CN104073849A - Technique for electroplating nickel-tungsten-phosphorus on surface of sintered neodymium-iron-boron magnet - Google Patents
Technique for electroplating nickel-tungsten-phosphorus on surface of sintered neodymium-iron-boron magnet Download PDFInfo
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Abstract
The invention discloses a technique for electroplating nickel-tungsten-phosphorus on the surface of a sintered neodymium-iron-boron magnet, which comprises the following steps: sequentially carrying out sanding, alkaline deoiling and hot water washing treatment on the surface of the sintered neodymium-iron-boron magnet, putting in an oxalic acid solution, carrying out immersion or ultrasonic activating treatment, and electroplating a nickel-tungsten-phosphorus alloy coating on the surface of the sintered neodymium-iron-boron magnet subjected to activating treatment. The technique solves the problems of chemical component and electrochemical nonuniformity on the surface of the sintered neodymium-iron-boron magnet, is capable of effectively uniformizing the surface of the neodymium-iron-boron magnet, enhancing the binding force between the neodymium-iron-boron magnet surface and the nickel-tungsten-phosphorus alloy coating and improving the corrosion resistance of the neodymium-iron-boron magnet, has the advantages of simple process and low production cost, and can be used in industry.
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, the people such as assistant river utilize powder metallurgic method to develop high performance neodymium iron boron series permanent magnet in Japan first, refreshed the highest record of permanent magnet performance, once coming out, just obtained develop rapidly, at magneticsubstance industry market dominate, make it in modern industry and electronic technology, obtain wide market outlook.But due to neodymium-iron-boron magnetic material surface porosity porous, chemically reactive by force, very easily a lot of defects such as oxidation corrosion have a strong impact on its range of application.Therefore, the prerequisite of NdFeB material widespread use is first to solve the not corrosion resistant critical defect of magnet.
Neodymium iron boron magnetic body is mainly by three phase composites, be principal phase, rich neodymium phase and boron-rich phase, wherein rich neodymium phase and boron-rich phase are generally all distributed in grain boundaries, rich neodymium is very easily oxidized mutually, and the volume fraction of magnet principal phase is far longer than the volume fraction of rich neodymium phase and boron-rich phase, so magnet easily has the feature of the electrochemistry local corrosion battery of the large negative electrode of primary anode, will further accelerate intergranular corrosion; In addition, because the corrosion potential of rich neodymium phase is lower, easily there is galvanic corrosion.Therefore, must carry out surfacecti proteon to neodymium-iron-boron magnetic material.
The main method that solves at present neodymium iron boron magnetic body etching problem is that main treatment process is the process of surface treatment such as plating or electroless plating at magnet surface deposition one deck corrosion-resistant coating.The key of neodymium iron boron magnetic body process for treating surface is pre-treating technology.If pre-treating technology is suitable, once successfully form after bottom in magnet surface, just can form the rete with property in magnet surface, to be applicable to various Working environments.Yet neodymium iron boron magnetic body is heterogeneous structure, this makes magnet is all inhomogeneous in chemical composition and electrochemistry, the potential difference that each alternate existence is very large, and when magnet is placed in treatment solution, different meeting shows different electrochemical behaviors.Therefore, people have carried out a large amount of research to neodymium iron boron magnetic body pre-treatment, at present to the most frequently used pre-treating process of neodymium iron boron magnetic body, be: polishing → alkali cleaning oil removing → nitric acid+thiocarbamide pickling → ammonium bifluoride+sulphosalicylic acid activation (Palladous chloride ethanol solution), because Nd-Fe-Bo permanent magnet material is the porous material being formed by powder metallurgical technique compacting, magnet can cause hydrogen embrittlement because of pickling, and pickle solution enters the further corrosion that can cause material in the hole of neodymium iron boron, thereby cause the surperficial efflorescence of Nd-Fe-B permanent magnet, coating easily comes off, degradation under magnetic property; Fluorion is harmful to human body and environment; Palladium is that precious metal makes its range of application limited; In addition, conventional pre-treatment is at present divided into pickling and two treatment steps of activation, and technique is more loaded down with trivial details, and the operating time is difficult to control, and plated item success ratio is lower.Nickel tungsten phosphorus electrolytic coating has high rigidity, high thermal stability, high-wearing feature and excellent corrosion resistance nature etc. and has broad application prospects, and the relevant research at neodymium iron boron magnetic body directly electroplating on surface ni-w-p alloy coating so far have not been reported.
Therefore, be badly in need of exploitation a kind of simple to operate, be easy to the neodymium iron boron magnetic body electroplating pretreatment process of controlling, so that success is good in neodymium iron boron magnetic body substrates bonding force, the ni-w-p alloy coating of excellent corrosion-proof performance, solve the poor critical defect of neodymium iron boron magnetic body solidity to corrosion.
Summary of the invention
Ability for neodymium iron boron magnetic body surface bonding ni-w-p alloy coating in prior art, cause the poor defect of neodymium iron boron magnetic body solidity to corrosion, the object of the invention is to be to provide a kind of simple process is carried out in neodymium-iron-boron surface, can be effectively by neodymium iron boron magnetic body surface uniform, strengthen neodymium-iron-boron surface and ni-w-p alloy binding force of cladding material, improve the method for the corrosion resisting property of neodymium iron boron magnetic body.
The invention provides a kind of technique of Sintered NdFeB magnet electroplating nickel on surface tungsten phosphorus, this technique be by the surface of Sintered NdFeB magnet successively after polishing, alkaline degreasing, hot wash are processed, be placed in the oxalic acid solution that concentration is 10～120g/L, soak activation treatment or ultrasonic auxiliary activation treatment; Sintered NdFeB magnet electroplating nickel on surface tungsten phosphor alloy coating after activation treatment.
The technique of Sintered NdFeB magnet electroplating nickel on surface tungsten phosphorus of the present invention also comprises following preferred version:
The concentration of preferred scheme mesoxalic acid solution is 20～100g/L; Most preferably be 40～90g/L.
In preferred scheme, soaking the activation treatment time is 1～8min; Most preferably be 3～8min.
In preferred scheme, ultrasonic auxiliary activation treatment is the ultrasonic auxiliary lower immersion treatment 1～8min that is 35000～45000Hz in frequency; Ultrasonic auxiliary lower activation treatment 2～4min that most preferably to be in frequency be 40000Hz.
In preferred scheme, hot wash is to adopt the hot water of 45～55 ℃ to carry out ultrasonic auxiliary washing.It is at least to adopt the hot water of 45～55 ℃ to carry out ultrasonic auxiliary washing once that described hot wash is processed, and washing for the first time must adopt hot water.
In preferred scheme, grinding process is the grease on Sintered NdFeB magnet surface, oxide skin and corrosion product to be carried out to machinery remove, and is polished in corner, obtains the magnet surface of smooth.
Preferred scheme neutral and alkali oil removal treatment is that Sintered NdFeB magnet is placed in to basic solution at the basic solution supersound process 3～8min of 65～70 ℃; Described basic solution comprises following component: sodium hydroxide, sodium phosphate, sodium carbonate, tensio-active agent and water.
The process using technique of the prior art of described Sintered NdFeB magnet electroplating nickel on surface tungsten phosphor alloy coating, plating solution formula and the processing parameter of the nickel tungsten electroplating phosphor alloy coating as described in employing patent ZL200810143741.X.
The technique of Sintered NdFeB magnet electroplating nickel on surface tungsten phosphorus of the present invention, comprises following concrete steps:
(1) polishing:
Mechanical grinding is entered in the grease on Sintered NdFeB magnet surface, oxide skin and corrosion product, corner and process, obtain evenly fresh magnet surface, then adopt the auxiliary washing of ultrasonic wave;
(2) alkaline degreasing:
With sodium hydroxide 5～15g/L, sodium phosphate 120～180g/L, sodium carbonate 30～80g/L, tensio-active agent 0.1～0.5g/L prepares alkaline aqueous solution; Sintered NdFeB magnet after grinding process is placed in to alkaline aqueous solution, supersound process 3～8min in the basic solution of 65～70 ℃; After alkaline degreasing, adopt the hot water of 45～55 ℃ to wash;
(3) oxalic acid activation treatment:
Sintered NdFeB magnet through chemical alkaline oil removal treatment is placed in to the oxalic acid solution that concentration is 10～120g/L, the ultrasonic auxiliary lower activation treatment 1～8min that soaks activation treatment 1～8 or be 35000～45000Hz in frequency;
(4) nickel tungsten electroplating phosphor alloy coating:
Sintered NdFeB magnet after activation treatment is carried out to nickel tungsten electroplating phosphor alloy coating, and then water is rinsed well.
Beneficial effect of the present invention: the present invention adopts oxalic acid solution to carry out Passivation Treatment to neodymium-iron-boron surface first, form the fine and close oxalate passive film uniformly of one deck, on the one hand this passive film provides a chemical composition and the uniform condition of surface of electrochemistry for follow-up nickel tungsten electroplating phosphor alloy coating, neodymium-iron-boron surface and ni-w-p alloy binding force of cladding material have effectively been improved, this passive film can be avoided the corrosion of neodymium iron boron magnetic body in subsequent handling simultaneously, has greatly improved the corrosion resisting property of neodymium iron boron magnetic body.Treatment process of the present invention has also been simplified the technique of neodymium iron boron magnetic body electroplating nickel on surface tungsten phosphor alloy coating of the prior art greatly, greatly reduces production cost.Simultaneously the present invention adopts oxalic acid solution to replace Fluoridizing of the prior art, effectively reduces the use to human body and the harmful fluorochemical of environment.And to obsolete fluorochemical in the preprocessing process of neodymium iron boron magnetic body.
By a large amount of experimental results show that: utilize technique of the present invention to obtain fine and close amorphous nickel tungsten phosphorus electrolytic coating uniformly in neodymium-iron-boron surface, by standard GB/T/T5270-2005 hot cold cycle test method, the bonding strength of this metal-plated coating is tested, result shows that electrolytic coating can bear (220 ℃ of 15 above thermal shock experiments, 1h), surface does not have bubbling, peeling and the phenomenon such as come off, and the bonding force of electrolytic coating and magnet is good; According to standard GB/T/T10125-1997 < < artificial atmosphere corrosion test-salt-fog test > >, in the neutral salt spray test of 5% salt solution, utilize the nickel tungsten phosphorus electrolytic coating experience 1024h rear surface that method of the present invention obtains in neodymium-iron-boron surface still without point corrosion, to occur, coating still has uniform metalluster, and the solidity to corrosion of the nickel tungsten phosphorus electrolytic coating that the present invention obtains in neodymium-iron-boron surface is good.Magnetic property detected result shows, by the method for the invention, the magnetic property of neodymium iron boron magnetic body is not made significant difference.
Accompanying drawing explanation
[Fig. 1] is the front and back contrast scans Electronic Speculum figure of embodiment 1 mesoxalic acid solution activation treatment neodymium-iron-boron surface; Before a is oxalic acid activation, after b is oxalic acid activation.
[Fig. 2] is for the Sintered NdFeB magnet that is coated with ni-w-p alloy coating that makes in embodiment 1 is after 1024h salt mist experiment, the variation comparison diagram of the ni-w-p alloy coating on Sintered NdFeB magnet surface: before a salt-fog test, b, after 1024h salt-fog test.
[Fig. 3] is that Sintered NdFeB magnet demagnetizing curve: a before and after nickel plating tungsten phosphor alloy coating in embodiment 1 is NdFeB magnet, and b is the NdFeB magnet after plating NiWP alloy.
Embodiment
Below in conjunction with specific embodiment, content of the present invention is described further, but the scope of protection of the invention is not limited only to these examples.
Embodiment 1
A Sintered NdFeB magnet electroplating nickel on surface tungsten phosphorus processing method, comprises the steps:
(1) polished to 2000# in the grease of neodymium-iron-boron surface, oxide skin and corrosion product, corner, obtain evenly fresh magnet surface, then ultrasonic wave or water are cleaned;
(2) chemical alkaline oil removal treatment, preparation alkaline degreasing liquid, this liquid comprises sodium hydroxide 10g/L, sodium phosphate 150g/L, sodium carbonate 50g/L, tensio-active agent 0.3g/L, surplus is water.Wherein tensio-active agent is sodium laurylsulfonate.Water is distilled water or deionized water; Alkaline degreasing liquid is heated to 65 ℃, the neodymium iron boron magnetic body of polishing is put into alkaline degreasing and wash 5min, then by ultrasonic wave, carry out three washings, wherein the first step washing is 50 ℃ of hot water wash;
(3) acidic activated processing, prepare acid activation solution, this liquid comprises oxalic acid 20g/L, surplus is water, water is distilled water or deionized water, by putting into acidic activated liquid through the neodymium iron boron magnetic body of alkaline degreasing, in room temperature, with 40000Hz frequency ultrasonic wave, process 2min, then with ultrasonic wave or water, clean;
(4) nickel tungsten electroplating phosphor alloy coating, plating solution formula and the processing parameter of the nickel tungsten electroplating phosphor alloy coating described in above-mentioned Sintered NdFeB magnet employing patent ZL200810143741.X after homogenizing pre-treatment are carried out to nickel tungsten electroplating phosphor alloy coating, and then water is rinsed well.
Embodiment 2
A Sintered NdFeB magnet electroplating nickel on surface tungsten phosphorus processing method, comprises the steps:
(1) polished to 2000# in the grease of neodymium-iron-boron surface, oxide skin and corrosion product, corner, obtain evenly fresh magnet surface, then ultrasonic wave or water are cleaned;
(2) chemical alkaline oil removal treatment, preparation alkaline degreasing liquid, this liquid comprises sodium hydroxide 8g/L, sodium phosphate 150g/L, sodium carbonate 50g/L, tensio-active agent 0.5g/L, surplus is water.Wherein tensio-active agent is octyl phenol Soxylat A 25-7-10 (OP-10).Water is distilled water or deionized water; Alkaline degreasing liquid is heated to 70 ℃, the neodymium iron boron magnetic body of polishing is put into alkaline degreasing and wash 8min, then by ultrasonic wave, carry out three washings, wherein the first step washing is 55 ℃ of hot water wash;
(3) acidic activated processing, prepares acid activation solution, and this liquid comprises oxalic acid 70g/L, surplus is water, water is distilled water or deionized water, by putting into acidic activated liquid through the neodymium iron boron magnetic body of alkaline degreasing, in soaking at room temperature, processes 8min, then with ultrasonic wave or water, cleans;
(4) nickel tungsten electroplating phosphor alloy coating, plating solution formula and the processing parameter of the nickel tungsten electroplating phosphor alloy coating described in above-mentioned Sintered NdFeB magnet employing patent ZL200810143741.X after homogenizing pre-treatment are carried out to nickel tungsten electroplating phosphor alloy coating, and then water is rinsed well.
Embodiment 3
A Sintered NdFeB magnet electroplating nickel on surface tungsten phosphorus processing method, comprises the steps:
(1) polished to 2000# in the grease of neodymium-iron-boron surface, oxide skin and corrosion product, corner, obtain evenly fresh magnet surface, then ultrasonic wave or water are cleaned;
(2) chemical alkaline oil removal treatment, preparation alkaline degreasing liquid, this liquid comprises sodium hydroxide 6g/L, sodium phosphate 120g/L, sodium carbonate 80g/L, tensio-active agent 0.5g/L, surplus is water.Wherein tensio-active agent is sodium laurylsulfonate.Water is distilled water or deionized water; Alkaline degreasing liquid is heated to 65 ℃, the neodymium iron boron magnetic body of polishing is put into alkaline degreasing and wash 5min, then by ultrasonic wave, carry out three washings, wherein the first step washing is 50 ℃ of hot water wash;
(3) acidic activated processing, prepares acid activation solution, and this liquid comprises oxalic acid 50g/L, surplus is water, water is distilled water or deionized water, by putting into acidic activated liquid through the neodymium iron boron magnetic body of alkaline degreasing at the auxiliary lower 4min of processing of room temperature ultrasonic, then with ultrasonic wave or water, cleans;
(4) nickel tungsten electroplating phosphor alloy coating, plating solution formula and the processing parameter of the nickel tungsten electroplating phosphor alloy coating described in above-mentioned Sintered NdFeB magnet employing patent ZL200810143741.X after homogenizing pre-treatment are carried out to nickel tungsten electroplating phosphor alloy coating, and then water is rinsed well.
Embodiment 4
A Sintered NdFeB magnet electroplating nickel on surface tungsten phosphorus processing method, comprises the steps:
(1) polished to 2000# in the grease of neodymium-iron-boron surface, oxide skin and corrosion product, corner, obtain evenly fresh magnet surface, then ultrasonic wave or water are cleaned;
(2) chemical alkaline oil removal treatment, preparation alkaline degreasing liquid, this liquid comprises sodium hydroxide 4g/L, sodium phosphate 180g/L, sodium carbonate 30g/L, tensio-active agent 0.5g/L, surplus is water.Wherein tensio-active agent is sodium laurylsulfonate.Water is distilled water or deionized water; Alkaline degreasing liquid is heated to 70 ℃, the neodymium iron boron magnetic body of polishing is put into alkaline degreasing and wash 3min, then by ultrasonic wave, carry out three washings, wherein the first step washing is 45 ℃ of hot water wash;
(3) acidic activated processing, prepares acid activation solution, and this liquid comprises oxalic acid 100g/L, surplus is water, water is distilled water or deionized water, by putting into acidic activated liquid through the neodymium iron boron magnetic body of alkaline degreasing, in soaking at room temperature, processes 3min, then with ultrasonic wave or water, cleans;
(4) nickel tungsten electroplating phosphor alloy coating, plating solution formula and the processing parameter of the nickel tungsten electroplating phosphor alloy coating described in above-mentioned Sintered NdFeB magnet employing patent ZL200810143741.X after homogenizing pre-treatment are carried out to nickel tungsten electroplating phosphor alloy coating, and then water is rinsed well.
Comparative example 1
Sintered NdFeB magnet is pressed to embodiment 1 method polishing, according to conventional pre-electroplating treatment, through polishing → chemical alkaline degreasing → pickling (rare nitric acid+thiocarbamide) → activation (ammonium bifluoride+sulphosalicylic acid) laggard electroplating nickel tungsten phosphorus coating, then water is rinsed well.
Embodiment 1～4 and comparative example's 1 testing method and data:
Neodymium iron boron magnetic body with the test of the cold circulation experiment of heat and neutral salt spray test after different pre-treatments art breading and bonding force and the corrosion resisting property between the ni-w-p alloy coating of plating are studied, and the results are shown in Table 1.
The neodymium iron boron magnetic body of table 1 after different pre-treatments art breading and bonding force and the corrosion resisting property between the ni-w-p alloy coating of plating
As can be seen from Table 1, the neodymium iron boron magnetic body of the plated nickel tungsten phosphorus electrolytic coating obtaining by Sintered NdFeB magnet electroplating nickel on surface tungsten phosphorus processing method of the present invention, can bear 15 thermal shocks experiment, coating surface is without bubbling, peeling and the phenomenon such as come off, and after can bearing the neutral salt spray test of 1024h, coating surface occurs without point corrosion.And by the method for comparative example at Sintered NdFeB magnet electroplating nickel on surface tungsten phosphor alloy coating, can bear at most thermal shock experiment surface and just there will be crackle and coating to burst phenomenon, and coating there will be spot corrosion and coating surface to occur bubbling phenomenon through 72h neutral salt spray test rear surface.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and substitute and improvement etc., all should be included in protection scope of the present invention.
Claims (6)
1. the technique of a Sintered NdFeB magnet electroplating nickel on surface tungsten phosphorus, it is characterized in that, by the surface of Sintered NdFeB magnet successively after polishing, alkaline degreasing, hot wash are processed, be placed in the oxalic acid solution that concentration is 10～120g/L, soak activation treatment or ultrasonic auxiliary activation treatment; Sintered NdFeB magnet electroplating nickel on surface tungsten phosphor alloy coating after activation treatment.
2. technique as claimed in claim 1, is characterized in that, the concentration of oxalic acid solution is 20～100g/L.
3. technique as claimed in claim 2, is characterized in that, the concentration of oxalic acid solution is 40～90g/L.
4. technique as claimed in claim 1, is characterized in that, the described immersion activation treatment time is 1～8min.
5. technique as claimed in claim 1, is characterized in that, ultrasonic auxiliary lower activation treatment 1～8min that described ultrasonic auxiliary activation treatment is is 35000～45000Hz in frequency.
6. the technique as described in claim 1～5 any one, is characterized in that, described hot wash is to adopt the hot water of 45～55 ℃ to carry out ultrasonic auxiliary washing.
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Cited By (6)
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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 |
| CN106435678A (en) * | 2016-11-21 | 2017-02-22 | 京磁材料科技股份有限公司 | Electroplating pretreatment method and equipment for neodymium-iron-boron magnet |
| 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 |
| CN111128502A (en) * | 2019-12-04 | 2020-05-08 | 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 |
| CN113699567A (en) * | 2021-08-27 | 2021-11-26 | 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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| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN106435678A (en) * | 2016-11-21 | 2017-02-22 | 京磁材料科技股份有限公司 | Electroplating pretreatment method and equipment for neodymium-iron-boron magnet |
| 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 |
| CN111128502A (en) * | 2019-12-04 | 2020-05-08 | 湖南航天磁电有限责任公司 | Preparation method of super-corrosion-resistant high-performance sintered samarium-cobalt magnet |
| 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 |
| CN113699567A (en) * | 2021-08-27 | 2021-11-26 | 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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