CN104630853A - Method for electroplating black nickel on neodymium-iron-boron magnet - Google Patents
Method for electroplating black nickel on neodymium-iron-boron magnet Download PDFInfo
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Abstract
The present invention provides a method for electroplating black nickel on a neodymium-iron-boron magnet. The method comprises: electroplating nickel-copper-nickel according to the conventional method; activating the neodymium-iron-boron magnet plated with the nickel-copper-nickel for black nickel electroplating; and plating black nickel, wherein a black nickel electroplating liquid is used to electroplate black nickel on the activated neodymium-iron-boron magnet plated with the nickel-copper-nickel, and comprises, by mass, 2 parts of nickel chloride, 1 part of stannous sulfate, 0.4 part of a complexing agent, 0.6 part of a blackening agent, and 0.1 part of cobalt sulfate.
Description
Technical field
The present invention relates to a kind of method at neodymium iron boron magnetic body black nickel plating.
Background technology
The application and development of rare-earth Nd-Fe-B (NdFeB) permanent magnet is very rapid in recent years, but the solidity to corrosion of Nd-Fe-B permanent magnet is very poor, very easily corrodes in wet condition.Once corrode, the magnetic property of magnet will decline, thus reduces the reliability and stability of product.Therefore, the application prerequisite of NdFeB material resolves the Anticorrosion of NdFeB material.
The anti-corrosion method of NdFeB material mainly contains plating, phosphatization, electrophoresis etc. at present.Owing to having, protective capacities is strong, the advantage of process stabilizing in plating, and is used as the anti-corrosion method of most of NdFeB material.Conventional neodymium iron boron electroplating technology is plating ambrose alloy nickel (Ni-Cu-Ni) technique, namely first at NdFeB material surface preplating one deck nickel, then in middle layer copper facing, finally electroplates dark nickel and bright nickel on top layer.The outer nickel plating of common process is silvery white, and same size neodymium iron boron workpiece often has different performance, mixes very easily mutually when client assembles.
In recent years, a kind of black nickel coating is used to Nd-Fe-B magnetic material because having well ornamental, and this black coating can distinguish with the white coating of routine, thus distinguishes measure-alike but performance or the different product of purposes, avoids mutually obscuring when using.
The mode of usual employing plating or electroless plating prepares black nickel coating, but has that corrosion resistance of coating difference, bonding force are bad, the shortcoming of the soft easy scuffing of coating.Because NdFeB material very easily corrodes, so the black nickel coating of routine is difficult to be applied in NdFeB material.
The open CN101054697A of Chinese patent application provides a kind of method of black nickel plating, the method adopts sexavalent chrome passivation after plating, do not meet RoHS environmental protection standard, and after passivation, also need immersion oil or dipping lacquer to close, after closing, the wetting property of workpiece surface sharply declines, product cannot be used by viscose glue, and this just greatly limit the use range of Nd-Fe-B magnetic material.
Summary of the invention
In view of the above problems, the object of this invention is to provide a kind of method at neodymium iron boron magnetic body black nickel plating, institute's black coating nickel coating not only has good appearance of black, and has good solidity to corrosion and can cementability.
The described method at neodymium iron boron magnetic body black nickel plating, comprises the following steps: method plating ambrose alloy nickel routinely; Activation is coated with the neodymium iron boron magnetic body of ambrose alloy nickel, to carry out black nickel plating; Black nickel plating, use black nickel plating solution to the neodymium iron boron magnetic body black nickel plating being coated with ambrose alloy nickel after activation, contain in described black nickel plating solution: 2 mass parts nickelous chlorides, 1 mass parts stannous sulfate, 0.4 mass parts complexing agent, 0.6 mass parts blackening agent for surface and 0.1 mass parts rose vitriol.
Described complexing agent be selected from citric acid, oxalic acid, EDTA, sodium tartrate, Trisodium Citrate one or more.Described blackening agent for surface be selected from potassium sulfocyanate, Sodium Thiocyanate 99, ammonium thiocyanate one or more.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is described.
Contain in black nickel plating solution used: nickelous chloride 2 mass parts, stannous sulfate 1 mass parts, complexing agent 0.4 mass parts, blackening agent for surface 0.6 mass parts, rose vitriol 0.1 mass parts.Its complexing agent selects one or more of citric acid, oxalic acid, EDTA, sodium tartrate, Trisodium Citrate; Blackening agent for surface selects one or more of potassium sulfocyanate, Sodium Thiocyanate 99, ammonium thiocyanate.
Nickelous chloride, as the main salt of plating, for coating provides metallic nickel ions, can increase the fragility of coating, coating color can be made when content is low to shoal during content height.Stannous sulfate is the main salt of another kind of plating, and for coating provides metallic tin ion, during content height, the protective of coating is good, and when content is low, coating is easy to change, and protective is poor.Complexing agent is used for the composition stablized in plating solution and pH value.Blackening agent for surface is used for controlling the blackness of coating.Rose vitriol provides cobalt metal ion, thus increases blackness and the hardness of coating.
The entire flow of black nickel plating comprises: and chamfer grinding-ultrasonic oil removing-ultrasonic cleaning-pickling-ultrasonic cleaning-pure water washes-nickel preplating-pure water washes-copper facing-pure water washes-nickel plating-pure water washes-activate-and black nickel plating-pure water washes-and dry.
Black nickel plating electroplating power supply used is high frequency switch power, and pH value is 4.0 ~ 6.0, and electroplating temperature is 45 ~ 65 DEG C.Electroplating voltage is at 1.0 ~ 1.8V.Electroplating time is 15 ~ 45 minutes.Galvanic anode pure nickel plate.
Before black nickel plating, adopt the technique plating ambrose alloy nickel of this area routine, then through hydrochloric acid activation, last black nickel plating, makes product have good appearance of black, can be used for appearance component, extend the use range of product.In addition, cost of the present invention is few, can use traditional the Equipments Used for Plating, process stabilizing, is applicable to barrel plating and rack plating process, and plating solution can life-time service.
embodiment 1
Pending product is of a size of 13mmX3mmX1mm.The magnet product of this dimensions, according to different purposes, as the appearance component with decorative purpose, or may use at interiors of products.
First, according to a conventional method to the bright nickel of magnet nickel-clad copper, the step that removing pure water is washed, mainly comprises following four steps.
The first step, chamfering.Adopt vibrations light polishing machine, brown corundum abrasive 50kg, vibration 6 hours.
Second step, oil removing.By the sodium hydroxide of 10 ~ 30g/L and the OP-10 emulsifying agent of 1 ~ 2g/L, ultrasonic oil removal at 40 DEG C, the time is 3 minutes, and ultrasonic frequency is 20KHz, and power is 2KW.
3rd step, pickling.Use 5% nitric acid, normal temperature pickling 40 seconds, after pickling, carry out ultrasonic cleaning.
4th step, plating.First be nickel preplating, contain in electroplate liquid used: single nickel salt 250 ~ 300g/L, nickelous chloride 30 ~ 50g/L and boric acid 35 ~ 50g/L, pH4.5 ~ 5.2, electroplating temperature is 45 ~ 55 DEG C, electroplate liquid continuous filtration, and electroplating time is 90 minutes.Following copper facing, contains in electroplate liquid used: cupric pyrophosphate 60 ~ 90g/L and potassium pyrophosphate 250 ~ 350g/L, makes pyrophosphate: cupric ion is 7.0:1 ~ 8.0:1, pH8.2 ~ 8.8, electroplating temperature is 40 ~ 50 DEG C, electroplate liquid continuous filtration, and electroplating time is 110 minutes.Then bright nickel plating, contain in electroplate liquid used: single nickel salt 250 ~ 300g/L, nickelous chloride 30 ~ 50g/L, boric acid 35 ~ 50g/L, brightening agent (commercially available) 0.3 ~ 0.8g/L, softening agent (commercially available) 2 ~ 4g/L and wetting agent (commercially available) 1 ~ 3g/L, pH4.5 ~ 5.2, electroplating temperature is 45 ~ 55 DEG C, electroplate liquid continuous filtration, electroplating time is 80 minutes.
Next, to the magnet black nickel plating needing black nickel plating.
First, according to a conventional method activation treatment is carried out to the surface of the magnet being coated with ambrose alloy nickel.
Then, to the magnet black coating nickel after activation treatment.Black nickel plating solution is prepared according to aforementioned formula, wherein, the concentration of nickelous chloride is in the scope of 150 ~ 200g/L, the concentration of stannous sulfate is in the scope of 70 ~ 110g/L, the concentration of complexing agent is in the scope of 20 ~ 50g/L, the concentration of blackening agent for surface is within the scope of 40 ~ 70g/L, and the concentration of rose vitriol is in the scope of 10 ~ 20g/L, and pH is 4.0 ~ 6.0.Electroplating temperature is 45 ~ 65 DEG C, and electroplating time is 30 minutes.
According to above-mentioned electro-plating method, to the magnet with same specifications and characteristics, according to different purposes, distinguished by nickel plating and black nickel, the magnet of black coating nickel has bright black outward appearance, the appearance component that can use as decorative purpose, and the magnet of common nickel plating uses at interiors of products.
embodiment 2
Handled product specification is 6mmX6mmX2mm.But product that performance different identical for physical dimension, in order to avoid user misuses, needs by apparent difference to show differentiation.
First, the bright nickel of technique nickel-clad copper routinely, mainly comprises following four steps.
The first step, chamfering.Adopt vibrations light polishing machine, brown corundum abrasive 50kg, vibration 5 hours.
Second step, oil removing.By the sodium hydroxide of 10 ~ 30g/L and the OP-10 emulsifying agent of 1 ~ 2g/L, ultrasonic oil removal at 40 DEG C, the time is 3 minutes, and ultrasonic frequency is 20KHZ, and power is 2KW.
3rd step, pickling.Use 5% nitric acid, normal temperature pickling 40 seconds, after pickling, carry out ultrasonic cleaning.
4th step, plating.First be nickel preplating, contain in electroplate liquid used: single nickel salt 250 ~ 300g/L, nickelous chloride 30 ~ 50g/L and boric acid 35 ~ 50g/L, PH4.5 ~ 5.2, electroplating temperature is 45 ~ 55 DEG C, plating solution continuous filtration, and electroplating time is 80 minutes.Following copper facing, contains in electroplate liquid used: cupric pyrophosphate 60 ~ 90g/L, potassium pyrophosphate 250 ~ 350g/L, wherein, pyrophosphate: cupric ion is 7.0:1 ~ 8.0:1, pH8.2 ~ 8.8, electroplating temperature is 40 ~ 50 DEG C, plating solution continuous filtration, electroplating time is 90 minutes.Then bright nickel plating, contain in electroplate liquid used: single nickel salt 250 ~ 300g/L, nickelous chloride 30 ~ 50g/L, boric acid 35 ~ 50g/L, brightening agent (commercially available) 0.3 ~ 0.8g/L, softening agent (commercially available) 2 ~ 4g/L and wetting agent (commercially available) 1 ~ 3g/L, pH4.5 ~ 5.2, electroplating temperature is 45 ~ 55 DEG C, plating solution continuous filtration, electroplating time is 80 minutes.
Next, to the magnet black nickel plating needing black coating nickel.
First, the magnet of the bright nickel of ambrose alloy is electroplate with according to a conventional method with hydrochloric acid activation process.
Then, black nickel plating.Black nickel plating solution is prepared according to aforementioned formula, wherein, the concentration of nickelous chloride is in the scope of 150 ~ 200g/L, the concentration of stannous sulfate is in the scope of 70 ~ 110g/L, the concentration of complexing agent is in the scope of 20 ~ 50g/L, the concentration of blackening agent for surface is within the scope of 40 ~ 70g/L, and the concentration of rose vitriol is in the scope of 10 ~ 20g/L, and pH is 4.0 ~ 6.0.Electroplating temperature is 45 ~ 65 DEG C, and electroplating time is 25 minutes.
According to aforesaid method, but product that performance different identical for physical dimension, can be distinguished by common nickel plating and black nickel plating, such as to high performance magnet black nickel plating, and to the common nickel plating of low-performance magnet, user can distinguish two kinds of magnets fast by the appearance color observing product, thus avoids misusing.
embodiment 3
Handled product is trapezium-shaped, and upper base is 6mm, goes to the bottom as 8mm, and height is 4mm, and thick is 4mm.Have the magnet of this shape, magnetizing direction is different because purposes is different.In order to avoid user misuses, can by they distinguish by common nickel plating and black nickel plating in appearance respectively.
First, technique carries out the bright nickel of nickel-clad copper routinely, specifically comprises following four steps.
The first step, chamfering.Adopt vibrations light polishing machine, brown corundum abrasive 50kg, vibration 7 hours.
Second step, oil removing.By the sodium hydroxide of 10 ~ 30g/L and the OP-10 emulsifying agent of 1 ~ 2g/L, ultrasonic oil removal at 40 DEG C, the time is 3 minutes, and ultrasonic frequency is 20KHZ, and power is 2KW.
3rd step, pickling.Use 5% nitric acid, normal temperature pickling 40 seconds, carries out ultrasonic cleaning after pickling.
4th step, plating.First be nickel preplating, contain in electroplate liquid used: single nickel salt 250 ~ 300g/L, nickelous chloride 30 ~ 50g/L and boric acid 35 ~ 50g/L, pH4.5 ~ 5.2, electroplating temperature is 45 ~ 55 DEG C, plating solution continuous filtration, and electroplating time is 80 minutes.Following copper facing, contains in electroplate liquid used: cupric pyrophosphate 60 ~ 90g/L, potassium pyrophosphate 250 ~ 350g/L, wherein pyrophosphate: cupric ion is 7.0:1 ~ 8.0:1, pH8.2 ~ 8.8, electroplating temperature is 40 ~ 50 DEG C, plating solution continuous filtration, and electroplating time is 90 minutes.Then bright nickel plating, contain in electroplate liquid used: single nickel salt 250 ~ 300g/L, nickelous chloride 30 ~ 50g/L, boric acid 35 ~ 50g/L, brightening agent (commercially available) 0.3 ~ 0.8g/L, softening agent (commercially available) 2 ~ 4g/L and wetting agent (commercially available) 1 ~ 3g/L, pH4.5 ~ 5.2, electroplating temperature is 45 ~ 55 DEG C, plating solution continuous filtration, electroplating time is 70 minutes.
Next, to the magnet black nickel plating needing black coating nickel.
First, according to a conventional method activation treatment is carried out to the magnet being coated with the bright nickel of ambrose alloy.
Then, black coating nickel.Black nickel plating solution is prepared according to aforementioned formula, wherein, the concentration of nickelous chloride is in the scope of 150 ~ 200g/L, the concentration of stannous sulfate is in the scope of 70 ~ 110g/L, the concentration of complexing agent is in the scope of 20 ~ 50g/L, the concentration of blackening agent for surface is within the scope of 40 ~ 70g/L, and the concentration of rose vitriol is in the scope of 10 ~ 20g/L, and pH is 4.0 ~ 6.0.Electroplating temperature is 45 ~ 65 DEG C, and electroplating time is 20 minutes.
According to aforesaid method, but product that magnetizing direction different identical for profile, distinguish respectively by electric bright nickel plating and black nickel, such as above-mentioned in trapezoidal magnet product, upper base is N pole, goes to the bottom as the magnet black nickel plating of S pole, and go to the bottom as N pole, upper base are the common nickel plating of magnet of S pole, user can distinguish the product of different magnetizing direction fast by the outward appearance of magnet, thus avoids misusing.
More than in conjunction with embodiment and embodiment, technical scheme of the present invention is illustrated, but the present invention is not limited to this.Under the prerequisite realizing the object of the invention, those skilled in the art can make a change the present invention and be out of shape.
Claims (2)
1., in a method for neodymium iron boron magnetic body black nickel plating, comprise the following steps:
Method is routinely to neodymium iron boron magnetic body plating ambrose alloy nickel;
Activation is coated with the neodymium iron boron magnetic body of ambrose alloy nickel, to carry out black nickel plating;
Black coating nickel, uses black nickel plating solution to the neodymium iron boron magnetic body black nickel plating being coated with ambrose alloy nickel after activation,
Contain in described black nickel plating solution: 2 mass parts nickelous chlorides, 1 mass parts stannous sulfate, 0.4 mass parts complexing agent, 0.6 mass parts blackening agent for surface and 0.1 mass parts rose vitriol.
2. the method at neodymium iron boron magnetic body black nickel plating according to claim 1, described complexing agent be selected from citric acid, oxalic acid, EDTA, sodium tartrate, Trisodium Citrate one or more, described blackening agent for surface be selected from potassium sulfocyanate, Sodium Thiocyanate 99, ammonium thiocyanate one or more.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105239083A (en) * | 2015-11-06 | 2016-01-13 | 和县隆盛精密机械有限公司 | Vehicle hub surface treatment process |
| CN105506694A (en) * | 2015-12-21 | 2016-04-20 | 中磁科技股份有限公司 | Protection technology of neodymium iron boron electroplated coating |
| CN110592623A (en) * | 2019-09-05 | 2019-12-20 | 宁波韵升股份有限公司 | Formula and method of nickel electroplating solution for improving uniform distribution of neodymium iron boron magnet coating |
| CN110983395A (en) * | 2019-12-17 | 2020-04-10 | 广东小天才科技有限公司 | Magnet, preparation method and wearable device |
| CN111005044A (en) * | 2019-12-18 | 2020-04-14 | 宁波韵升股份有限公司 | Dark nickel barrel plating process for improving surface tension of neodymium iron boron magnet |
| CN114540896A (en) * | 2022-03-24 | 2022-05-27 | 东莞市立敏达电子科技有限公司 | Matte black electroplating structure and electroplating method for surface of iron piece |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105239083A (en) * | 2015-11-06 | 2016-01-13 | 和县隆盛精密机械有限公司 | Vehicle hub surface treatment process |
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| CN110592623A (en) * | 2019-09-05 | 2019-12-20 | 宁波韵升股份有限公司 | Formula and method of nickel electroplating solution for improving uniform distribution of neodymium iron boron magnet coating |
| CN110592623B (en) * | 2019-09-05 | 2021-01-05 | 宁波韵升股份有限公司 | Formula and method of nickel electroplating solution for improving uniform distribution of neodymium iron boron magnet coating |
| CN110983395A (en) * | 2019-12-17 | 2020-04-10 | 广东小天才科技有限公司 | Magnet, preparation method and wearable device |
| CN111005044A (en) * | 2019-12-18 | 2020-04-14 | 宁波韵升股份有限公司 | Dark nickel barrel plating process for improving surface tension of neodymium iron boron magnet |
| CN114540896A (en) * | 2022-03-24 | 2022-05-27 | 东莞市立敏达电子科技有限公司 | Matte black electroplating structure and electroplating method for surface of iron piece |
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