms, and dutycycle is 10%, and the working hour is 10ms.
The coating of the foregoing description all passes through following test:
1) outward appearance
Coating outward appearance even compact, light, defectives such as no peeling, bubbling, spot.200 times of 3D renderings that adopt super degree of depth surface somatometry of physique microscope to be obtained show that the coating microcosmic is wavy, the imporosity, and the planeness of whole silvered film is 4 μ m.
2) bonding force
Draw some the dark cuts that reach matrix with scriber on coating, these cuts are parallel to each other and interlock, and distance is not more than 2mm between cut, does not observe phenomenons such as the coating peeling comes off.
Claims (1)
1. the method for a non-cyanide silver electroplating, comprise: with substrate material surface nickel plating, nickel layer activation treatment, electrosilvering on nickel layer, the nickel layer activation treatment is with nickel layer electric activation treatment in acid solution, the electrosilvering method be included on the nickel layer chemical silvering and in nicotinic acid electrosilvering system double-pulse plating silver, it is characterized in that the method for described electricity activation nickel layer is: the body material of plating nickel on surface is put into H is housed
2SO
4In the electric activated bath of solution, H
2SO
4Solution is every liter of H
2SO
4The H that contains the 80-250 milliliter in the solution
2SO
4, H
2SO
4Concentration is 98%, and solution temperature remains on 4-8 ℃, and electric activatory cathode current density is 1-2.5A/dm
2, electric soak time is 1-5min, the activation back is taken out clean with flushing with clean water; Described chemical silvering processing method is: the body material after the nickel layer activation is put into Na is housed
2SO
3And AgNO
3In the plating tank of mixing solutions, Na in every liter of mixing solutions in the plating tank
2SO
3Content is 100-200g, AgNO
3Content is 0.8-1.5g, and solution temperature keeps 12-25 ℃, and electroplating time is 5-60s; Described in nicotinic acid electrosilvering system the processing method of double-pulse plating silver be: the nicotinic acid plating silver solution is by nicotinic acid: 80-150g/L, AgNO
3: 20-55g/L, K
2CO
3: 60-100g/L, KOH:40-65g/L, NH
4AC:60-80g/L, NH
3H
2O:15-40ml/L forms, and the electroplating solution temperature remains on 12-25 ℃, and the forward pulsewidth of Double-pulse Plating Power Source is 2ms, and dutycycle is 20%, and the working hour is 100ms; Oppositely pulsewidth is 1ms, and dutycycle is 10%, and the working hour is 10ms, electroplating time 0.5-6h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100110059A CN101260551B (en) | 2008-04-11 | 2008-04-11 | Non-cyanide silver electroplating method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100110059A CN101260551B (en) | 2008-04-11 | 2008-04-11 | Non-cyanide silver electroplating method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101260551A CN101260551A (en) | 2008-09-10 |
| CN101260551B true CN101260551B (en) | 2010-06-09 |
Family
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|---|---|---|---|
| CN2008100110059A Expired - Fee Related CN101260551B (en) | 2008-04-11 | 2008-04-11 | Non-cyanide silver electroplating method |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5346965B2 (en) * | 2011-02-08 | 2013-11-20 | Ｄｏｗａメタルテック株式会社 | Silver plating material and method for producing the same |
| CN102181892B (en) * | 2011-05-18 | 2012-07-25 | 中国电子科技集团公司第三十八研究所 | Method for improving bonding force of non-cyanide silver plating layer on nickel layer |
| CN103436931A (en) * | 2013-08-26 | 2013-12-11 | 中国人民解放军第五七一九工厂 | Bidirectional pulse silver-plating method |
| US10889907B2 (en) | 2014-02-21 | 2021-01-12 | Rohm And Haas Electronic Materials Llc | Cyanide-free acidic matte silver electroplating compositions and methods |
| CN107419267A (en) * | 2017-07-21 | 2017-12-01 | 广东欧珀移动通信有限公司 | Terminal enclosure, electronic equipment and terminal enclosure processing technology |
| CN107541759A (en) * | 2017-09-05 | 2018-01-05 | 江小平 | A kind of method for combining stainless steel with silver |
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| CN1286321A (en) * | 1999-09-01 | 2001-03-07 | 中国科学院金属研究所 | Process for plating flexible graphite products with thick silver layer |
| CN1680630A (en) * | 2005-01-26 | 2005-10-12 | 上海大学 | Technology of non-cyanide silver coating |
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- 2008-04-11 CN CN2008100110059A patent/CN101260551B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1286321A (en) * | 1999-09-01 | 2001-03-07 | 中国科学院金属研究所 | Process for plating flexible graphite products with thick silver layer |
| CN1680630A (en) * | 2005-01-26 | 2005-10-12 | 上海大学 | Technology of non-cyanide silver coating |
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| Publication number | Publication date |
|---|---|
| CN101260551A (en) | 2008-09-10 |
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