CN103710739B - The preparation method of sintered Nd-Fe-B permanent magnet surface ceramic coat - Google Patents
The preparation method of sintered Nd-Fe-B permanent magnet surface ceramic coat Download PDFInfo
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- CN103710739B CN103710739B CN201210379309.7A CN201210379309A CN103710739B CN 103710739 B CN103710739 B CN 103710739B CN 201210379309 A CN201210379309 A CN 201210379309A CN 103710739 B CN103710739 B CN 103710739B
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Abstract
The preparation method of a kind of sintered Nd-Fe-B permanent magnet surface ceramic coat, it comprises the following steps: (one) chamfering is polished: adopt machinery vibration, barreling chamfering method that sintered Nd-Fe-B permanent magnetic material is carried out surface grinding process；(2) degreasing degreasing: grinded for chamfering magnet is put into alkaline degreaser and carries out degreasing degreasing；(3) acid pickling and rust removing: put into acid solution and carry out acid pickling and rust removing；(4) differential arc oxidation: the permanent magnet after acid pickling and rust removing is put in electrolyte and carry out differential arc oxidation process；(5) flushing is dry: natural drying after the Nd-Fe-B permanent magnet distilled water flushing after being processed by differential arc oxidation, finally forms oxide ceramic coating at surface of Nd-Fe-B permanent magnet；It is simple that the present invention realizes commercial Application, and production cost is relatively low, not by the impact of magnet material contour structures, environmentally safe, can be effectively improved corrosion resistance and the wearability of neodymium iron boron magnetic body, extend the service life of magnet.
Description
Technical field
The present invention relates to the field of surface modification of metal material, the preparation method particularly relating to a kind of sintered Nd-Fe-B permanent magnet surface ceramic coat.
Background technology
Nd-Fe-B permanent magnet is because it has high saturation magnetization, coercivity and magnetic energy product and is widely used in fields such as microwave communication, audio-visual technology, high energy micromachine, instrument and meter, computer, magnetic separation technique, wind power generation, auto industry and medical apparatus and instruments.But owing to sintered Nd-Fe-B permanent magnet is subject to the restriction of production technology, there is substantial amounts of hole in surface, and neodymium iron boron itself is heterogeneous structure structure (Nd2Fe14B Hard Magnetic phase, rich-Nd phase and rich B phase), each alternate there is bigger chemical-electrical potential difference, easily form corrosion cell in a humid environment, occur to produce intercrystalline corrosion.The shortcoming of this corrosion resistance difference of sintered Nd-Fe-B permanent magnet has had a strong impact on it and has applied further, so the anticorrosion research of neodymium iron boron magnetic body receives significant attention.It is improve the maximally efficient way of Nd-Fe-B permanent magnet decay resistance that current surfacecti proteon processes, mainly have the sufacings such as bonderizing, plating, electrophoretic coating, chemical plating, magnetron sputtering, ion plating, rare-earth conversion coatings, sol-gel individually or compound apply to the protection of Nd-Fe-B permanent magnet material.These methods are mainly formed with organic coating, metal coating and ceramic coating at surface of Nd-Fe-B permanent magnet, and wherein ceramic coating has corrosion resistance, the good anti-wear performance of excellence and can use in hot environment, becomes recent research focus.Existing magnetron sputtering technique can prepare aluminum oxide coating layer (ShoudongMao at surface of Nd-Fe-B permanent magnet at present, HengxiuYang, FengHuang, etal.AppliedSurfaceScience.2011,257:3980-3984) prepare titanium nitride coating (A.Ali with gas phase deposition technology, A.Ahmad, K.M.Deen.MaterialsandCorrosion.2010,61 (2): 130-135).Differential arc oxidation is to be placed in electrolyte aqueous solution by the metals such as Ti, Mg, Al or its alloy, utilize electrochemical method, the surface micropore of this material produces spark discharge speckle, under heat chemistry, plasma chemistry and electrochemical combined effect, the method for in-situ preparation ceramic membrane.But both at home and abroad prepare the report of ceramic coating but without carrying out differential arc oxidation process about sintered Nd-Fe-B permanent magnet up to now.
Summary of the invention
The preparation method that it is an object of the invention to provide a kind of sintered Nd-Fe-B permanent magnet surface ceramic coat, it is simple that it has technique, and cost is low, the advantage with the life-span of enhancing product performance.
The present invention is achieved like this, the preparation method of a kind of sintered Nd-Fe-B permanent magnet surface ceramic coat, it is characterised in that described preparation method comprises the following steps: (one) chamfering is polished: adopt machinery vibration, barreling chamfering method that sintered Nd-Fe-B permanent magnetic material is carried out surface grinding process；(2) degreasing degreasing: grinded for chamfering magnet is put into alkaline degreaser and carries out degreasing degreasing；(3) acid pickling and rust removing: put into acid solution and carry out acid pickling and rust removing；(4) differential arc oxidation: the permanent magnet after acid pickling and rust removing is put in electrolyte and carry out differential arc oxidation process；(5) flushing is dry: natural drying after the Nd-Fe-B permanent magnet distilled water flushing after being processed by differential arc oxidation, finally forms oxide ceramic coating at surface of Nd-Fe-B permanent magnet.Described acid solution is nitric acid, and concentration mass fraction is 2～20%, and pickling time is 10～180 seconds.Described electrolyte is sodium aluminate system, the mixed liquor that namely sodium aluminate and potassium dihydrogen phosphate are prepared with deionized water for solvent, its concentration respectively 10～30 g/l and 0.1 ~ 10 g/l.Described electrolyte is potassium fluorozirconate system, the mixed liquor that namely potassium fluorozirconate and phosphoric acid are prepared with deionized water for solvent, its concentration respectively 10～30 g/l and 5 ~ 20 g/l.Described electrolyte is potassium fluotitanate system, the mixed liquor that namely potassium fluotitanate and dipotassium hydrogen phosphate are prepared with deionized water for solvent, its concentration respectively 5～10 g/l and 5 ~ 10 g/l.Described differential arc oxidation processes as adopting bidirectional pulse mao power source, and with neodymium iron boron for positive pole, with stainless steel electrolytic groove for negative pole, and to control electrolyte temperature be 10～40 DEG C.The dutycycle that described differential arc oxidation processes the positive pulse voltage used to be 300 ~ 500V, negative pulse voltage be 10 ~ 200V, positive negative pulse stuffing operating frequency is 30 ~ 3000Hz and positive negative pulse stuffing processes 5 ~ 90min when being 5～50%.
The solution have the advantages that: the present invention can obtain oxide ceramic coating on sintered Nd-Fe-B permanent magnet surface, the magnetic property that Nd-Fe-B permanent magnet is intrinsic is uniformly 2～30 μm without impact, thickness by coating, coating and Nd-Fe-B permanent magnet bond strength > 20MPa, the corrosion potential relatively matrix covering ceramic coating Nd-Fe-B permanent magnet improves 0.1～0.5V, corrosion current improves 2～4 orders of magnitude, its salt-fog resistant test > 300h, PCT test > 100h；And it is simple that preparation method of the present invention realizes commercial Application, and production cost is relatively low, not by the impact of magnet material contour structures, environmentally safe, corrosion resistance and the wearability of neodymium iron boron magnetic body can be effectively improved, extend the service life of magnet.
Accompanying drawing explanation
Fig. 1 is the oxide ceramic coating surface SEM photograph that embodiment 1 obtains.
Fig. 2 is the oxide ceramic coating surface XRD figure spectrum that embodiment 1 obtains.
Detailed description of the invention
Embodiment 1
The preparation method of present embodiment sintered Nd-Fe-B permanent magnet surface ceramic coat sequentially includes the following steps:
(1) chamfering polishing: adopting machinery vibration, barreling chamfering method that 38SH sintered Nd-Fe-B permanent magnet is carried out surface grinding process, final size is 30 × 15 × 4mm；
(2) degreasing degreasing: grinded for chamfering magnet is put into 60 DEG C of alkaline degreasers (being mainly composed of sodium carbonate, sodium phosphate, sodium silicate and emulsifying agent etc.) and carries out 10min degreasing degreasing；
(3) acid pickling and rust removing: put into 5%HNO3Solution carries out acid pickling and rust removing 30s；
(4) differential arc oxidation: the permanent magnet after acid pickling and rust removing is put in electrolyte and carry out differential arc oxidation process, electrolyte is sodium aluminate system, namely the mixed liquor that sodium aluminate and potassium dihydrogen phosphate are prepared with deionized water for solvent, its concentration respectively 15 g/l and 5 g/l, differential arc oxidation processes and adopts bidirectional pulse mao power source, with neodymium iron boron for positive pole, with stainless steel electrolytic groove for negative pole, and to control electrolyte temperature be 10～40 DEG C, the positive pulse voltage used is 450V, negative pulse voltage is 10V, positive negative pulse stuffing operating frequency is the dutycycle of 300Hz and positive negative pulse stuffing processes 60min when being 5%；
(5) rinse dry: natural drying after the Nd-Fe-B permanent magnet distilled water flushing after differential arc oxidation is processed, finally form oxide ceramic coating at surface of Nd-Fe-B permanent magnet, it is thus achieved that surface SEM photograph such as accompanying drawing 1 of oxide ceramic coating；
The coating that present embodiment obtains is alumina ceramic coating, its oxide ceramic coating surface XRD figure is composed such as accompanying drawing 2, wherein " ▲ " represent sintered NdFeB matrix, " ◆ " represents aluminium oxide, it is thus achieved that alumina ceramic coating thickness be 5 ~ 10 μm, coating and Nd-Fe-B permanent magnet bond strength > 30MPa, the corrosion potential relatively matrix covering ceramic coating Nd-Fe-B permanent magnet improves 0.3V, corrosion current improves 4 orders of magnitude, its salt-fog resistant test > 600h, PCT test > 300h.
Embodiment 2
The preparation method of present embodiment sintered Nd-Fe-B permanent magnet surface ceramic coat sequentially includes the following steps:
(1) chamfering polishing: adopting machinery vibration, barreling chamfering method that 38SH sintered Nd-Fe-B permanent magnet is carried out surface grinding process, final size is 30 × 15 × 4mm；
(2) degreasing degreasing: grinded for chamfering magnet is put into 60 DEG C of alkaline degreasers (being mainly composed of sodium carbonate, sodium phosphate, sodium silicate and emulsifying agent etc.) and carries out 10min degreasing degreasing；
(3) acid pickling and rust removing: put into 10%HNO3Solution carries out acid pickling and rust removing 20s；
(4) differential arc oxidation: the permanent magnet after acid pickling and rust removing is put in electrolyte and carry out differential arc oxidation process, electrolyte is potassium fluorozirconate system, namely the mixed liquor that potassium fluorozirconate and phosphoric acid are prepared with deionized water for solvent, its concentration respectively 10 g/l and 10 g/l, differential arc oxidation processes and adopts bidirectional pulse mao power source, with neodymium iron boron for positive pole, with stainless steel electrolytic groove for negative pole, and to control electrolyte temperature be 10～40 DEG C, the positive pulse voltage used is 400V, negative pulse voltage is 30V, positive negative pulse stuffing operating frequency is the dutycycle of 60Hz and positive negative pulse stuffing processes 60min when being 5%；
(5) flushing is dry: natural drying after the Nd-Fe-B permanent magnet distilled water flushing after being processed by differential arc oxidation, finally forms oxide ceramic coating at surface of Nd-Fe-B permanent magnet；
The coating that present embodiment obtains is zirconia ceramics coating, thickness is 10 ~ 15 μm, coating and Nd-Fe-B permanent magnet bond strength > 25MPa, the corrosion potential relatively matrix covering ceramic coating Nd-Fe-B permanent magnet improves 0.15V, corrosion current improves 3 orders of magnitude, its salt-fog resistant test > 500h, PCT test > 100h.
Embodiment 3
The preparation method of present embodiment sintered Nd-Fe-B permanent magnet surface ceramic coat sequentially includes the following steps:
(1) chamfering polishing: adopting machinery vibration, barreling chamfering method that 38SH sintered Nd-Fe-B permanent magnet is carried out surface grinding process, final size is 30 × 15 × 4mm；
(2) degreasing degreasing: grinded for chamfering magnet is put into 60 DEG C of alkaline degreasers (being mainly composed of sodium carbonate, sodium phosphate, sodium silicate and emulsifying agent etc.) and carries out 10min degreasing degreasing；
(3) acid pickling and rust removing: put into 10%HNO3Solution carries out acid pickling and rust removing 20s；
(4) differential arc oxidation: the permanent magnet after acid pickling and rust removing is put in electrolyte and carry out differential arc oxidation process, electrolyte is potassium fluotitanate system, namely the mixed liquor that potassium fluotitanate and dipotassium hydrogen phosphate are prepared with deionized water for solvent, its concentration respectively 8 g/l and 6 g/l, differential arc oxidation processes as adopting bidirectional pulse mao power source, with neodymium iron boron for positive pole, with stainless steel electrolytic groove for negative pole, and to control electrolyte temperature be 10～40 DEG C, the positive pulse voltage used is 500V, negative pulse voltage is 100V, positive negative pulse stuffing operating frequency is the dutycycle of 500Hz and positive negative pulse stuffing processes 30min when being 10%；
(5) flushing is dry: natural drying after the Nd-Fe-B permanent magnet distilled water flushing after being processed by differential arc oxidation, finally forms oxide ceramic coating at surface of Nd-Fe-B permanent magnet；
The coating that present embodiment obtains is titanium oxide ceramics coating, thickness is 15 ~ 20 μm, coating and Nd-Fe-B permanent magnet bond strength > 20MPa, the corrosion potential relatively matrix covering ceramic coating Nd-Fe-B permanent magnet improves 0.1V, corrosion current improves 3 orders of magnitude, its salt-fog resistant test > 500h, PCT test > 100h.
Embodiment 4
The preparation method of present embodiment sintered Nd-Fe-B permanent magnet surface ceramic coat sequentially includes the following steps:
(1) chamfering polishing: adopting machinery vibration, barreling chamfering method that 28AH sintered Nd-Fe-B permanent magnet is carried out surface grinding process, final size is Φ 30 × 10mm；
(2) degreasing degreasing: grinded for chamfering magnet is put into 60 DEG C of alkaline degreasers (being mainly composed of sodium carbonate, sodium phosphate, sodium silicate and emulsifying agent etc.) and carries out 10min degreasing degreasing；
(3) acid pickling and rust removing: put into 5%HNO3Solution carries out acid pickling and rust removing 30s；
(4) differential arc oxidation: the permanent magnet after acid pickling and rust removing is put in electrolyte and carry out differential arc oxidation process, electrolyte is sodium aluminate system, namely the mixed liquor that sodium aluminate and potassium dihydrogen phosphate are prepared with deionized water for solvent, its concentration respectively 20 g/l and 5 g/l, differential arc oxidation processes as adopting bidirectional pulse mao power source, with neodymium iron boron for positive pole, with stainless steel electrolytic groove for negative pole, and to control electrolyte temperature be 10～40 DEG C, the positive pulse voltage used is 500V, negative pulse voltage is 10V, positive negative pulse stuffing operating frequency is the dutycycle of 50Hz and positive negative pulse stuffing processes 60min when being 5%；
(5) flushing is dry: natural drying after the Nd-Fe-B permanent magnet distilled water flushing after being processed by differential arc oxidation, finally forms oxide ceramic coating at surface of Nd-Fe-B permanent magnet；
The coating that present embodiment obtains is alumina ceramic coating, thickness is 15 ~ 20 μm, coating and Nd-Fe-B permanent magnet bond strength > 20MPa, the corrosion potential relatively matrix covering ceramic coating Nd-Fe-B permanent magnet improves 0.1V, corrosion current improves 3 orders of magnitude, its salt-fog resistant test > 400h, PCT test > 100h.
Claims (5)
1. the preparation method of a sintered Nd-Fe-B permanent magnet surface ceramic coat, it is characterised in that described preparation method comprises the following steps:
(1) chamfering polishing: adopt machinery vibration, barreling chamfering method that sintered Nd-Fe-B permanent magnetic material is carried out surface grinding process；
(2) degreasing degreasing: grinded for chamfering magnet is put into alkaline degreaser and carries out degreasing degreasing；
(3) acid pickling and rust removing: put into acid solution and carry out acid pickling and rust removing；
(4) differential arc oxidation: the permanent magnet after acid pickling and rust removing is put in electrolyte and carry out differential arc oxidation process；(5) flushing is dry: natural drying after the Nd-Fe-B permanent magnet distilled water flushing after being processed by differential arc oxidation, finally forms oxide ceramic coating at surface of Nd-Fe-B permanent magnet；
Described acid solution is nitric acid, and concentration mass fraction is 2～20%, and pickling time is 10～180 seconds；
It is sodium aluminate system, potassium fluorozirconate system or potassium fluotitanate system that described differential arc oxidation processes the electrolyte adopted；The dutycycle that described differential arc oxidation processes the positive pulse voltage used to be 300 ~ 500V, negative pulse voltage be 10 ~ 200V, positive negative pulse stuffing operating frequency is 30 ~ 3000Hz and positive negative pulse stuffing processes 5 ~ 90min when being 5～50%.
2. the preparation method of sintered Nd-Fe-B permanent magnet surface ceramic coat according to claim 1, it is characterized in that described electrolyte is sodium aluminate system, namely the mixed liquor that sodium aluminate and potassium dihydrogen phosphate are prepared with deionized water for solvent, its concentration respectively 10～30 g/l and 0.1 ~ 10 g/l.
3. the preparation method of sintered Nd-Fe-B permanent magnet surface ceramic coat according to claim 1, it is characterized in that described electrolyte is potassium fluorozirconate system, namely the mixed liquor that potassium fluorozirconate and phosphoric acid are prepared with deionized water for solvent, its concentration respectively 10～30 g/l and 5 ~ 20 g/l.
4. the preparation method of sintered Nd-Fe-B permanent magnet surface ceramic coat according to claim 1, it is characterized in that described electrolyte is potassium fluotitanate system, namely the mixed liquor that potassium fluotitanate and dipotassium hydrogen phosphate are prepared with deionized water for solvent, its concentration respectively 5～10 g/l and 5 ~ 10 g/l.
5. the preparation method of sintered Nd-Fe-B permanent magnet surface ceramic coat according to claim 1, it is characterized in that described differential arc oxidation processes as adopting bidirectional pulse mao power source, with neodymium iron boron for positive pole, with stainless steel electrolytic groove for negative pole, and to control electrolyte temperature be 10～40 DEG C.
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| CN104120377B (en) * | 2014-07-25 | 2017-03-15 | 北京航空航天大学 | A kind of method that adopts detonation flame spraying to prepare Al coating on sintered Nd Fe B surface |
| CN105420669B (en) * | 2015-11-29 | 2018-02-02 | 中国人民解放军装甲兵工程学院 | A kind of CVD method for permanent magnet anti-corrosion pre-treatment |
| CN106245026B (en) * | 2016-08-31 | 2018-11-23 | 安徽大地熊新材料股份有限公司 | A method of metal coating is prepared on Sintered NdFeB magnet surface |
| CN107937879B (en) * | 2017-11-30 | 2020-08-25 | 金力永磁(宁波)科技有限公司 | Neodymium-iron-boron magnet and surface coating method thereof |
| CN108754424A (en) * | 2018-06-11 | 2018-11-06 | 安徽大地熊新材料股份有限公司 | A kind of preparation method of corrosion-resistant sintered Nd-Fe-B permanent magnet of the surface with Al-base ceramic composite coating |
| CN111073466B (en) * | 2019-12-20 | 2021-04-30 | 浙江中杭新材料科技有限公司 | Preparation method of low-cost high-corrosion-resistance neodymium iron boron |
| CN111926366B (en) * | 2020-08-18 | 2023-03-31 | 南昌航空大学 | Sintered neodymium-iron-boron magnet surface corrosion-resistant coating and preparation method thereof |
| CN113005440A (en) * | 2020-12-30 | 2021-06-22 | 昆明狴犴人力资源服务有限公司 | Neodymium-iron-boron permanent magnet surface coating and preparation method thereof |
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| RU2086713C1 (en) * | 1995-07-11 | 1997-08-10 | Федорова Людмила Петровна | Thin-layer ceramic coating and method of manufacturing thereof |
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| CN1900361A (en) * | 2006-07-14 | 2007-01-24 | 西南大学 | Process for preparing neodymium-iron-boron permanent magnetic material surface gradient function coating layer |
| CN101029389A (en) * | 2007-04-12 | 2007-09-05 | 北京中科三环高技术股份有限公司 | Surface protection of neodymium iron boron permanent-magnet material |
| CN102400189A (en) * | 2010-09-10 | 2012-04-04 | 北京中科三环高技术股份有限公司 | Surface treatment method for neodymium iron boron permanent magnetic material by organic aluminum plating |
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