CN101724869B - Application of ion liquid addictive in watt nickel electroplating bath - Google Patents
Application of ion liquid addictive in watt nickel electroplating bath Download PDFInfo
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- CN101724869B CN101724869B CN2009102429400A CN200910242940A CN101724869B CN 101724869 B CN101724869 B CN 101724869B CN 2009102429400 A CN2009102429400 A CN 2009102429400A CN 200910242940 A CN200910242940 A CN 200910242940A CN 101724869 B CN101724869 B CN 101724869B
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- ion liquid
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Abstract
The invention discloses application of an ion liquid addictive in a watt nickel electroplating bath, belonging to the technical field of electroplating. The application is realized by the steps of: adding an ion liquid addictive and a complexing agent into a conventionally-electrplated watt nickel bath and electroplating a nickel layer on a conductive substrate at the temperature of 10-80 DEG C, wherein the concentration of the ion liquid addictive in the electroplating bath is 0.1-15g/L; the concentration of the complexing agent is 1-60g/L; the pH value of the electroplating bath is 0.5-7; and the current density is 1-50A/dm<2>. The invention can provide the nickel electroplating layer with high quality on an inductive substrate. The nickel electroplating layer prepared by the method hashigher hardness and excellent corrosion resistant performance. The microhardness HV0.02 of the nickel electroplating layer is over 380; and the corrosion speed of the nickel electroplating layer in 0.5M NaCl solution is 0.10mg<-2>h<-1>.
Description
Technical field
The invention belongs to the electroplating technology field, the application of particularly a kind of ion liquid addictive in watt nickel electroplating bath.
Background technology
Because to have sedimentation velocity with respect to chemical nickel plating fast in a watt electronickelling, cost is low, plating temperature is low and plating bath characteristics such as maintenances easily, and increasing component adopt watt electronickelling technology to carry out surfacecti proteon.But the hardness of the nickel coating that traditional watt nickel electroplating bath is prepared is lower, can not be applied to not only require wear-resisting but also require anti-corrosion Working environment.
In order to improve the hardness of watts nickel layer, traditional way is to add asccharin (C in the watt electroplate liquid
7H
5O
3Organic additive such as NS).Though this method can significantly improve the hardness of coating,, reduced the corrosion resistance nature of coating owing to contain the S element in the asccharin.
In recent years, utilize ionic liquid to improve the structure of electrodeposition of metals and the research of performance is more and more paid attention to.Characteristics such as ionic liquid has good conductivity, electrochemical window is wide, chemical stability is strong and the liquid temperature scope is wide.Therefore, seek that a kind of can to increase the ion liquid addictive that watt electroless nickel layer hardness can improve corrosion resistance coating again be the task of top priority that improves the watt electroplate liquid.
Summary of the invention
The purpose of this invention is to provide the application of a kind of ion liquid addictive in watt nickel electroplating bath.
The application of a kind of ion liquid addictive in watt nickel electroplating bath, this ion liquid addictive are ethyl group-2-hydroxyethyl-Dimethyl Ammonium tetrafluoride boron (C
2BF
4, commercially available), it is characterized in that, add ion liquid addictive and complexing agent in the watt nickel solution in routine is electroplated, electroplate liquid intermediate ion fluid additive concentration is 0.1～15g/L, and complexing agent concentration is 1～60g/L, electroplate liquid pH value is 0.5～7, and current density is 1～50A/dm
2, under 10～80 ℃ of temperature on conductive substrates electroless nickel layer, wherein, the preferred 1～30A/dm of current density
2, be preferably 1～10A/dm
2, preferred 20～70 ℃ of temperature is preferably 30～60 ℃, and electroplate liquid pH value is preferred 2～5.5, is preferably 3～5, and the preferred 0.1～3g/L of ion liquid addictive concentration is preferably 1.5～2.5g/L, the preferred 5～30g/L of complexing agent concentration.
Described complexing agent is Trisodium Citrate (C
6H
5Na
3O
7).
Each component and the content thereof of the watt nickel solution in described conventional the plating are as follows: NiSO
47H
2O:50～600g/L; NiCl
26H
2O:5～100g/L; H
3BO
3: 5～80g/L.Each component and the content thereof of the watt nickel solution in preferred conventional the plating are as follows: NiSO
47H
2O:150～450g/L; NiCl
26H
2O:20～50g/L; H
3BO
3: 20～40g/L.
Each component and content thereof are as follows in the electroplate liquid of the present invention: NiSO
47H
2O:50～600g/L; NiCl
26H
2O:5～100g/L; H
3BO
3: 5～80g/L; C
2BF
4: 0.1～3g/L; C
6H
5Na
3O
7: 1～60g/L.
A kind of optimized technical scheme is: each component and the content thereof of electroplate liquid are as follows: NiSO
47H
2O:150～450g/L; NiCl
26H
2O:20～50g/L; H
3BO
3: 20～40g/L; C
2BF
4: 1.5～2.5g/L; C
6H
5Na
3O
7: 5～30g/L.
Described conductive substrates (negative electrode) can be any conductive substrates, can be polymeric substrates or dielectric base also, is covered with one deck conductive material such as metal or carbon above it.
Used anode is that purity is 99.99% soluble nickel plate in the inventive method.
Described electroless nickel layer carries out under agitation condition, provides uniform temperature control more for " overheated " that prevent high current density region and to solution, can stir solution.During alr mode can adopt pneumatic blending, mechanical stirring, pump to take out to move with negative electrode any one.In addition, solution also can be operated under the stirring condition not having.
Electric plating method is to switch on for some time between anode in electroplate liquid and cathode substrate, and this time should be enough to electroplate required nickel coating on negative electrode.
Though embodiment is that example is described electro-plating method of the present invention to electroplate in the carbon steel substrate, but can use any conductive substrates, no matter be polymkeric substance, plastics, pure metal, metal alloy, and comprise the nonferrous alloy substrate or based on metal or mischmetal in IB, IIB, IIIA, IVA, IVB, VA, VB, VIB, VIIB or the VIIIB family element, these alloys comprise the composition of the composition of two or more these metals and element, particularly two components, three components or four component metals and element.
Beneficial effect of the present invention is: the present invention can provide the fine nickel coating on conductive substrates.The nickel coating of preparing in method of the present invention has higher hardness and excellent corrosion resistant performance.The microhardness HV of nickel coating
0.02More than 380, the erosion rate in 0.5M NaCl solution is at 0.10mgdm
-2h
-1Below.
Description of drawings
Fig. 1 is ion liquid addictive C
2BF
4The chemical structure synoptic diagram.
Embodiment
The invention will be further described below in conjunction with accompanying drawing:
Embodiment 1
Preparation contains 200g/L NiSO
47H
2O, 20g/L NiCl
26H
2O, 30g/L H
3BO
3And 10g/LC
6H
5Na
3O
7Electroplate liquid, do not add C
2BF
4Ion liquid addictive.
With 1 liter plating tank, in load onto and state electroplate liquid electronickelling coating on the S235JR carbon steel sheet, this moment, temperature was 30 ℃, and leniently stirred with air, anode is that a purity is 99.99% soluble nickel plate, average current density is about 5A/dm
2When beginning to electroplate, the pH of electroplate liquid is 4.5, electroplates when finishing, and the pH of electroplate liquid is 4.4.
Plating was carried out 30 minutes, produced the coating of 20～30 micron thickness.This coating is smooth and half light.The microhardness of coating is HV
0.02Be 362, the erosion rate in 0.5M NaCl solution is 1.56mgdm
-2h
-1
Embodiment 2
Preparation contains 300g/LNiSO
47H
2O, 15g/LNiCl
26H
2O, 30g/LH
3BO
3, 15g/L C
6H
5Na
3O
7With 2g/L C
2BF
4The improvement watt electroplate liquid of ion liquid addictive.
With 1 liter plating tank, in load onto and state electroplate liquid electronickelling coating on the S235JR carbon steel sheet, this moment, temperature was 45 ℃, and leniently stirred with air, anode is that a purity is 99.99% soluble nickel plate, average current density is about 5A/dm
2When beginning to electroplate, the pH of electroplate liquid is 4.5, electroplates when finishing, and the pH of electroplate liquid is 4.4.
Plating was carried out 30 minutes, produced the coating of 20～30 micron thickness.This coating is smooth and half light.The microhardness of coating is HV
0.02Be 407, the erosion rate in 0.5M NaCl solution is 0.09mgdm
-2h
-1
Embodiment 3
Preparation contains 300g/L NiSO
47H
2O, 15g/L NiCl
26H
2O, 30g/LH
3BO
3, 15g/L C
6H
5Na
3O
7With 1.8g/L C
2BF
4The improvement watt electroplate liquid of ion liquid addictive.
With 1 liter plating tank, in load onto and state electroplate liquid electronickelling coating on the S235JR carbon steel sheet, this moment, temperature was 45 ℃, and leniently stirred with air, anode is that a purity is 99.99% soluble nickel plate, average current density is about 5A/dm
2When beginning to electroplate, the pH of electroplate liquid is 4.5, electroplates when finishing, and the pH of electroplate liquid is 4.4.
Plating was carried out 30 minutes, produced the coating of 20～30 micron thickness.This coating is smooth and half light.The microhardness of coating is HV
0.02Be 380, the erosion rate in 0.5M NaCl solution is 0.10mgdm
-2h
-1
Embodiment 4
Preparation contains 300g/L NiSO
47H
2O, 15g/L NiCl
26H
2O, 30g/LH
3BO
3, 15g/L C
6H
5Na
3O
7With 2.5g/L C
2BF
4The improvement watt electroplate liquid of ion liquid addictive.
With 1 liter plating tank, in load onto and state electroplate liquid electronickelling coating on the S235JR carbon steel sheet, this moment, temperature was 45 ℃, and leniently stirred with air, anode is that a purity is 99.99% soluble nickel plate, average current density is about 5A/dm
2When beginning to electroplate, the pH of electroplate liquid is 4.5, electroplates when finishing, and the pH of electroplate liquid is 4.4.
Plating was carried out 30 minutes, produced the coating of 20～30 micron thickness.This coating is smooth and half light.The microhardness of coating is HV
0.02Be 442, the erosion rate in 0.5M NaCl solution is 0.07mgdm
-2h
-1
Comparative Examples 1-6
With containing 300g/L NiSO
47H
2O, 40g/L NiCl
26H
2O, 35g/LH
3BO
3, 20g/L C
6H
5Na
3O
7Electroplate liquid electroplate research temperature and C
2BF
4Ion liquid addictive content is to the influence of the microhardness and the erosion rate in 0.5M NaCl solution of six kinds of coating of gained.Current density is 3A/dm
2, the pH of electroplate liquid is 4.5 before electroplating, and thickness of coating is 25 ± 2 μ m, and comparing result is as shown in table 1.
Table 1. coating performance comparative test result
The result sums up
Do not add C in the electroplate liquid
2BF
4During ion liquid addictive, the microhardness of all coating and solidity to corrosion are all than having added C
2BF
4The prepared coating of ion liquid addictive is poor, so C
2BF
4Ion liquid addictive can significantly improve the hardness and the solidity to corrosion of coating.
In whole specification sheets, the inventor mentions various materials used among the present invention on the basis of some component, and its meaning is that these materials mainly comprise described component, or described component comprises the basal component in these materials at least.
As long as without departing from the spirit and scope of the present invention, those skilled in the art obviously can be used for various modifications and change the compositions and methods of the invention.In other words, if these improvement of the present invention and changing in the scope of appended claims and equivalent thereof, they are also included among the present invention.
Claims (9)
1. the application of ion liquid addictive in watt nickel electroplating bath, this ion liquid addictive is ethyl group-2-hydroxyethyl-Dimethyl Ammonium tetrafluoride boron, it is characterized in that, add ion liquid addictive and complexing agent in the watt nickel solution in routine is electroplated, electroplate liquid intermediate ion fluid additive concentration is 0.1～15g/L, complexing agent concentration is 1～60g/L, and electroplate liquid pH value is 0.5～7, and current density is 1～50A/dm
2, under 10～80 ℃ of temperature on conductive substrates electroless nickel layer, described complexing agent is C
6H
5Na
3O
7
2. the application of a kind of ion liquid addictive according to claim 1 in watt nickel electroplating bath is characterized in that, described electroplate liquid intermediate ion fluid additive concentration is 0.1～3g/L.
3. the application of a kind of ion liquid addictive according to claim 1 in watt nickel electroplating bath is characterized in that, described electroplate liquid intermediate ion fluid additive concentration is 1.5～2.5g/L.
4. according to claim 1,2 or 3 application of described a kind of ion liquid addictive in watt nickel electroplating bath, it is characterized in that the pH value is 2～5.5 in the described electroplate liquid, current density is 1～30A/dm
2, temperature is 20～70 ℃.
5. according to claim 1,2 or 3 application of described a kind of ion liquid addictive in watt nickel electroplating bath, it is characterized in that the pH value is 3～5 in the described electroplate liquid, current density is 1～10A/dm
2, temperature is 30～60 ℃.
6. according to claim 1,2 or 3 application of described a kind of ion liquid addictive in watt nickel electroplating bath, it is characterized in that each component and the content thereof of the watt nickel solution in described conventional the plating are as follows: NiSO
47H
2O:50～600g/L; NiCl
26H
2O:5～100g/L; H
3BO
3: 5～80g/L.
7. according to claim 1,2 or 3 application of described a kind of ion liquid addictive in watt nickel electroplating bath, it is characterized in that each component and the content thereof of the watt nickel solution in described conventional the plating are as follows: NiSO
47H
2O:150～450g/L; NiCl
26H
2O:20～50g/L; H
3BO
3: 20～40g/L.
8. the application of a kind of ion liquid addictive according to claim 1 in watt nickel electroplating bath is characterized in that each component and content thereof are as follows in the described electroplate liquid: NiSO
47H
2O:50～600g/L; NiCl
26H
2O:5～100g/L; H
3BO
3: 5～80g/L; Ethyl group-2-hydroxyethyl-Dimethyl Ammonium tetrafluoride boron: 0.1～3g/L; C
6H
5Na
3O
7: 1～60g/L.
9. the application of a kind of ion liquid addictive according to claim 1 in watt nickel electroplating bath is characterized in that each component and content thereof are as follows in the described electroplate liquid: NiSO
47H
2O:150～450g/L; NiCl
26H
2O:20～50g/L; H
3BO
3: 20～40g/L; Ethyl group-2-hydroxyethyl-Dimethyl Ammonium tetrafluoride boron: 1.5～2.5g/L; C
6H
5Na
3O
7: 5～30g/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102429400A CN101724869B (en) | 2009-12-18 | 2009-12-18 | Application of ion liquid addictive in watt nickel electroplating bath |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102429400A CN101724869B (en) | 2009-12-18 | 2009-12-18 | Application of ion liquid addictive in watt nickel electroplating bath |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101724869A CN101724869A (en) | 2010-06-09 |
| CN101724869B true CN101724869B (en) | 2011-06-22 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5887065B2 (en) * | 2010-06-29 | 2016-03-16 | ミヨシ油脂株式会社 | Hydrophilic ionic liquid |
| CN109440142B (en) * | 2018-12-29 | 2020-05-26 | 常州大学 | Additive for electroplating pearl nickel, electroplating pearl nickel solution and electroplating method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2325242A (en) * | 1997-05-14 | 1998-11-18 | Motorola Inc | Electroplating using an electrical current density modifier |
| EP1983078A1 (en) * | 2007-04-17 | 2008-10-22 | Nederlandse Organisatie voor toegepast- natuurwetenschappelijk onderzoek TNO | Electrodeposition |
| CN101384752A (en) * | 2006-02-15 | 2009-03-11 | 阿克佐诺贝尔股份有限公司 | Method to electrodeposit metals using ionic liquids |
-
2009
- 2009-12-18 CN CN2009102429400A patent/CN101724869B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2325242A (en) * | 1997-05-14 | 1998-11-18 | Motorola Inc | Electroplating using an electrical current density modifier |
| CN1204702A (en) * | 1997-05-14 | 1999-01-13 | 摩托罗拉公司 | Process for depositing layer of material on substrate and plating system |
| CN101384752A (en) * | 2006-02-15 | 2009-03-11 | 阿克佐诺贝尔股份有限公司 | Method to electrodeposit metals using ionic liquids |
| EP1983078A1 (en) * | 2007-04-17 | 2008-10-22 | Nederlandse Organisatie voor toegepast- natuurwetenschappelijk onderzoek TNO | Electrodeposition |
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Effective date of registration: 20190402 Address after: 101407 No. 11 Xingke East Street, Yanqi Economic Development Zone, Huairou District, Beijing Patentee after: Research Institute of engineering and Technology Co., Ltd. Address before: 100088, 2, Xinjie street, Beijing Patentee before: General Research Institute for Nonferrous Metals |
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