CN104630853B - A method of in neodymium iron boron magnetic body black nickel plating - Google Patents
A method of in neodymium iron boron magnetic body black nickel plating Download PDFInfo
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- CN104630853B CN104630853B CN201310561208.6A CN201310561208A CN104630853B CN 104630853 B CN104630853 B CN 104630853B CN 201310561208 A CN201310561208 A CN 201310561208A CN 104630853 B CN104630853 B CN 104630853B
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Abstract
The present invention provides a kind of method in neodymium iron boron magnetic body black nickel plating.This approach includes the following steps：Electronickelling cupro-nickel by a conventional method；Activation is coated with the neodymium iron boron magnetic body of ambrose alloy nickel, to carry out black nickel plating；Black coating nickel is contained using black nickel plating solution to the neodymium iron boron magnetic body black nickel plating for being coated with ambrose alloy nickel after activation in the black nickel plating solution：2 mass parts nickel 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 cobaltous sulfate.
Description
Technical field
The present invention relates to a kind of methods in neodymium iron boron magnetic body black nickel plating.
Background technology
The application and development of rare-earth Nd-Fe-B (NdFeB) permanent magnet are very rapid in recent years, but Nd-Fe-B permanent magnet
Corrosion resistance is very poor, easily corrodes in wet condition.Once corroding, the magnetic property of magnet will decline, to drop
The reliability and stability of low product.Therefore, the application of NdFeB material is on condition that resolve the Anticorrosion of NdFeB material.
The anti-corrosion method of NdFeB material mainly has plating, phosphatization, electrophoresis etc. at present.Plating is due to protective capacities
By force, the advantages of process stabilizing, and it is used as the anti-corrosion method of most of NdFeB materials.Conventional neodymium iron boron electroplating technology is electricity
Nickel plating cupro-nickel (Ni-Cu-Ni) technique, i.e., first in one layer of nickel of NdFeB material surface preplating, then in middle layer copper facing, finally
Dark nickel and bright nickel is electroplated on surface layer.The outer layer nickel plating of common process is silvery white, and same size neodymium iron boron workpiece often has not
Same performance, client easily mutually mix when assembling.
In recent years, a kind of black nickel coating is used for Nd-Fe-B magnetic material because having dicoration well, this black
Coating can be distinguished with conventional white coating, to distinguish the product that size is identical but performance or use is different, avoid using
When mutually obscure.
Generally use is electroplated or the mode of chemical plating prepares black nickel coating, but there are corrosion resistance of coating poor, binding force is not
The shortcomings that good, coating soft easy scuffing.Since NdFeB material easily corrodes, so conventional black nickel coating is difficult to apply in neodymium iron
Boron material.
Chinese patent application discloses CN101054697A and provides a kind of method of black nickel plating, and this method is adopted after plating
With sexavalence chromium passivating, RoHS environmental protection standards are not met, and also need to immersion oil or dipping lacquer closing, workpiece surface after closing after being passivated
Wellability drastically declines so that product can not viscose glue use, this just greatly limits the use scope of Nd-Fe-B magnetic material.
Invention content
In view of the above problems, the object of the present invention is to provide a kind of method in neodymium iron boron magnetic body black nickel plating, institute's black coatings
Nickel coating not only has good appearance of black, and has good corrosion resistance and can cementability.
The method in neodymium iron boron magnetic body black nickel plating includes the following steps：Electronickelling cupro-nickel by a conventional method；It is living
Change the neodymium iron boron magnetic body for being coated with ambrose alloy nickel, to carry out black nickel plating；Black nickel plating, using black nickel plating solution to the plating after activation
There is the neodymium iron boron magnetic body black nickel plating of ambrose alloy nickel, contains in the black nickel plating solution：Nickel chloride 150-200g/L, stannous sulfate
70-110g/L, complexing agent 20-30g/L, blackening agent for surface 40-70g/L and cobaltous sulfate 10-20g/L.
The complexing agent be selected from citric acid, oxalic acid, EDTA, sodium tartrate, sodium citrate it is one or more.The nigrescence
Agent be selected from potassium rhodanide, sodium sulfocyanate, ammonium thiocyanate it is one or more.
Specific implementation mode
Technical scheme of the present invention is illustrated below in conjunction with specific implementation mode.
Contain in black nickel plating solution used：2 mass parts of nickel chloride, 1 mass parts of stannous sulfate, 0.4 mass parts of complexing agent,
0.6 mass parts of blackening agent for surface, 0.1 mass parts of cobaltous sulfate.Its complexing agent selects citric acid, oxalic acid, EDTA, sodium tartrate, lemon
The one or more of sour sodium；Blackening agent for surface selects the one or more of potassium rhodanide, sodium sulfocyanate, ammonium thiocyanate.
Nickel chloride provides metallic nickel ions as electroplating main salt, for coating, can increase the brittleness of coating, content when content is high
Coating color can be made to shoal when low.Stannous sulfate is another electroplating main salt, provides metal tin ion for coating, is plated when content is high
The protective of layer is good, and coating is easy to change when content is low, and protective is poor.Complexing agent is used to stablize the ingredient and pH value in plating solution.Hair
The black dose of blackness for being used for controlling coating.Cobaltous sulfate provides metal cobalt ions, to increase the blackness and hardness of coating.
The entire flow of black nickel plating includes：Chamfer grinding-ultrasound oil removing-ultrasonic cleaning-pickling-ultrasonic cleaning-pure water
Wash-nickel preplating-pure water washes-copper facing-pure water washes-nickel plating-pure water is washed-and activates-black nickel plating-pure water is washed-and dry.
Electroplating power supply used in black nickel plating is high frequency switch power, and pH value is 4.0~6.O, and electroplating temperature is 45~65
℃.Electroplating voltage is in 1.0~1.8V.Electroplating time is 15~45 minutes.Galvanic anode pure nickel plate.
The technique electronickelling cupro-nickel that this field routine is used before black nickel plating, then passes through hydrochloric acid activation, is finally electroplated
Black nickel makes product have good appearance of black, can be used for appearance member, extend the use scope of product.In addition, the present invention at
This is few, traditional the Equipments Used for Plating, process stabilizing can be used to be suitable for barrel plating and rack plating process, plating solution can be used for a long time.
Embodiment 1
The size of pending product is 13mm X 3mm X 1mm.The magnet product of this dimensions is according to different use
On the way, the appearance member with decorative purpose is possibly served for, or is used in interiors of products.
First, the step of pure water is washed is removed to the bright nickel of magnet nickel-clad copper according to a conventional method, includes mainly that following four walks
Suddenly.
The first step, chamfering.Using vibrations light polishing machine, brown corundum abrasive 50kg, vibration 6 hours.
Second step, oil removing.It is ultrasonic at 40 DEG C with the sodium hydroxide of 10~30g/L and the OP-10 emulsifiers of 1~2g/L
Wave oil removing, time are 3 minutes, ultrasonic frequency 20KHz, power 2KW.
Third walks, pickling.It is cleaned by ultrasonic after pickling in room temperature pickling 40 seconds with 5% nitric acid.
4th step, plating.It is nickel preplating first, contains in electroplate liquid used：250~300g/L of nickel sulfate, nickel chloride 30
35~50g/L of~50g/L and boric acid, pH4.5~5.2, electroplating temperature are 45~55 DEG C, and electroplate liquid continuously filters, electroplating time
It is 90 minutes.Following copper facing contains in electroplate liquid used：250~350g/L of 60~90g/L of cupric pyrophosphate and potassium pyrophosphate,
So that pyrophosphate: copper ion 7.0: 1~8.0: 1, pH8.2~8.8, electroplating temperature are 40~50 DEG C, the continuous mistake of electroplate liquid
Filter, electroplating time are 110 minutes.Then bright nickel plating contains in electroplate liquid used：250~300g/L of nickel sulfate, nickel chloride 30~
50g/L, 35~50g/L of boric acid, brightener (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 are 45~55 DEG C, and electroplate liquid continuously filters, and electroplating time is 80 minutes.
Next, the magnet black nickel plating to needing black nickel plating.
First, the surface of the magnet to being coated with ambrose alloy nickel carries out activation process according to a conventional method.
Then, to the magnet black coating nickel after activation process.Black nickel plating solution is prepared according to aforementioned formula, wherein nickel chloride
Concentration in the range of 150~200g/L, in the range of 70~110g/L, the concentration of complexing agent exists the concentration of stannous sulfate
The range of 20~50g/L, the concentration of blackening agent for surface is within the scope of 40~70g/L, the range of the concentration of cobaltous sulfate in 10~20g/L
Interior, 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, by nickel plating and
Black nickel is distinguished, and the magnet of black coating nickel has brilliant black colored appearance, the appearance member that can be used as decorative purpose, and commonly plates
The magnet of nickel is used in interiors of products.
Embodiment 2
Handled product specification is 6mm X 6mm X 2mm.The identical but different performance product for appearance and size is
It avoids user from misusing, needs different to distinguish to show by apparent.
First, the routinely bright nickel of technique nickel-clad copper includes mainly following four step.
The first step, chamfering.Using vibrations light polishing machine, brown corundum abrasive 50kg, vibration 5 hours.
Second step, oil removing.It is ultrasonic at 40 DEG C with the sodium hydroxide of 10~30g/L and the OP-10 emulsifiers of 1~2g/L
Wave oil removing, time are 3 minutes, ultrasonic frequency 20KHZ, power 2KW.
Third walks, pickling.It is cleaned by ultrasonic after pickling in room temperature pickling 40 seconds with 5% nitric acid.
4th step, plating.It is nickel preplating first, contains in electroplate liquid used：250~300g/L of nickel sulfate, nickel chloride 30
35~50g/L of~50g/L and boric acid, PH4.5~5.2, electroplating temperature are 45~55 DEG C, and plating solution continuously filters, and electroplating time is
80 minutes.Following copper facing contains in electroplate liquid used：60~90g/L of cupric pyrophosphate, 250~350g/L of potassium pyrophosphate,
In, pyrophosphate: copper ion 7.0: 1~8.0: 1, pH8.2~8.8, electroplating temperature are 40~50 DEG C, and plating solution continuously filters,
Electroplating time is 90 minutes.Then bright nickel plating contains in electroplate liquid used：250~300g/L of nickel sulfate, 30~50g/ of nickel chloride
L, 35~50g/L of boric acid, brightener (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 are 45~55 DEG C, and plating solution continuously filters, and electroplating time is 80 minutes.
Next, the magnet black nickel plating to needing black coating nickel.
First, the magnet for being electroplate with the bright nickel of ambrose alloy is handled with hydrochloric acid activation according to a conventional method.
Then, black nickel plating.Prepare black nickel plating solution according to aforementioned formula, wherein the concentration of nickel chloride 150~
In the range of 200g/L, the concentration of stannous sulfate is in the range of 70~110g/L, the model of the concentration of complexing agent in 20~50g/L
Enclose, the concentration of blackening agent for surface within the scope of 40~70g/L, the concentration of cobaltous sulfate in the range of 10~20g/L, pH be 4.0~
6.0.Electroplating temperature is 45~65 DEG C, and electroplating time is 25 minutes.
According to the above method, product identical for appearance and size but different performance can pass through common nickel plating and plating
Black nickel is distinguished, such as to high performance magnet black nickel plating, and to the common nickel plating of low-performance magnet, user, which passes through, observes product
Appearance color can quickly distinguish two kinds of magnets, to avoid misusing.
Embodiment 3
The trapezoidal shape of handled product, upper bottom are 6mm, are gone to the bottom as 8mm, a height of 4mm, thickness 4mm.With this shape
The magnet of shape, magnetizing direction are different because of purposes difference.In order to avoid user misuses, common nickel plating and electricity respectively can be passed through
Black coating nickel in appearance distinguishes them.
First, routinely technique carries out the bright nickel of nickel-clad copper, specifically includes following four step.
The first step, chamfering.Using vibrations light polishing machine, brown corundum abrasive 50kg, vibration 7 hours.
Second step, oil removing.It is ultrasonic at 40 DEG C with the sodium hydroxide of 10~30g/L and the OP-10 emulsifiers of 1~2g/L
Wave oil removing, time are 3 minutes, ultrasonic frequency 20KHZ, power 2KW.
Third walks, pickling.With 5% nitric acid, room temperature pickling 40 seconds is cleaned by ultrasonic after pickling.
4th step, plating.It is nickel preplating first, contains in electroplate liquid used：250~300g/L of nickel sulfate, nickel chloride 30
35~50g/L of~50g/L and boric acid, pH4.5~5.2, electroplating temperature are 45~55 DEG C, and plating solution continuously filters, and electroplating time is
80 minutes.Following copper facing contains in electroplate liquid used：60~90g/L of cupric pyrophosphate, 250~350g/L of potassium pyrophosphate, wherein
Pyrophosphate: copper ion 7.0: 1~8.0: 1, pH8.2~8.8, electroplating temperature are 40~50 DEG C, and plating solution continuously filters, plating
Time is 90 minutes.Then bright nickel plating contains in electroplate liquid used：250~300g/L of nickel sulfate, 30~50g/L of nickel chloride, boron
35~50g/L of acid, brightener (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 are 45~55 DEG C, and plating solution continuously filters, and electroplating time is 70 minutes.
Next, the magnet black nickel plating to needing black coating nickel.
First, activation process is carried out to the magnet for being coated with the bright nickel of ambrose alloy according to a conventional method.
Then, black coating nickel.Black nickel plating solution is prepared according to aforementioned formula, wherein the concentration of nickel chloride is in 150~200g/L
In the range of, for the concentration of stannous sulfate in the range of 70~110g/L, the concentration of complexing agent is in the range of 20~50g/L, hair
Black dose of concentration is within the scope of 40~70g/L, and for the concentration of cobaltous sulfate in the range of 10~20g/L, pH is 4.0~6.0.Plating
Temperature is 45~65 DEG C, and electroplating time is 20 minutes.
According to the above method, product identical for shape but different magnetizing direction passes through electric bright nickel plating and black nickel respectively
And distinguish, such as above-mentioned trapezoidal magnet product, it is that the poles N, bottom are the magnet black nickel plating of the poles S, and go to the bottom to upper bottom
For the poles N, the common nickel plating of magnet that upper bottom is the poles S, user can quickly distinguish different magnetizing directions by the appearance of magnet
Product, to avoid misusing.
Technical scheme of the present invention is illustrated above in association with specific implementation mode and embodiment, but the present invention is not
It is limited to this.Under the premise of realizing the object of the invention, those skilled in the art can make a change and deform to the present invention.
Claims (2)
1. a kind of method in neodymium iron boron magnetic body black nickel plating includes the following steps：
By a conventional method to neodymium iron boron magnetic body electronickelling cupro-nickel；
Activation is coated with the neodymium iron boron magnetic body of ambrose alloy nickel, to carry out black nickel plating；
Black coating nickel, using black nickel plating solution to the neodymium iron boron magnetic body black nickel plating for being coated with ambrose alloy nickel after activation,
Contain in the black nickel plating solution：Nickel chloride 150-200g/L, stannous sulfate 70-110g/L, complexing agent 20-50g/L, hair
Black dose of 40-70g/L and cobaltous sulfate 10-20g/L,
The pH values of the black nickel plating solution are 4.0-6.0.
2. the method according to claim 1 in neodymium iron boron magnetic body black nickel plating, the complexing agent is selected from citric acid, grass
Acid, EDTA, sodium tartrate, sodium citrate it is one or more, the blackening agent for surface be selected from potassium rhodanide, sodium sulfocyanate, thiocyanic acid
Ammonium it is one or more.
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| CN201310561208.6A CN104630853B (en) | 2013-11-12 | 2013-11-12 | A method of in neodymium iron boron magnetic body black nickel plating |
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| 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 |
| 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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