CN109023446A - A kind of method of neodymium-iron boron permanent magnetic material electroplating copper - Google Patents
A kind of method of neodymium-iron boron permanent magnetic material electroplating copper Download PDFInfo
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- CN109023446A CN109023446A CN201810965503.0A CN201810965503A CN109023446A CN 109023446 A CN109023446 A CN 109023446A CN 201810965503 A CN201810965503 A CN 201810965503A CN 109023446 A CN109023446 A CN 109023446A
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- copper
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- iron boron
- plating
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/36—Pretreatment of metallic surfaces to be electroplated of iron or steel
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/001—Magnets
Abstract
The invention discloses a kind of methods of neodymium-iron boron permanent magnetic material electroplating copper.The step of this method is as follows: the plating solution is made of stannous chloride and chlorination 1- ethyl 3- methylimidazole, molar ratio 1:1；Pickling pre-treatment is first carried out to NdFeB material to be plated, is activated being transferred in the glove box of argon atmosphere after NdFeB material to be plated drying, the oxidation film that removal surface produces again, and play the role of leveling to matrix；In coating bath, bath temperature is 25~80 DEG C, and current density is 5~50mA/cm2；Anode is copper wire, and cathode is the neodymium iron boron matrix by pre-treatment, is connected respectively with DC power supply positive and negative anodes, and the current density and required thickness of coating when plating time is according to plating determine.The present invention can directly plating obtains copper coating on neodymium iron boron, and plated layer compact is uniform, and binding force is good；Using the environmental protection ionic liquid copper facing system of no cyanogen, there is environmental protection feature.
Description
Technical field
The present invention relates to the copper-plating techniques in process for treating surface, more particularly, to a kind of neodymium-iron boron permanent magnetic material electroplating copper
Method.
Background technique
Neodymium iron boron (NdFeB) permanent-magnet material is third generation rare-earth permanent magnet, has excellent magnetic property, is widely used in vapour
The fields such as turner industry, electrical engineering, space flight and aviation, microwave technology.But, NdFeB material contains the high rare earth member of chemical activity
Plain neodymium, and be heterogeneous structure, each interphase potential difference is larger, easily corrodes in use, significantly reduces its magnetic property.For
This, needs to be surface-treated neodymium iron boron to improve its anti-corrosion capability, and such as plating, chemical plating, vacuum vapor deposition, electrophoresis apply
Dress etc., wherein plating is the important method of NdFeB material surfacecti proteon, is industrially used widely.It is most mature at present
, it is in neodymium iron boron electroplating surface zinc and nickel.
Compared with zinc coating, nickel coating is since its hardness is high, corrosion resistance and the advantages that good decorative property, in the plating of neodymium iron boron
It is most widely used in protection.Ni/Cu/Ni multilayer system (3 μm/12 μm/5 μ are generally taken in traditional neodymium iron boron nickel plating
M).Centre uses copper coating, is on the one hand the porosity for reducing Plating System, improves corrosion resistance coating, on the other hand can generation
For part nickel coating, weaken magnetic screen of the nickel to matrix.But the solution of nickel preplating will cause the biggish decaying of neodymium-iron-boron energy
(MA etc., Electrodeposition of amorphous Ni-P coatings onto Nd-Fe-B permanent
Magnet substrates [J] Applied Surface Science, 2006,253 (4): 2251- 2256).And it is direct
Copper facing then because displacement reaction can occur between neodymium iron boron matrix and plating solution, is not easy to obtain copper coating continuous, that binding force is good.
To solve the above problems, researcher proposes the new method of the direct plating Cu on neodymium iron boron.For example, patent
201310219308.0 with the copper plating bath of no cyanogen in neodymium iron boron electroplating surface Cu, the copper plating bath includes bivalent cupric ion, wine
Stone acid potassium, citric acid etc., this plating solution can reduce coating blistering, corrosion of the liberation of hydrogen to neodymium iron boron when reducing plating.Patent
201610675886.9 disclose the electroplating technology and electroplate liquid of a kind of neodymium iron boron, it is characterised in that are impacted first with high current fast
Speed plates layers of copper on neodymium iron boron surface, the copper plating bath include open cylinder liquid (mantoquita, phosphoric acid, potassium dihydrogen phosphate, water, di 2 ethylhexyl phosphonic acid),
Aqueous slkali and wetting agent etc..Patent 201710518591.5 discloses a kind of electroplate liquid of direct electro-coppering of neodymium iron boron, the plating
Copper liquid includes cupric pyrophosphate, hydrazine hydrate, EDTA, borax, neopelex, lactic acid etc..The characteristics of electroplate liquid is can
Inhibit the generation of displacement layers of copper, to obtain fine and close and bright coating on neodymium iron boron surface.Li Yue et al. then proposes utilization
In the technique of the direct acid copper in neodymium iron boron magnetic body surface, (Li Yue, Zhu Liqun, Li Weiping wait to alkaline HEDP complexing agent plating solution
Neodymium iron boron device surface electric deposited copper floor and performance [J] material engineering, 2017,45 (6): 55-60.), obtained copper coating
Compact structure is good with the binding force of neodymium iron boron.
Above-mentioned surface treatment all carries out in aqueous solution, and neodymium iron boron surface easily reacts in aqueous solution, therefore
It is difficult to ensure that the binding force between neodymium iron boron matrix and coating；On the other hand, aqueous solution copper facing is not easy to handle etc. there is also waste liquid
Environmental issue (Liu Wei, marquis is into neodymium iron boron electroplating technology production status and prospect [J] is electroplated and finish, and 2012,34
(4): 20-25).Recently, it is a kind of with aqueous solution is entirely different, the new liquid " ionic liquid " that is made of ion, it is electric because having
The features such as position window width, steam force down, is not aqueous, environmentally protective, earns widespread respect in field of electroplating.Such as patent
201210248413.2 replace imidazolitm chloride-aluminum chloride type ionic liquid to be medium using two, and are added wherein a certain amount of
Aromatic series organic additive obtains the Al coating that silvery white is bright, fine and close on neodymium iron boron.2015104371166 disclosure of patent
A method of the ionic liquid electroless copper using simple, environmentally protective ionic liquid as solution, the ionic liquid of use
It is the choline chloride and urea system that molar ratio is 1:2, belongs to electroless copper technology；Patent 2015109762467 discloses one
Electro-plating method without cyanogen copper zinc electroplate liquid of the kind containing ionic liquid, electroplate liquid contain ion liquid addictive, it is seen that the copper plating bath
It is still aqueous solution, ionic liquid is only used as additive to use.Patent 201611044308.1 discloses a kind of no cryanide ion liquid
Copper plating solution and copper-plating technique carry out copper facing, copper-plated wide temperature range, current density model by the environmental non-cyanide copper plating bath
It encloses big.
Summary of the invention
The purpose of the present invention is to provide a kind of methods of neodymium-iron boron permanent magnetic material electroplating copper, are in Nd-Fe-B permanent magnet material
On using the direct electro-coppering of ionic liquid method.
In order to achieve the above object of the invention, the step of the technical solution adopted by the present invention is as follows:
1) plating solution forms:
The plating solution is made of stannous chloride and chlorination 1- ethyl 3- methylimidazole, wherein stannous chloride and chlorination 1- ethyl 3- first
The molar ratio of base imidazoles is 1:1；Under room temperature, by two kinds of massages, your quality is weighed, and plating solution is obtained after mixing；
2) copper-plating technique:
(1) NdFeB material pre-treatment:
Pickling pre-treatment is first carried out to NdFeB material to be plated, it may be assumed that alkali cleaning oil removing-deionization washing-nitric acid acidwashing-deionized water
- alcohol ultrasound is washed, is activated being transferred in the glove box of argon atmosphere after NdFeB material to be plated drying, removes table
The oxidation film that face produces again, and play the role of leveling to matrix；
(2) NdFeB material copper facing:
Technological parameter: in coating bath, bath temperature is 25~80 DEG C, and current density is 5~50mA/cm2；
Anode is copper wire, and cathode is the neodymium iron boron matrix by pre-treatment, is connected respectively with DC power supply positive and negative anodes, when plating
Between, current density and required thickness of coating when according to plating determine.
The technological parameter is best are as follows: bath temperature is 60 DEG C, and current density is 5~20 mA/cm2, electroplating time 7
~28 min, 6~10 μm of thickness of coating；At this point, the copper coating dense uniform obtained.
The invention has the advantages that:
1) it can be directly electroplated on neodymium iron boron and obtain copper coating, and plated layer compact is uniform, binding force is good；
2) the environmental protection ionic liquid copper facing system without cyanogen is used, there is environmental protection feature.
Detailed description of the invention
Fig. 1 is the SEM pattern of the neodymium iron boron matrix by pre-treatment.
Fig. 2 is with 5 mA/cm2The SEM pattern of the copper coating of 28min is electroplated in current density.
Fig. 3 is with 5 mA/cm2The X ray diffracting spectrum of the copper coating of 28min is electroplated in current density.
Fig. 4 is with 20 mA/cm2The SEM pattern of the copper coating of 7 min is electroplated in current density.
Fig. 5 is with 20 mA/cm2The X ray diffracting spectrum of the copper coating of 7 min is electroplated in current density.
Fig. 6 is with 10 mA/cm2The SEM pattern of the copper coating of 23 min is electroplated in current density.
Fig. 7 is with 10 mA/cm2The X ray diffracting spectrum of the copper coating of 23 min is electroplated in current density.
Fig. 8 is with 5 mA/cm2The SEM pattern of the copper coating of 28 min is electroplated in current density.
Fig. 9 is with 5 mA/cm2The X ray diffracting spectrum of the copper coating of 28 min is electroplated in current density.
Figure 10 is with 50 mA/cm2The SEM pattern of the copper coating of 3 min is electroplated in current density.
Figure 11 is with 50 mA/cm2The X ray diffracting spectrum of the copper coating of 3 min is electroplated in current density.
Specific embodiment
Present invention will be further explained below with reference to the attached drawings and examples.
Plating solution composition:
The plating solution is made of stannous chloride and chlorination 1- ethyl 3- methylimidazole, wherein stannous chloride and chlorination 1- ethyl 3- first
The molar ratio of base imidazoles is 1:1；Under room temperature, by two kinds of massages, your quality is weighed, and plating solution is obtained after mixing；
NdFeB material pre-treatment:
Pickling pre-treatment is first carried out to NdFeB material to be plated, it may be assumed that alkali cleaning oil removing-deionization washing-nitric acid acidwashing-deionized water
- alcohol ultrasound is washed, is activated being transferred in the glove box of argon atmosphere after NdFeB material to be plated drying, removes table
The oxidation film that face produces again；The SEM pattern electromicroscopic photograph of the neodymium iron boron matrix obtained after pre-treatment, as shown in Fig. 1.
Technological parameter: in coating bath, bath temperature is 25~80 DEG C, and temperature is too low, and copper-plated current density is small；Temperature mistake
Height, to the materials such as coating bath requirement height, energy consumption is high；Current density is 5~50mA/cm2；Current density is too low, the time required to copper facing
It is long；Current density is excessively high, easily forms dendroid coating.
Embodiment 1
5 mA/cm of current density2, 28 6 μm of min(coating theoretic throat of electroplating time)
Bath temperature is 60 DEG C, and anode is copper wire, and cathode is the neodymium iron boron matrix by pre-treatment, positive and negative with DC power supply respectively
Extremely it is connected, with 5 mA/cm228 min of current density plating, coating theoretic throat reaches 6 μm, the SEM pattern electricity of copper coating
Mirror photo is as shown in Figure 2, it is seen that copper coating dense uniform.X-ray diffraction spectrum is as shown in Figure 3, it is seen that coating is the copper of crystalline state.
Embodiment 2
20 mA/cm of current density2, 76 μm of min(coating theoretic throat of electroplating time)
Bath temperature is 60 DEG C, and anode is copper wire, and cathode is the neodymium iron boron matrix by pre-treatment, positive and negative with DC power supply respectively
Extremely it is connected, with 20 mA/cm27 min of current density plating, coating theoretic throat reaches 6 μm, the SEM pattern electricity of copper coating
Mirror photo is as shown in Figure 4, it is seen that copper coating dense uniform.X-ray diffraction spectrum is as shown in Figure 5, it is seen that coating is the copper of crystalline state.
Embodiment 3
10 mA/cm of current density2, 23 10 μm of min(coating theoretic throat of electroplating time)
Bath temperature is 60 DEG C, and anode is copper wire, and cathode is the neodymium iron boron matrix by pre-treatment, positive and negative with DC power supply respectively
Extremely it is connected, with 10 mA/cm223 min of current density plating, coating theoretic throat reaches 10 μm, the SEM pattern of copper coating
Electromicroscopic photograph is as shown in Figure 6, it is seen that copper coating dense uniform.X-ray diffraction spectrum is as shown in Figure 7, it is seen that coating is the copper of crystalline state.
Embodiment 4
5 mA/cm of current density2, 28 6 μm of min(coating theoretic throat of electroplating time)
Bath temperature is 25 DEG C, and anode is copper wire, and cathode is the neodymium iron boron matrix by pre-treatment, positive and negative with DC power supply respectively
Extremely it is connected, with 5 mA/cm228 min of current density plating, coating theoretic throat reaches 6 μm, the SEM pattern electricity of copper coating
Shown in mirror photo Fig. 8, it is seen that copper coating dense uniform.X-ray diffraction spectrum is as shown in Fig. 9 figure, it is seen that coating is the copper of crystalline state.
Embodiment 5
50 mA/cm of current density2, 36 μm of min(coating theoretic throat of electroplating time)
Bath temperature is 80 DEG C, and anode is copper wire, and cathode is the neodymium iron boron matrix by pre-treatment, positive and negative with DC power supply respectively
Extremely it is connected, with 50 mA/cm23 min of current density plating, coating theoretic throat reaches 6 μm, the SEM pattern electricity of copper coating
Shown in mirror photo Figure 10, it is seen that copper coating dense uniform.X-ray diffraction spectrum is as shown in figure 11, it is seen that coating is the copper of crystalline state.
Power test is combined to coating with hubbing, coating and binder interface separation as 9.2 Mpa, it is known that copper
The binding force of coating and neodymium iron boron matrix is greater than 9.2 Mpa, and binding force is excellent.
Claims (2)
1. a kind of method of neodymium-iron boron permanent magnetic material electroplating copper, which is characterized in that the step of this method is as follows:
1) plating solution forms:
The plating solution is made of stannous chloride and chlorination 1- ethyl 3- methylimidazole, wherein stannous chloride and chlorination 1- ethyl 3- first
The molar ratio of base imidazoles is 1:1；Under room temperature, by two kinds of massages, your quality is weighed, and plating solution is obtained after mixing；
2) copper-plating technique:
(1) NdFeB material pre-treatment:
Pickling pre-treatment is first carried out to NdFeB material to be plated, it may be assumed that alkali cleaning oil removing-deionization washing-nitric acid acidwashing-deionized water
- alcohol ultrasound is washed, is activated being transferred in the glove box of argon atmosphere after NdFeB material to be plated drying, removes table
The oxidation film that face produces again, and play the role of leveling to matrix；
(2) NdFeB material copper facing:
Technological parameter: in coating bath, bath temperature is 25~80 DEG C, and current density is 5~50mA/cm2；
Anode is copper wire, and cathode is the neodymium iron boron matrix by pre-treatment, is connected respectively with DC power supply positive and negative anodes, when plating
Between, current density and required thickness of coating when according to plating determine.
2. a kind of method of neodymium-iron boron permanent magnetic material electroplating copper according to claim 1, it is characterised in that: the technique ginseng
Number is best are as follows: bath temperature is 60 DEG C, and current density is 5~20 mA/cm2, electroplating time is 7~28 min, thickness of coating 6
~10 μm；At this point, the copper coating dense uniform obtained.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109825861A (en) * | 2019-03-18 | 2019-05-31 | 辽宁科技大学 | A kind of pure iron base basic plating copper coating technique |
| CN114438556A (en) * | 2022-02-18 | 2022-05-06 | 安泰科技股份有限公司 | Method for electroplating low-roughness Ra-value alkali copper on surface of rare earth permanent magnet material |
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| CN102839403A (en) * | 2012-09-10 | 2012-12-26 | 太原理工大学 | Method for electroplating aluminum in ionic liquid |
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| CN102766891A (en) * | 2012-07-18 | 2012-11-07 | 中国科学院宁波材料技术与工程研究所 | Method for electrodepositing Al protective plated layer on surface of NdFeB magnet by using ionic liquid |
| CN102839403A (en) * | 2012-09-10 | 2012-12-26 | 太原理工大学 | Method for electroplating aluminum in ionic liquid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109825861A (en) * | 2019-03-18 | 2019-05-31 | 辽宁科技大学 | A kind of pure iron base basic plating copper coating technique |
| CN114438556A (en) * | 2022-02-18 | 2022-05-06 | 安泰科技股份有限公司 | Method for electroplating low-roughness Ra-value alkali copper on surface of rare earth permanent magnet material |
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