CN102828207A - Nickel electroplating solution and electroplating method thereof - Google Patents

Nickel electroplating solution and electroplating method thereof Download PDF

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CN102828207A
CN102828207A CN2012103388005A CN201210338800A CN102828207A CN 102828207 A CN102828207 A CN 102828207A CN 2012103388005 A CN2012103388005 A CN 2012103388005A CN 201210338800 A CN201210338800 A CN 201210338800A CN 102828207 A CN102828207 A CN 102828207A
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nickel
electroplating
plating solution
nickel plating
electroplating solution
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CN102828207B (en
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陈蔡喜
罗迎花
蔡志华
刘红霞
牛艳丽
黄超玉
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Guangdong Dazhi Chemical Technology Co ltd
Hunan Lingpai Technology Co ltd
Hunan Lead Power Dazhi Technology Inc
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GUANGDONG DAZHI ENVIRONMENTAL PROTECTION TECHNOLOGY Co Ltd
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Abstract

The invention provides nickel electroplating solution and an electroplating method thereof. The nickel electroplating solution comprises main salt, stabilizer, complexing agent, conducting salt and reducing agent, wherein the content of the reducing agent is 10-40g/liter. The electroplating method adopting the nickel electroplating solution comprises the following steps of: firstly, putting the metal nickel into nickel electroplating solution to serve as an anode; putting a workpiece into the nickel electroplating solution to serve as a cathode; and finally, introducing a direct-current power supply, wherein the cathode current density is 0.5-5 amperes/square centimtre, the electroplating solution temperature is 40-55DEG C, and the electroplating time is 1-10 minutes. According to the invention, the technical problems existing in the traditional electronickelling and chemical nickel-plating are solved. Reducing agent is added into the electroplating solution to obviously improve the plating solution coverage capability and the corrosion-resistant capability of a nickel layer, and the electroplating solution has the advantages of strong corrosion-resistant capability and good coverage capability.

Description

A kind of nickel plating solution and electro-plating method thereof
Technical field
The present invention relates to the metallic substance field of electroplating, be specifically related to a kind of nickel plating solution and electro-plating method thereof.
Background technology
Nickel has good ornamental and functional, is to use one of the most general plating at present.It is dissimilar to be divided into two kinds of electronickelling and chemical nickel on the technology.The advantage of electronickelling is that the coating crystallization is careful, level and smooth light, and internal stress is less, and is strong with basal body binding force.The shortcoming of electronickelling is: 1. receive the influence of cleaning and the pure degree of plating bath of matrix surface big, cause the defective of electroplating the back matrix more, for example peeling bubbles pit, stain etc.; 2. very easily receive Electropolating hangers and the different influence in position in the plating cylinder, cause covering power poor, blocking each other between the workpiece also can cause workpiece surface that the phenomenon of male and female face is arranged in addition; 3. for complex-shaped or have the workpiece of tiny deep hole or blind hole can not obtain plate surface preferably.Chemical nickel plating is claimed electroless plating or autocatalytic plating again; It is under a kind of situation that does not add external electric current; Utilize reductive agent self catalyzed reduction deposition on the activation piece surface to obtain nickel dam; This process, nickel dam has the autocatalysis ability after depositing to the activatory piece surface, so will go on automatically owing to nickel.What general chemical nickel plating obtained is alloy layer, commonly Ni-P alloy and Ni-B alloy.Compare the Ni-P alloy, the melting welding ability of Ni-B alloy is better, and eutectic temperature is high, and internal stress is less, is a kind of even more ideal chemical nickel plating mode.The advantage of chemical nickel plating is not need current and power supply equipment, the thickness even compact, and pin hole is few, and all plating property is good, and simulation capacity is strong, can be at the complicated shape surface deposition, covering power is strong, and etch resistant properties is good, and the speed of nickel plating is fast.The shortcoming of chemical nickel plating is that 1. coating is amorphous laminate structure, though after heat-treating, the coating crystallization, its laminate structure fades away, and the tensile strength of matrix metal is decreased; 2. the cost of plating bath is high, and the life-span is short, and power consumption is big; 3. plating bath is responsive to impurity, needs often to handle, thereby makes the relative complex of the operability change of technology.
Summary of the invention
In order to solve existing electronickelling and the existing technical problem of chemical nickel plating, the present invention provides a kind of nickel plating solution and electro-plating method thereof.
For realizing above-mentioned purpose, technical scheme of the present invention is following:
A kind of nickel plating solution comprises: main salt, stablizer, complexing agent and conducting salt is characterized in that: also include reductive agent; Said reductive agent content is the 10-40 grams per liter.
As the further improvement of technique scheme, said reductive agent is one or more the combination in inferior sodium phosphate, Peng Qinghuana, dimethyamine borane, diethylamine borane, the hydrazine.
As the further improvement of technique scheme, said reductive agent is an inferior sodium phosphate.
As the further improvement of technique scheme, the content of said inferior sodium phosphate is the 15-28 grams per liter.
As the further improvement of technique scheme, said main salt is one or more combination in single nickel salt, nickelous chloride, the nickel acetate.
As the further improvement of technique scheme, said main salt is nickelous chloride.
As the further improvement of technique scheme, said main salts contg is the 15-50 grams per liter.
As the further improvement of technique scheme, said nickelous chloride content is the 20-40 grams per liter.
As the further improvement of technique scheme, said stablizer is lead, cadmium ion, tin ion, contains S, Se, Te compound, oxygenatedchemicals MoO 3In one or more combinations.
As the further improvement of technique scheme, said stabiliser content is the 0.005-2 grams per liter.
As the further improvement of technique scheme, said complexing agent is one or more combinations in acetic acid, lactic acid, succsinic acid, oxysuccinic acid, Hydrocerol A, glycocoll and its esters.
As the further improvement of technique scheme, said complexing agent content is the 20-100 grams per liter.
As the further improvement of technique scheme, said conducting salt is one or more combinations in vitriolate of tartar, Potcrate, ammonium sulfate, the ammonium chloride.
As the further improvement of technique scheme, said conducting salt content is the 30-80 grams per liter.
As the further improvement of technique scheme, the pH value of said nickel plating solution is 8.0-10.0; With ammoniacal liquor or hydrochloric acid adjustment.
A kind of nickel electro-plating method that adopts nickel plating solution is characterized in that: said method comprising the steps of:
A) metallic nickel is put into the electroplating solution of nickel, as anode;
B) workpiece is put into the electroplating solution of nickel, as negative electrode;
C) feed direct supply, cathode current density 0.5-5 ampere/square decimeter, temperature of electroplating solution 40-55 ° C, electroplating time 1-10 minute.
As the further improvement of technique scheme, cathode current density is 1-3 ampere/square decimeter among the said step c; Said temperature of electroplating solution is 45-50 ° of C; Said electroplating time is 3-8 minute.
A kind of nickel plating solution and the electro-plating method thereof of embodiment of the present invention have following beneficial effect:
Through in electroplate liquid, adding reductive agent, can significantly improve the covering power and the nickel dam resistance to corrosion of plating bath, make this electroplate liquid have advantages such as the strong and covering power of resistance to corrosion is good.
Embodiment:
But do not constitute to any restriction of the present invention.
The present invention provides a kind of nickel plating solution, comprises main salt, stablizer, complexing agent and conducting salt, reductive agent; Reductive agent content is the 10-40 grams per liter.Reductive agent is one or more the combination in inferior sodium phosphate, Peng Qinghuana, dimethyamine borane, diethylamine borane, the hydrazine.Reductive agent is preferably inferior sodium phosphate, and the content of this sodium phosphite is the 15-28 grams per liter.Main salt is one or more combination in single nickel salt, nickelous chloride, the nickel acetate, and main salts contg is the 15-50 grams per liter.Main salt is preferably nickelous chloride, and nickelous chloride content is the 20-40 grams per liter.Stablizer is lead, cadmium ion, tin ion, contains S, Se, Te compound, oxygenatedchemicals MoO 3In one or more combinations, this stabiliser content is the 0.005-2 grams per liter.Complexing agent is one or more combinations in acetic acid, lactic acid, succsinic acid, oxysuccinic acid, Hydrocerol A, glycocoll and its esters, and complexing agent content is the 20-100 grams per liter.Conducting salt is one or more combinations in vitriolate of tartar, Potcrate, ammonium sulfate, the ammonium chloride, and conducting salt content is the 30-80 grams per liter.The pH value of this nickel plating solution is 8.0-10.0, and with ammoniacal liquor or hydrochloric acid adjustment.
The electro-plating method of employing nickel plating solution provided by the invention, this method may further comprise the steps: step 1, metallic nickel is put into the electroplating solution of above-mentioned a kind of functional nickel, as anode; Step 2 is put into the electroplating solution of above-mentioned a kind of functional nickel with workpiece, as negative electrode; Step 3 feeds direct supply, cathode current density 0.5-5 ampere/square decimeter, temperature of electroplating solution 40-55 ° C, electroplating time 1-10 minute; Wherein, middle cathode current density is preferably 1-3 ampere/square decimeter; Temperature of electroplating solution is preferably 45-50 ° of C; Electroplating Best Times is 3-8 minute.
Below in conjunction with specific embodiment the present invention is done further detailed description,
Embodiment 1
Electroplating bath components:
Surplus is a water
Electro-plating method: adopting internal diameter is the thin-walled iron pipe of Ф 10X100mm, in the beaker of 1000ml, electroplates test, and condition is: 50 ℃ of temperature, galvanic current are 1 ampere, electroplated 8 minutes, and anode uses the nickel plate, obtains nickeling layer iron pipe A1.
Electroplating effect is estimated: the length that observation iron pipe inwall plates nickel dam is 100mm, and then estimates the covering power of plating bath.Nickeling layer iron pipe A1 did neutral salt spray test 8 hours, did not see the nickel dam corrosion.
Embodiment 2
Electroplating bath components:
Surplus is a water
Electro-plating method: adopting internal diameter is the thin-walled iron pipe of Ф 10X100mm, in the beaker of 1000ml, electroplates test, and condition is: 55 ℃ of temperature, galvanic current are 0.5 ampere, electroplated 7 minutes, and anode uses the nickel plate, obtains nickeling layer iron pipe A2.
Electroplating effect is estimated: the length that observation iron pipe inwall plates nickel dam is 100mm, and then estimates the covering power of plating bath.Nickeling layer iron pipe A2 did neutral salt spray test 7 hours, did not see the nickel dam corrosion.
Embodiment 3
Electroplating bath components:
Figure BDA00002133197600042
Surplus is a water
Electro-plating method: adopting internal diameter is the thin-walled iron pipe of Ф 10X100mm, in the beaker of 1000ml, electroplates test, and condition is: 55 ℃ of temperature, galvanic current are 0.5 ampere, electroplated 7 minutes, and anode uses the nickel plate, obtains nickeling layer iron pipe A3.
Electroplating effect is estimated: the length that observation iron pipe inwall plates nickel dam is 100mm, and then estimates the covering power of plating bath.Nickeling layer iron pipe A3 did neutral salt spray test 7 hours, did not see the nickel dam corrosion.
Embodiment 4
Electroplating bath components:
Figure BDA00002133197600051
Surplus is a water
Electro-plating method: adopting internal diameter is the thin-walled iron pipe of Ф 10X100mm, in the beaker of 1000ml, electroplates test, and condition is: 45 ℃ of temperature, galvanic current are 1.5 amperes, electroplated 10 minutes, and anode uses the nickel plate, obtains nickeling layer iron pipe A4.
Electroplating effect is estimated: the length that observation iron pipe inwall plates nickel dam is 100mm, and then estimates the covering power of plating bath.Nickeling layer iron pipe A4 did neutral salt spray test 10 hours, did not see the nickel dam corrosion.
Embodiment 5
Electroplating bath components:
Surplus is a water
Electro-plating method: adopting internal diameter is the thin-walled iron pipe of Ф 10X100mm, in the beaker of 1000ml, electroplates test, and condition is: 50 ℃ of temperature, galvanic current are 0.8 ampere, electroplated 5 minutes, and anode uses the nickel plate, obtains nickeling layer iron pipe A5.
Electroplating effect is estimated: the length that observation iron pipe inwall plates nickel dam is 100mm, and then estimates the covering power of plating bath.Nickeling layer iron pipe A5 did neutral salt spray test 10 hours, did not see the nickel dam corrosion.
Embodiment 6
Electroplating bath components:
Figure BDA00002133197600061
Surplus is a water
Electro-plating method: adopting internal diameter is the thin-walled iron pipe of Ф 10X100mm, in the beaker of 1000ml, electroplates test, and condition is: 50 ℃ of temperature, galvanic current are 1.5 amperes, electroplated 4 minutes, and anode uses the nickel plate, obtains nickeling layer iron pipe A6.
Electroplating effect is estimated: the length that observation iron pipe inwall plates nickel dam is 100mm, and then estimates the covering power of plating bath.Nickeling layer iron pipe A6 did neutral salt spray test 8 hours, did not see the nickel dam corrosion.
Embodiment 7
Electroplating bath components:
Figure BDA00002133197600062
Surplus is a water
Electro-plating method: adopting internal diameter is the thin-walled iron pipe of Ф 10X100mm, in the beaker of 1000ml, electroplates test, and condition is: 50 ℃ of temperature, galvanic current are 1.5 amperes, electroplated 9 minutes, and anode uses the nickel plate, obtains nickeling layer iron pipe A7.
Electroplating effect is estimated: the length that observation iron pipe inwall plates nickel dam is 100mm, and then estimates the covering power of plating bath.Nickeling layer iron pipe A7 did neutral salt spray test 11 hours, did not see the nickel dam corrosion.
Embodiment 8
Electroplating bath components:
Figure BDA00002133197600071
Surplus is a water
Regulating pH is 10.0
Electro-plating method: adopting internal diameter is the thin-walled iron pipe of Ф 10X100mm, in the beaker of 1000ml, electroplates test, and condition is: 50 ℃ of temperature, galvanic current are 1.5 amperes, electroplated 10 minutes, and anode uses the nickel plate, obtains nickeling layer iron pipe A8.
Electroplating effect is estimated: the length that observation iron pipe inwall plates nickel dam is 100mm, and then estimates the covering power of plating bath.Nickeling layer iron pipe A8 did neutral salt spray test 12 hours, did not see the nickel dam corrosion.
Embodiment 9
Electroplating bath components:
Figure BDA00002133197600072
Surplus is a water
Regulating pH is 8.0
Electro-plating method: adopting internal diameter is the thin-walled iron pipe of Ф 10X100mm, in the beaker of 1000ml, electroplates test, and condition is: 50 ℃ of temperature, galvanic current are 1.0 amperes, electroplated 5 minutes, and anode uses the nickel plate, obtains nickeling layer iron pipe A9.
Electroplating effect is estimated: the length that observation iron pipe inwall plates nickel dam is 100mm, and then estimates the covering power of plating bath.Nickeling layer iron pipe A9 did neutral salt spray test 8 hours, did not see the nickel dam corrosion.
Comparative Examples 1
Electroplating bath components: the watt nickel prescription that adopts the public to use always.
Electro-plating method: adopting internal diameter is the thin-walled iron pipe of Ф 10X100mm, in the beaker of 1000ml, electroplates test, and condition is: 50 ℃ of temperature, galvanic current are 1.0 amperes, electroplated 8 minutes, and anode uses the nickel plate, obtains nickeling layer iron pipe B1.
Electroplating effect is estimated: the length that observation iron pipe inwall plates nickel dam is 50mm, and then estimates the covering power of plating bath.Nickeling layer iron pipe B1 did neutral salt spray test 5 hours, did not see the nickel dam corrosion.
The above-mentioned nickeling layer iron pipe that obtains is done neutral salt spray test, result such as table 1.
Table 1 electroplating effect evaluation table
Figure BDA00002133197600081
Embodiment 1-9 plating bath contains inferior sodium phosphate, and the plating bath of Comparative Examples 1 does not contain inferior sodium phosphate, and the endoporus of embodiment 1-9 plates nickel dam length and reaches 100 millimeters, much larger than 50 millimeters of Comparative Examples 1.The present invention is through adding inferior sodium phosphate in plating bath in this explanation, can significantly improve the covering power of plating bath.Embodiment 1-9 neutral salt spray test can reach 7-12 hour does not see corrosion, and greater than Comparative Examples 1 neutral salt spray test 5 hours, the present invention was through in plating bath, adding inferior sodium phosphate in this explanation, obviously improves the nickel dam resistance to corrosion.In sum, functional nickel electro-plating method provided by the invention, it is strong to have covering power, the advantage that resistance to corrosion is strong.
The above embodiments are merely the preferred embodiments of the present invention, can not limit interest field of the present invention with this, and therefore, the equivalent variations according to claim of the present invention is done still belongs to the scope that the present invention is contained.

Claims (10)

1. nickel plating solution, comprising: main salt, stablizer, complexing agent and conducting salt is characterized in that: also include reductive agent; Reductive agent is one or more the combination in inferior sodium phosphate, Peng Qinghuana, dimethyamine borane, diethylamine borane, the hydrazine, and said reductive agent content is the 10-40 grams per liter.
2. nickel plating solution according to claim 1 is characterized in that: said main salt is one or more combination in single nickel salt, nickelous chloride, the nickel acetate, and said main salts contg is the 15-50 grams per liter.
3. nickel plating solution according to claim 2 is characterized in that: said nickelous chloride content is the 20-40 grams per liter.
4. nickel plating solution according to claim 1 is characterized in that: said stablizer is lead, cadmium ion, tin ion, contains S, Se, Te compound, oxygenatedchemicals MoO 3In one or more combinations.
5. nickel plating solution according to claim 4 is characterized in that: said stabiliser content is the 0.005-2 grams per liter.
6. nickel plating solution according to claim 1 is characterized in that: said complexing agent is one or more combinations in acetic acid, lactic acid, succsinic acid, oxysuccinic acid, Hydrocerol A, glycocoll and its esters, and said complexing agent content is the 20-100 grams per liter.
7. nickel plating solution according to claim 1 is characterized in that: said conducting salt is one or more combinations in vitriolate of tartar, Potcrate, ammonium sulfate, the ammonium chloride, and said conducting salt content is the 30-80 grams per liter.
8. according to the described nickel plating solution of claim 1-7, it is characterized in that: the pH value of said nickel plating solution is 8.0-10.0; With ammoniacal liquor or hydrochloric acid adjustment.
9. one kind as adopting the electro-plating method of nickel plating solution in the arbitrary claim of claim 1-8, it is characterized in that: said method comprising the steps of:
1) metallic nickel is put into the electroplating solution of nickel, as anode;
2) workpiece is put into the electroplating solution of nickel, as negative electrode;
3) feed direct supply, cathode current density 0.5-5 ampere/square decimeter, temperature of electroplating solution 40-55 ° C, electroplating time 1-10 minute.
10. the electro-plating method of employing nickel plating solution according to claim 9 is characterized in that: cathode current density is 1-3 ampere/square decimeter in the said step 3; Said temperature of electroplating solution is 45-50 ° of C; Said electroplating time is 3-8 minute.
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CN104773794A (en) * 2015-04-30 2015-07-15 湖南富莱明节能环保科技有限公司 Composite additive for electrolysis
CN104862763A (en) * 2015-06-21 2015-08-26 李文东 Workpiece surface treatment liquid and using method thereof
CN105002525A (en) * 2015-08-21 2015-10-28 无锡桥阳机械制造有限公司 Semi-bright nickel plating solution
CN105040057A (en) * 2015-07-21 2015-11-11 安徽江威精密制造有限公司 Aluminum piece silver plating method
CN105239112A (en) * 2015-11-03 2016-01-13 江苏梦得电镀化学品有限公司 Electroplating process for high-performance direct-plating nickel plating solutions
CN106119910A (en) * 2016-08-31 2016-11-16 佛山市仁昌科技有限公司 A kind of nano nickel solution and utilize it that communication filter is carried out electric plating method
CN106283128A (en) * 2016-08-04 2017-01-04 浙江工业大学义乌科学技术研究院有限公司 A kind of method of electrolytic preparation bright nickel in alkaline electrolyte
CN106937491A (en) * 2017-04-05 2017-07-07 广东浪潮大数据研究有限公司 One kind is based on pcb board card gold finger galvanizing nickel and plating gold process and its application
CN107058988A (en) * 2017-04-20 2017-08-18 上海丰豫新材料科技有限公司 A kind of chemical nickel plating tungsten phosphorus formula
CN107460506A (en) * 2017-09-29 2017-12-12 佛山市春暖花开科技有限公司 A kind of electroplate liquid of nickel
CN107829114A (en) * 2017-11-28 2018-03-23 江苏澳光电子有限公司 A kind of terminal surfaces electroplate liquid and its application
CN110076071A (en) * 2019-03-21 2019-08-02 苏州铁博士金属制品有限公司 A kind of preparation method of high-wearing feature aluminum alloy materials
CN110144608A (en) * 2019-06-13 2019-08-20 苏州普雷特电子科技有限公司 A kind of nickel plating solution and nickel plating process applied to plating processing
CN110756924A (en) * 2019-10-12 2020-02-07 哈尔滨飞机工业集团有限责任公司 Electrochemical cutting method for nickel-coated blade
CN111876797A (en) * 2020-07-08 2020-11-03 佛山亚特表面技术材料有限公司 High-corrosion-resistance neutral nickel plating solution and neutral nickel priming process
CN114808048A (en) * 2021-05-31 2022-07-29 上海亿尚金属有限公司 Chemical nickel electroplating solution and electroplating process thereof
CN114808048B (en) * 2021-05-31 2024-04-30 上海亿尚金属有限公司 Electroless nickel plating solution and plating process thereof

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CN104773794A (en) * 2015-04-30 2015-07-15 湖南富莱明节能环保科技有限公司 Composite additive for electrolysis
CN104862763A (en) * 2015-06-21 2015-08-26 李文东 Workpiece surface treatment liquid and using method thereof
CN105040057A (en) * 2015-07-21 2015-11-11 安徽江威精密制造有限公司 Aluminum piece silver plating method
CN105002525A (en) * 2015-08-21 2015-10-28 无锡桥阳机械制造有限公司 Semi-bright nickel plating solution
CN105239112A (en) * 2015-11-03 2016-01-13 江苏梦得电镀化学品有限公司 Electroplating process for high-performance direct-plating nickel plating solutions
CN106283128A (en) * 2016-08-04 2017-01-04 浙江工业大学义乌科学技术研究院有限公司 A kind of method of electrolytic preparation bright nickel in alkaline electrolyte
CN106119910A (en) * 2016-08-31 2016-11-16 佛山市仁昌科技有限公司 A kind of nano nickel solution and utilize it that communication filter is carried out electric plating method
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CN107058988A (en) * 2017-04-20 2017-08-18 上海丰豫新材料科技有限公司 A kind of chemical nickel plating tungsten phosphorus formula
CN107460506A (en) * 2017-09-29 2017-12-12 佛山市春暖花开科技有限公司 A kind of electroplate liquid of nickel
CN107829114A (en) * 2017-11-28 2018-03-23 江苏澳光电子有限公司 A kind of terminal surfaces electroplate liquid and its application
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CN110144608A (en) * 2019-06-13 2019-08-20 苏州普雷特电子科技有限公司 A kind of nickel plating solution and nickel plating process applied to plating processing
CN110756924A (en) * 2019-10-12 2020-02-07 哈尔滨飞机工业集团有限责任公司 Electrochemical cutting method for nickel-coated blade
CN110756924B (en) * 2019-10-12 2021-02-09 哈尔滨飞机工业集团有限责任公司 Electrochemical cutting method for nickel-coated blade
CN111876797A (en) * 2020-07-08 2020-11-03 佛山亚特表面技术材料有限公司 High-corrosion-resistance neutral nickel plating solution and neutral nickel priming process
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CN114808048B (en) * 2021-05-31 2024-04-30 上海亿尚金属有限公司 Electroless nickel plating solution and plating process thereof

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