CN107116211B - NdFeB magnetic powder surface oxidation-resistant processing method - Google Patents

NdFeB magnetic powder surface oxidation-resistant processing method Download PDF

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CN107116211B
CN107116211B CN201710167798.2A CN201710167798A CN107116211B CN 107116211 B CN107116211 B CN 107116211B CN 201710167798 A CN201710167798 A CN 201710167798A CN 107116211 B CN107116211 B CN 107116211B
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magnetic powder
solution
spray evaporation
ndfeb magnetic
ndfeb
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CN107116211A (en
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雷成龙
曹江平
唐少龙
都有为
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JIANGSU JUXIN MAGNET CO Ltd
HAIAN INSTITUTE OF HIGH-TECH RESEARCH NANJING UNIVERSITY
Nanjing University
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JIANGSU JUXIN MAGNET CO Ltd
HAIAN INSTITUTE OF HIGH-TECH RESEARCH NANJING UNIVERSITY
Nanjing University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14Treatment of metallic powder
    • B22F1/145Chemical treatment, e.g. passivation or decarburisation
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Hard Magnetic Materials (AREA)
  • Soft Magnetic Materials (AREA)

Abstract

This application discloses a kind of NdFeB magnetic powder surface oxidation-resistant processing methods, comprising steps of (1), using spray evaporation mode to NdFeB magnetic powder carry out pre-oxidation treatment, spray evaporation solution be 1~2wt.% of mass concentration dichromate solution, mass concentration 3~5wt.% phosphoric acid solution mixed liquor;(2), secondary treatment is carried out using NdFeB magnetic powder of the spray evaporation mode to pre-oxidation, spray evaporation solution is 1~5wt.% solution of sodium bisulfite;(3), NdFeB magnetic powder is post-processed using spray evaporation mode, spray evaporation solution is sodium hydroxide solution;(4), it dries, obtains the ultra-fine NdFeB permanet magnetic powder that surface has fine and close oxygen-proof film.The present invention realizes efficiently quickly magnetic powder surface modification processing using spray evaporation device, the composite membrane of formation is comparatively dense and uniform, the burr and corner angle of super-fine magnetic powder are eliminated by preoxidation process, the mobility and apparent density for increasing neodymium iron boron super-fine magnetic powder, improve the inoxidizability of neodymium iron boron super-fine magnetic powder.

Description

NdFeB magnetic powder surface oxidation-resistant processing method
Technical field
This application involves the process of surface treatment of magnetic material, at a kind of NdFeB magnetic powder surface oxidation-resistant Reason method.
Background technique
The characteristics of nd-fe-b permanent magnetic alloy powder is: magnetic property is good, and mechanical property is good, but Curie temperature Tc is low, and temperature is stablized Property is poor, and chemical inoxidizability is bad, therefore limits its application range.The premise of iron B permanent magnetic material application is to first have to solve Certainly anti-oxidation, the Anticorrosion of good material.Rare earth element especially in Nd Fe B alloys powder, property is active, makes entire neodymium The antioxygenic property of iron boron magnetic powder becomes very poor, the easily oxidation and rusting in damp and hot environment.In addition, Nd-Fe-B permanent magnet material Magnetic property and its institutional framework have very big relationship, and the main phase of Nd-Fe-B permanent magnet is the main source of magnet magnetic property, wherein Maximum to coercivity contribution is Nd-rich phase.After Nd-Fe-B permanent magnet material aoxidizes, the magnetic property of material will occur huge Big variation.The decline or damage of magnetic property, have seriously affected neodymium iron boron forever caused by Nd-Fe-B permanent magnet fails because of oxidation peeling The service life of magnet reduces the stability and reliability of product.Therefore, the inoxidizability problem one of Nd-Fe-B permanent magnet material It is directly the main problem that Nd-Fe-B permanent magnet material needs to solve.At present, anti-oxidant, the anti-corrosion method of Nd-Fe-B permanent magnet material have very It is more.Wherein have galvanoplastic (CN1421547A), phosphorization filming method (105803443 A of CN), the modified organic coated method (CN in surface 105788793 A), a variety of methods such as preoxidation (105478787 A of CN).But wherein galvanoplastic higher cost, environment Pollution is big.Although traditional Nd-Fe-B permanent magnetic super-fine magnetic powder surface oxidation-resistant method effect is preferable, inefficiency, it is more difficult to control table Face modification process.
Summary of the invention
The purpose of the present invention is to provide a kind of NdFeB magnetic powder surface oxidation-resistant processing methods, to overcome in the prior art Deficiency.
To achieve the above object, the invention provides the following technical scheme:
The embodiment of the present application discloses a kind of NdFeB magnetic powder surface oxidation-resistant processing method, comprising steps of
(1), pre-oxidation treatment is carried out to NdFeB magnetic powder using spray evaporation mode, spray evaporation solution is mass concentration The mixed liquor of 1~2wt.% dichromate solution, mass concentration 3~5wt.% phosphoric acid solution;
(2), secondary treatment is carried out using NdFeB magnetic powder of the spray evaporation mode to pre-oxidation, spray evaporation solution is 1 ~5wt.% solution of sodium bisulfite;
(3), NdFeB magnetic powder is post-processed using spray evaporation mode, spray evaporation solution is that sodium hydroxide is molten Liquid;
(4), it dries, obtains the ultra-fine NdFeB permanet magnetic powder that surface has fine and close oxygen-proof film.
Preferably, in above-mentioned NdFeB magnetic powder surface oxidation-resistant processing method, in the step (1), spray evaporation In the process, the environment temperature for controlling NdFeB magnetic powder is 50 DEG C -60 DEG C, relative humidity 50%-80%.
Preferably, in above-mentioned NdFeB magnetic powder surface oxidation-resistant processing method, in the step (2), spray evaporation In the process, pH=9~10 that moisture is controlled by adjusting evaporation rate, the environment temperature for controlling NdFeB magnetic powder is 50~60 DEG C, relative humidity 60~80%.
Preferably, in above-mentioned NdFeB magnetic powder surface oxidation-resistant processing method, in the step (4), drying temperature It is 80~90 DEG C, drying time is 25~45min.
Preferably, in above-mentioned NdFeB magnetic powder surface oxidation-resistant processing method, in the step (1) and step (2), NdFeB magnetic powder is tiled on a moving belt and with 0.3~0.5m/min with certain thickness by spray evaporation room.
Preferably, in above-mentioned NdFeB magnetic powder surface oxidation-resistant processing method, NdFeB magnetic powder is flat with 1-2mm thickness Paving is on a moving belt.
Compared with the prior art, the advantages of the present invention are as follows: the present invention is realized efficiently quickly using spray evaporation device Magnetic powder surface modification processing, the composite membrane of formation is comparatively dense and uniform, eliminates super-fine magnetic powder by preoxidation process Burr and corner angle increase the mobility and apparent density of neodymium iron boron super-fine magnetic powder, improve the antioxygen of neodymium iron boron super-fine magnetic powder The property changed.
Specific embodiment
The present invention is described further by the following example: according to following embodiments, the present invention may be better understood. However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described in embodiment are only used In illustrating the present invention, without the present invention described in detail in claims should will not be limited.
Embodiment 1
Nd-Fe-B permanent magnetic 10um or so superfine powder is tiled on a moving belt with 1mm thickness, and with 0.5m/min by spraying Vaporization chamber, oxidizing temperature are 60 DEG C, relative humidity 80%, and spray evaporation solution is composite solution, and solution includes mass concentration 2wt.% dichromate solution and mass concentration 3wt.% phosphoric acid solution;Gained pre-oxidation neodymium iron boron super-fine magnetic powder again with The tiling of 1mm thickness passes through spray evaporation room on a moving belt with 0.5m/min, at this point, the solution of spray evaporation is 1~5wt.% Solution of sodium bisulfite, and increase a spray evaporator for sodium hydroxide solution spray evaporation in evaporation chamber outlet end, lead to The PH=9 of evaporation rate control moisture is overregulated, temperature is 50 DEG C, relative humidity 80%;Last neodymium iron boron super-fine magnetic powder passes through Conveyer belt, which is sent into drying room, dries, and drying temperature is 90 DEG C, drying time 25min, vibrates sub-sieve in next step, will meet grain Degree requires and is that dry powder is fallen into collector to get the ultra-fine NdFeB permanet magnetic powder with fine and close oxygen-proof film.
Embodiment 2
Nd-Fe-B permanent magnetic 20-40um or so fine powder is tiled on a moving belt with 1.5mm thickness, and with 0.4m/min by spraying Mist vaporization chamber, oxidizing temperature are 60 DEG C, relative humidity 80%, and spray evaporation solution is composite solution, and solution includes mass concentration 1wt.% dichromate solution quality and quantity concentration 4wt.% phosphoric acid solution;Gained pre-oxidation neodymium iron boron super-fine magnetic powder again with The tiling of 1mm thickness passes through spray evaporation room on a moving belt with 0.5m/min, at this point, the solution of spray evaporation is a certain amount of sulfurous Sour hydrogen sodium solution, and increase a spray evaporator for sodium hydroxide solution spray evaporation in evaporation chamber outlet end, pass through adjusting Evaporation rate controls the PH=10 of moisture, and temperature is 60 DEG C, relative humidity 70%;Last neodymium iron boron super-fine magnetic powder passes through conveyer belt It is sent into drying room and dries, drying temperature is 80 DEG C, drying time 30min, vibrates sub-sieve in next step, will meet granularity requirements It and is that dry powder is fallen into collector to get the ultra-fine NdFeB permanet magnetic powder with fine and close oxygen-proof film.
Finally, it is to be noted that, the terms "include", "comprise" or its any other variant be intended to it is non-exclusive Property include so that include a series of elements process, method, article or equipment not only include those elements, but also Further include other elements that are not explicitly listed, or further include for this process, method, article or equipment it is intrinsic Element.

Claims (5)

1. a kind of NdFeB magnetic powder surface oxidation-resistant processing method, which is characterized in that comprising steps of
(1), using spray evaporation mode to NdFeB magnetic powder carry out pre-oxidation treatment, spray evaporation solution be mass concentration 1~ The mixed liquor of 2wt.% dichromate solution, mass concentration 3~5wt.% phosphoric acid solution;
(2), secondary treatment being carried out to the NdFeB magnetic powder of pre-oxidation using spray evaporation mode, spray evaporation solution is 1~ 5wt.% solution of sodium bisulfite;
(3), NdFeB magnetic powder is post-processed using spray evaporation mode, spray evaporation solution is sodium hydroxide solution;
(4), it dries, obtains the ultra-fine NdFeB permanet magnetic powder that surface has fine and close oxygen-proof film.
2. NdFeB magnetic powder surface oxidation-resistant processing method according to claim 1, it is characterised in that: the step (1) In, during spray evaporation, the environment temperature for controlling NdFeB magnetic powder is 50 DEG C -60 DEG C, relative humidity 50%-80%.
3. NdFeB magnetic powder surface oxidation-resistant processing method according to claim 1, it is characterised in that: the step (2) In, during spray evaporation, pH=9~10 of moisture are controlled by adjusting evaporation rate, control the environment temperature of NdFeB magnetic powder Degree is 50~60 DEG C, relative humidity 60~80%.
4. NdFeB magnetic powder surface oxidation-resistant processing method according to claim 1, it is characterised in that: the step (4) In, drying temperature is 80~90 DEG C, and drying time is 25~45min.
5. NdFeB magnetic powder surface oxidation-resistant processing method according to claim 1, it is characterised in that: the step (1) In step (2), NdFeB magnetic powder is tiled on a moving belt and with 0.3~0.5m/min with 1-2mm thickness by spray evaporation Room.
CN201710167798.2A 2017-03-21 2017-03-21 NdFeB magnetic powder surface oxidation-resistant processing method Active CN107116211B (en)

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CN111362681B (en) * 2019-12-11 2021-09-17 横店集团东磁股份有限公司 High-performance permanent magnetic ferrite magnet sintered after injection molding and preparation method thereof
CN111370198B (en) * 2019-12-20 2021-08-20 横店集团东磁股份有限公司 Injection-molded soft magnetic ferrite magnet and preparation method thereof
CN111370216B (en) * 2020-03-12 2021-10-01 江苏巨鑫磁业有限公司 Oxidation resisting method for omnibearing film attachment on surface of magnetic powder particles
CN114101687A (en) * 2021-12-07 2022-03-01 鞍山安特磁材有限公司 Novel pressure-resistant magnetic powder
CN116511497A (en) * 2023-03-23 2023-08-01 江苏巨鑫磁业有限公司 Magnetic powder surface antioxidation processing device

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CN1085963A (en) * 1993-11-03 1994-04-27 胡景云 The swimming of neodymium-iron-boron magnetic material cathode of surface applies production technique
CN1528952A (en) * 2003-09-27 2004-09-15 沈阳工业学院 Neodymium-iron-boron magnet zinc plating and cathode electrophoresis composite protection process
JP5016513B2 (en) * 2008-02-07 2012-09-05 テイカ株式会社 Insulating film-forming metal powder using peelable double hydroxide and method for producing the same
CN102464902B (en) * 2010-11-16 2015-11-25 北京中科三环高技术股份有限公司 A kind of surface treatment method of chromium spelter coating of Nd-Fe-Bo permanent magnet material
CN105478787A (en) * 2015-12-03 2016-04-13 江苏巨鑫磁业有限公司 Oxidization method of rapidly-quenched bonded neodymium iron boron (NdFeB) permanent magnet powder

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