CN104073849B - A kind of technique of Sintered NdFeB magnet electroplating nickel on surface tungsten phosphorus - Google Patents
A kind of technique of Sintered NdFeB magnet electroplating nickel on surface tungsten phosphorus Download PDFInfo
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Abstract
The technique that the invention discloses a kind of Sintered NdFeB magnet electroplating nickel on surface tungsten phosphorus, this technique be the surface of Sintered NdFeB magnet is sequentially passed through polishing, alkaline degreasing, hot wash process after, it is placed in oxalic acid solution, carry out soaking or ultrasonic activation process, the Sintered NdFeB magnet electroplating nickel on surface tungsten phosphor alloy coating after activation processing；This technique overcomes Sintered NdFeB magnet surface chemical composition and the uneven problem of electrochemistry, can be effectively by neodymium iron boron magnetic body Surface uniformization, strengthen neodymium-iron-boron surface and ni-w-p alloy binding force of cladding material, improve the corrosion resisting property of neodymium iron boron magnetic body, this technique is simple, production cost is low, can be with industrial applications.
Description
Technical field
The technique that the present invention relates to a kind of Sintered NdFeB magnet electroplating nickel on surface tungsten phosphorus, belongs to metal material surface
Process field.
Background technology
From nineteen eighty-three, assistant river et al. utilizes powder metallurgic method to develop high performance Nd-Fe-B series in Japan first
Row permanent magnet, has refreshed the highest record of permanent magnet performance, is just developed rapidly, in magnetic once coming out
Materials industry market occupies leading position so that it is before obtaining wide market in modern industry and electronic technology
Scape.But due to neodymium-iron-boron magnetic material surface porosity porous, chemism by force, easily oxide etch etc. a lot
Defect has a strong impact on its range of application.Therefore, the wide variety of premise of NdFeB material is to first have to solve magnet
The most corrosion resistant critical defect.
Neodymium iron boron magnetic body mainly by three phase compositions, i.e. principal phase, rich neodymium phase and boron-rich phase, wherein rich neodymium phase and richness
Boron is typically all distributed in grain boundaries mutually, and rich neodymium is the most oxidized, and the volume fraction of magnet principal phase is the biggest
In rich neodymium phase and the volume fraction of boron-rich phase, so magnet easily has the electrochemistry local corrosion of the big negative electrode of primary anode
The feature of battery, it will further speed up intercrystalline corrosion；Further, since the corrosion potential of rich neodymium phase is relatively low, hold
Easily there is electrochemical corrosion.Therefore, it is necessary to neodymium-iron-boron magnetic material is carried out surfacecti proteon.
The main method solving neodymium iron boron magnetic body etching problem at present is to deposit one layer of corrosion-resistant coating in magnet surface,
Main processing method is the process of surface treatment such as plating or chemical plating.The pass of neodymium iron boron magnetic body process for treating surface
Key is pre-treating technology.If pre-treating technology is suitable, once after magnet surface has been successfully formed bottom, just
The film layer of property can be had, to be applicable to various working environments in magnet surface formation.But, neodymium ferrum
Boron magnet is heterogeneous structure, and this makes magnet be all uneven in chemical composition and electrochemistry, each alternate deposits
In the biggest potential difference, in magnet is placed in treatment fluid, different meeting shows different electrochemical behaviors.
Therefore, people have carried out substantial amounts of research to neodymium iron boron magnetic body pre-treatment, the most frequently used to neodymium iron boron magnetic body at present
Pre-treating method is: polishing → alkali cleaning oil removing → nitric acid+thiourea pickling → ammonium acid fluoride+sulfosalisylic acid activation
(Palladous chloride. ethanol solution), because Nd-Fe-B permanent magnet material is formed many by powder metallurgical technique compacting
Porous materials, magnet can cause because of pickling in hydrogen embrittlement, and the hole of pickle entrance neodymium iron boron can cause material
Further corrosion, thus cause the surface efflorescence of Nd-Fe-B permanent magnet, coating is easy to fall off, degradation under magnetic property；
Fluorion is to human body and bad environmental；Palladium is that noble metal makes its range of application limited；It addition, before the most conventional
Process is divided into pickling and activation two to process step, and technique is cumbersome, and the operating time is difficult to control to, electroplated product
Success rate is relatively low.Nickel tungsten phosphorus electrodeposited coating has the corrosion resistant of high rigidity, high thermal stability, high-wearing feature and excellence
Erosion performance etc. has broad application prospects, relevant at neodymium iron boron magnetic body directly electroplating on surface ni-w-p alloy so far
The research of coating have not been reported.
Therefore, exploitation it is badly in need of a kind of simple to operate, it is easy to the neodymium iron boron magnetic body electroplating pretreatment process of control, with
Become that merit is good in neodymium iron boron magnetic body substrates adhesion, the ni-w-p alloy coating of excellent corrosion-proof performance, solve
The critical defect of neodymium iron boron magnetic body corrosion resistance difference.
Summary of the invention
Combine the ability of ni-w-p alloy coating for neodymium-iron-boron surface in prior art, cause neodymium iron boron
The defect of magnet corrosion resistance difference, it is an object of the invention to be to provide one to carry out neodymium-iron-boron surface simply
Process, neodymium-iron-boron surface and ni-w-p alloy coating can be strengthened effectively by neodymium iron boron magnetic body Surface uniformization
Adhesion, the method improving the corrosion resisting property of neodymium iron boron magnetic body.
The technique that the invention provides a kind of Sintered NdFeB magnet electroplating nickel on surface tungsten phosphorus, this technique is to sinter
After the surface of neodymium iron boron magnetic body sequentially passes through polishing, alkaline degreasing, hot wash process, being placed in concentration is
In the oxalic acid solution of 10～120g/L, carry out soaking activation processing or ultrasonic wave added activation processing；In activation processing
After Sintered NdFeB magnet electroplating nickel on surface tungsten phosphor alloy coating.
The technique of the Sintered NdFeB magnet electroplating nickel on surface tungsten phosphorus of the present invention also includes following preferred version:
Preferably the concentration of scheme mesoxalic acid solution is 20～100g/L；Most preferably 40～90g/L.
Preferably in scheme, the immersion activation processing time is 1～8min；Most preferably 3～8min.
Preferably in scheme, ultrasonic wave added activation processing is under the ultrasonic wave added that frequency is 35000～45000Hz
Immersion treatment 1～8min；Most preferably activation processing 2～4min under the ultrasonic wave added that frequency is 40000Hz.
Preferably in scheme, hot wash is to use the hot water of 45～55 DEG C to carry out ultrasonic wave added washing.Described heat
Water washing is at least to use the hot water of 45～55 DEG C to carry out ultrasonic wave added washed once, and washing for the first time
Hot water must be used.
Preferably in scheme, grinding process is by oils and fats, oxide skin and the corrosion product on Sintered NdFeB magnet surface
Carry out machinery removing, and is polished in corner, it is thus achieved that the magnet surface of smooth.
Preferably scheme neutral and alkali oil removal treatment is to be placed in alkaline solution by Sintered NdFeB magnet 65～70
DEG C alkaline solution in supersound process 3～8min；Described alkaline solution includes following components: sodium hydroxide,
Sodium phosphate, sodium carbonate, surfactant and water.
The technique of described Sintered NdFeB magnet electroplating nickel on surface tungsten phosphor alloy coating uses of the prior art
Technique, used the plating solution formula of the nickel tungsten electroplating phosphor alloy coating as described in patent ZL200810143741.X
And technological parameter.
The technique of the Sintered NdFeB magnet electroplating nickel on surface tungsten phosphorus of the present invention, including step in detail below:
(1) polishing:
Oils and fats, oxide skin and corrosion product, the corner on Sintered NdFeB magnet surface is entered mechanical grinding and is processed,
Obtain the freshest magnet surface, then use ultrasonic assistant washing；
(2) alkaline degreasing:
With sodium hydroxide 5～15g/L, sodium phosphate 120～180g/L, sodium carbonate 30～80g/L, surfactant
0.1～0.5g/L preparation alkaline aqueous solution；Sintered NdFeB magnet after grinding process is placed in alkaline aqueous solution,
Supersound process 3～8min in the alkaline solution of 65～70 DEG C；The hot water of 45～55 DEG C is used to carry out after alkaline degreasing
Washing；
(3) oxalic acid activation processing:
Sintered NdFeB magnet through chemistry alkalescence oil removal treatment is placed in concentration is 10～120g/L
In oxalic acid solution, carry out soaking activation processing 1～8 or under the ultrasonic wave added that frequency is 35000～45000Hz
Activation processing 1～8min；
(4) nickel tungsten electroplating phosphor alloy coating:
Sintered NdFeB magnet after activation processing is carried out nickel tungsten electroplating phosphor alloy coating, then rinses with water dry
Clean.
Beneficial effects of the present invention: the present invention uses oxalic acid solution that neodymium-iron-boron surface is passivated place first
Reason, forms the oxalates passivating film of one layer of dense uniform, and on the one hand this passivating film is follow-up nickel tungsten electroplating phosphorus alloy
Coating provides a chemical composition and the uniform apparent condition of electrochemistry, effectively improves neodymium-iron-boron surface
With ni-w-p alloy binding force of cladding material, this passivating film can avoid neodymium iron boron magnetic body corruption in subsequent handling simultaneously
Erosion, substantially increases the corrosion resisting property of neodymium iron boron magnetic body.The process technique of the present invention also simplifies existing skill
The technique of the neodymium iron boron magnetic body electroplating nickel on surface tungsten phosphor alloy coating in art, greatly reduces production cost.Simultaneously
The present invention uses oxalic acid solution to replace fluoride of the prior art and processes, and effectively reduces and has human body and environment
The use of the fluoride of evil.And to the fluoride not used in the preprocessing process of neodymium iron boron magnetic body.
Proved by substantial amounts of experiment: utilize the technique of the present invention to obtain dense uniform in neodymium-iron-boron surface
Amorphous nickel tungsten phosphorus electrodeposited coating, by standard GB/T/T5270-2005 hot cold cycle test method to this gold
The bond strength belonging to coating layer is tested, and result shows that electrodeposited coating can bear more than 15 times thermal shocks experiment
(220 DEG C, 1h), surface does not has bubbling, peeling and the phenomenon such as come off, and electrodeposited coating is good with the adhesion of magnet；
According to standard GB/T/T10125-1997 " artificial atmosphere corrosion testing-salt spray test ", at 5% saline solution
In neutral salt spray test, utilize the nickel tungsten phosphorus electrodeposited coating experience that the method for the present invention obtains in neodymium-iron-boron surface
1024h rear surface still occurs without point corrosion, and coating still has uniform metallic luster, and the present invention is at neodymium ferrum
The corrosion resistance of the nickel tungsten phosphorus electrodeposited coating that boron magnet surface obtains is good.Magnetic property testing result shows, uses the present invention
Described method, does not makes significant difference to the magnetic property of neodymium iron boron magnetic body.
Accompanying drawing explanation
[Fig. 1] is contrast scans Electronic Speculum figure before and after embodiment 1 mesoxalic acid solution activation processing neodymium-iron-boron surface；
Before a is oxalic acid activation, after b is oxalic acid activation.
[Fig. 2] is that the Sintered NdFeB magnet being coated with ni-w-p alloy coating prepared in embodiment 1 is through 1024h
After salt mist experiment, the change comparison diagram of the ni-w-p alloy coating on Sintered NdFeB magnet surface: a salt spray test
Before, b, after 1024h salt spray test.
[Fig. 3] is demagnetizing curve: a before and after nickel plating tungsten phosphor alloy coating of the Sintered NdFeB magnet in embodiment 1
For NdFeB magnet, b is the NdFeB magnet after plating NiWP alloy.
Detailed description of the invention
Below in conjunction with specific embodiment, present disclosure is described further, but the scope of protection of the invention
It is not limited only to these examples.
Embodiment 1
A kind of Sintered NdFeB magnet electroplating nickel on surface tungsten phosphorus process, comprises the steps:
(1) oils and fats, oxide skin and the corrosion product of neodymium-iron-boron surface, corner are polishing to 2000#,
Obtaining the freshest magnet surface, then ultrasound wave or water are cleaned；
(2) chemistry alkalescence oil removal treatment, prepares alkaline degreasing liquid, and this liquid includes sodium hydroxide 10g/L,
Sodium phosphate 150g/L, sodium carbonate 50g/L, surfactant 0.3g/L, surplus is water.Wherein surfactant
For dodecyl sodium sulfate.Water is distilled water or deionized water；Alkaline degreasing liquid is heated to 65 DEG C, will
The neodymium iron boron magnetic body of polishing is put into and is washed 5min in alkaline degreasing, then carries out three washings, wherein with ultrasound wave
First step washing is 50 DEG C of hot water wash；
(3) acidic activated process, the acid activating solution of preparation, this liquid includes oxalic acid 20g/L, and surplus is
Water, water is distilled water or deionized water, the neodymium iron boron magnetic body through alkaline degreasing is put into acidic activated liquid and exists
Room temperature 40000Hz frequency ultrasonic wave processes 2min, then cleans with ultrasound wave or water；
(4) nickel tungsten electroplating phosphor alloy coating, by above-mentioned Sintered NdFeB magnet after homogenization pre-treatment
The plating solution formula of employing nickel tungsten electroplating phosphor alloy coating described in patent ZL200810143741.X and technique
Parameter carries out nickel tungsten electroplating phosphor alloy coating, then rinses well with water.
Embodiment 2
A kind of Sintered NdFeB magnet electroplating nickel on surface tungsten phosphorus process, comprises the steps:
(1) oils and fats, oxide skin and the corrosion product of neodymium-iron-boron surface, corner are polishing to 2000#,
Obtaining the freshest magnet surface, then ultrasound wave or water are cleaned；
(2) chemistry alkalescence oil removal treatment, prepares alkaline degreasing liquid, and this liquid includes sodium hydroxide 8g/L,
Sodium phosphate 150g/L, sodium carbonate 50g/L, surfactant 0.5g/L, surplus is water.Wherein surfactant
For octyl phenol polyoxyethylene ether-10 (OP-10).Water is distilled water or deionized water；By alkaline degreasing
Liquid is heated to 70 DEG C, is put into by the neodymium iron boron magnetic body of polishing and washes 8min in alkaline degreasing, then enters with ultrasound wave
Three washings of row, wherein first step washing is 55 DEG C of hot water wash；
(3) acidic activated process, the acid activating solution of preparation, this liquid includes oxalic acid 70g/L, and surplus is
Water, water is distilled water or deionized water, the neodymium iron boron magnetic body through alkaline degreasing is put into acidic activated liquid and exists
Soaking at room temperature processes 8min, then cleans with ultrasound wave or water；
(4) nickel tungsten electroplating phosphor alloy coating, by above-mentioned Sintered NdFeB magnet after homogenization pre-treatment
The plating solution formula of employing nickel tungsten electroplating phosphor alloy coating described in patent ZL200810143741.X and technique
Parameter carries out nickel tungsten electroplating phosphor alloy coating, then rinses well with water.
Embodiment 3
A kind of Sintered NdFeB magnet electroplating nickel on surface tungsten phosphorus process, comprises the steps:
(1) oils and fats, oxide skin and the corrosion product of neodymium-iron-boron surface, corner are polishing to 2000#,
Obtaining the freshest magnet surface, then ultrasound wave or water are cleaned；
(2) chemistry alkalescence oil removal treatment, prepares alkaline degreasing liquid, and this liquid includes sodium hydroxide 6g/L,
Sodium phosphate 120g/L, sodium carbonate 80g/L, surfactant 0.5g/L, surplus is water.Wherein surfactant
For dodecyl sodium sulfate.Water is distilled water or deionized water；Alkaline degreasing liquid is heated to 65 DEG C, will
The neodymium iron boron magnetic body of polishing is put into and is washed 5min in alkaline degreasing, then carries out three washings, wherein with ultrasound wave
First step washing is 50 DEG C of hot water wash；
(3) acidic activated process, the acid activating solution of preparation, this liquid includes oxalic acid 50g/L, and surplus is
Water, water is distilled water or deionized water, the neodymium iron boron magnetic body through alkaline degreasing is put into acidic activated liquid and exists
Process 4min under room temperature ultrasonic auxiliary, then clean with ultrasound wave or water；
(4) nickel tungsten electroplating phosphor alloy coating, by above-mentioned Sintered NdFeB magnet after homogenization pre-treatment
The plating solution formula of employing nickel tungsten electroplating phosphor alloy coating described in patent ZL200810143741.X and technique
Parameter carries out nickel tungsten electroplating phosphor alloy coating, then rinses well with water.
Embodiment 4
A kind of Sintered NdFeB magnet electroplating nickel on surface tungsten phosphorus process, comprises the steps:
(1) oils and fats, oxide skin and the corrosion product of neodymium-iron-boron surface, corner are polishing to 2000#,
Obtaining the freshest magnet surface, then ultrasound wave or water are cleaned；
(2) chemistry alkalescence oil removal treatment, prepares alkaline degreasing liquid, and this liquid includes sodium hydroxide 4g/L,
Sodium phosphate 180g/L, sodium carbonate 30g/L, surfactant 0.5g/L, surplus is water.Wherein surfactant
For dodecyl sodium sulfate.Water is distilled water or deionized water；Alkaline degreasing liquid is heated to 70 DEG C, will
The neodymium iron boron magnetic body of polishing is put into and is washed 3min in alkaline degreasing, then carries out three washings, wherein with ultrasound wave
First step washing is 45 DEG C of hot water wash；
(3) acidic activated process, the acid activating solution of preparation, this liquid includes oxalic acid 100g/L, and surplus is
Water, water is distilled water or deionized water, the neodymium iron boron magnetic body through alkaline degreasing is put into acidic activated liquid and exists
Soaking at room temperature processes 3min, then cleans with ultrasound wave or water；
(4) nickel tungsten electroplating phosphor alloy coating, by above-mentioned Sintered NdFeB magnet after homogenization pre-treatment
The plating solution formula of employing nickel tungsten electroplating phosphor alloy coating described in patent ZL200810143741.X and technique
Parameter carries out nickel tungsten electroplating phosphor alloy coating, then rinses well with water.
Comparative example 1
Sintered NdFeB magnet is polished by embodiment 1 method, according to conventional pre-electroplating treatment through polishing → changing
Electroplate after learning alkaline degreasing → pickling (dust technology+thiourea) → activation (ammonium acid fluoride+sulfosalicylic acid)
Nickel tungsten phosphorus coating, then rinses well with water.
Embodiment 1～4 and the method for testing of comparative example 1 and data:
The neodymium iron boron after different pre-treatments PROCESS FOR TREATMENT with the experiment of hot SAPMAC method and neutral salt spray test test
Adhesion and corrosion resisting property between the ni-w-p alloy coating of magnet and plating are studied, and the results are shown in Table
1。
Between the table 1 neodymium iron boron magnetic body and the ni-w-p alloy coating of plating after different pre-treatments PROCESS FOR TREATMENT
Adhesion and corrosion resisting property
From table 1 it follows that obtain by the Sintered NdFeB magnet electroplating nickel on surface tungsten phosphorus process of the present invention
The neodymium iron boron magnetic body of the plated nickel tungsten phosphorus electrodeposited coating obtained, can bear 15 thermal shocks experiment, and coating surface is without drum
Bubble, peeling and the phenomenon such as come off, and after the neutral salt spray test of 1024h can be born coating surface without spot corrosion
Phenomenon occurs.And by the method for comparative example at Sintered NdFeB magnet electroplating nickel on surface tungsten phosphor alloy coating, at most
Thermal shock experiment surface can be born and arise that crackle and coating burst phenomenon, and coating is through 72h
Neutral salt spray test rear surface there will be spot corrosion and bubbling phenomenon occurs in coating surface.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, all in the present invention
Spirit and principle within any amendment of being made, equivalent substitute and improvement etc., the guarantor of the present invention all should be included in
In the range of protecting.
Claims (6)
1. the technique of a Sintered NdFeB magnet electroplating nickel on surface tungsten phosphorus, it is characterised in that by sintered NdFeB magnetic
After the surface of body sequentially passes through polishing, alkaline degreasing, hot wash process, being placed in concentration is 10～120g/L
In oxalic acid solution, carry out soaking activation processing or ultrasonic wave added activation processing；Sintering neodymium ferrum after activation processing
Boron magnet surface nickel tungsten electroplating phosphor alloy coating.
2. technique as claimed in claim 1, it is characterised in that the concentration of oxalic acid solution is 20～100g/L.
3. technique as claimed in claim 2, it is characterised in that the concentration of oxalic acid solution is 40～90g/L.
4. technique as claimed in claim 1, it is characterised in that the described immersion activation processing time is 1～8min.
5. technique as claimed in claim 1, it is characterised in that described ultrasonic wave added activation processing is in frequency
It it is activation processing 1～8min under the ultrasonic wave added of 35000～45000Hz.
6. the technique as described in any one of Claims 1 to 5, it is characterised in that described hot wash is to use 45～55
DEG C hot water carry out ultrasonic wave added washing.
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| CN106298220A (en) * | 2016-08-30 | 2017-01-04 | 浙江凯文磁业有限公司 | A kind of preparation method of the composite coating of motor Sintered NdFeB magnet |
| CN106435678B (en) * | 2016-11-21 | 2019-02-19 | 京磁材料科技股份有限公司 | The electro-plating pre-treatment method and equipment of neodymium iron boron magnetic body |
| CN106544664A (en) * | 2016-12-07 | 2017-03-29 | 北京京磁电工科技有限公司 | Neodymium iron boron magnetic body passivator and its application |
| CN111128502B (en) * | 2019-12-04 | 2022-03-25 | 湖南航天磁电有限责任公司 | Preparation method of super-corrosion-resistant high-performance sintered samarium-cobalt magnet |
| CN113684480A (en) * | 2021-08-17 | 2021-11-23 | 杭州象限科技有限公司 | Process for regulating and controlling chemical nickel stability in neodymium iron boron electroplating |
| CN113699567B (en) * | 2021-08-27 | 2022-08-26 | 杭州象限科技有限公司 | Ultrathin plating electroplating method applied to neodymium iron boron surface treatment |
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| JPH02310395A (en) * | 1989-05-26 | 1990-12-26 | Johoku Riken Kogyo:Kk | Method for preventing corrosion of neodymium-iron-boron sintered magnet |
| JP2006070280A (en) * | 2004-08-31 | 2006-03-16 | Tdk Corp | Plating method |
| CN101373651B (en) * | 2007-08-23 | 2011-12-07 | 北京中科三环高技术股份有限公司 | Surface pretreating method of wet method spray sand type neodymium iron boron permanent magnetic material |
| CN101728042B (en) * | 2008-10-16 | 2012-07-18 | 北京中科三环高技术股份有限公司 | Technique for treating surface of permanent magnet material |
| CN101445946B (en) * | 2008-11-27 | 2011-02-09 | 湖南纳菲尔新材料科技股份有限公司 | Anticorrosive wearable electrodeposit clad layer of Ni-W-P ternary alloy and manufacturing technique and electroplate liquid thereof |
| CN102108511A (en) * | 2010-12-24 | 2011-06-29 | 烟台正海磁性材料股份有限公司 | Electroplating and chemical plating composite protecting process for NdFeB permanent magnet and NdFeB permanent magnet with composite protective layer |
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