CN105839045A - Method for improving anticorrosion performance of sintered neodymium-iron-boron magnet - Google Patents

Method for improving anticorrosion performance of sintered neodymium-iron-boron magnet Download PDF

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Publication number
CN105839045A
CN105839045A CN201610237819.9A CN201610237819A CN105839045A CN 105839045 A CN105839045 A CN 105839045A CN 201610237819 A CN201610237819 A CN 201610237819A CN 105839045 A CN105839045 A CN 105839045A
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CN
China
Prior art keywords
nitrogen
iron
boron magnet
neodymium
magnet
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610237819.9A
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Chinese (zh)
Inventor
王亮
王波
严辉
宋雪梅
王如志
张铭
侯育冬
朱满康
刘晶冰
汪浩
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Beijing University of Technology
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Beijing University of Technology
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Priority to CN201610237819.9A priority Critical patent/CN105839045A/en
Publication of CN105839045A publication Critical patent/CN105839045A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • C23C8/24Nitriding
    • C23C8/26Nitriding of ferrous surfaces
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/02Pretreatment of the material to be coated

Abstract

The invention provides a method for improving the anticorrosion performance of a sintered neodymium-iron-boron magnet and belongs to the field of rare earth magnetic materials and surface treatment. The method includes the steps that pretreatment is performed, and the neodymium-iron-boron magnet is polished and cleaned; the pre-treated neodymium-iron-boron magnet is put into a vacuum furnace to be sealed, vacuumizing is performed through a vacuum pump, 0.1 Mpa to 0.2 Mpa of nitrogen is injected when the air pressure in the furnace drops below 20 pa, then vacuumizing is performed, the operation is performed for 2 to 3 times, and gas washing is performed; and then the temperature of the vacuum furnace is increased, nitrogen is injected after the temperature reaches 400 DEG C to 750 DEG C, the pressure of nitrogen is maintained within the range of 1*10<3> pa to 1*10<5> pa, the treatment time is controlled to be within the range of 2 h to 24 h, natural cooling in the furnace is performed after anticorrosion treatment is completed, and a compound anticorrosion layer containing the nitrogen element is generated on the surface of the magnet, wherein the thickness of the compound anticorrosion layer ranges from 1 micrometer to 50 micrometers. By the adoption of the method for improving the anticorrosion performance of the sintered neodymium-iron-boron magnet, operation is easy, pollution is avoided, the treated neodymium-iron-boron magnet is high in anticorrosion performance, and the method is suitable for mass production and is no limitations on sizes and shapes of magnets.

Description

A kind of method improving Sintered NdFeB magnet antiseptic property
Technical field
The invention belongs to rareearth magnetic material and field of surface treatment, particularly relate to a kind of raising Sintered NdFeB magnet The method of antiseptic property.
Background technology
Neodymium iron boron is as third generation rare-earth permanent magnet material, owing to having the magnetic property of excellence and good machining characteristics, It is widely used in many technical fields such as Aero-Space, microwave communication, motor, wind-power electricity generation and automobile.But this kind of forever Magnet poor chemical stability, the most oxidizable, serious electrochemical corrosion can occur under humid conditions, Deteriorate magnetic property and affect the service life of magnet.
At present, the method for the antiseptic property improving neodymium iron boron magnetic body mainly adds alloying element and surface processes, and adds and closes Gold element can improve magnet corrosion stability on certain Cheng Du, but due to the addition of alloying element, Partial Elements can be dissolved in neodymium In iron boron magnet principal phase, the magnetic property of infringement magnet.Surface treatment method is to improve Sintered NdFeB magnet antiseptic property Important channel, main process technique has the process of surface treatment such as plating, chemical plating, spraying and vacuum ion plating, but There is obvious shortcoming in these techniques, there is wall and corner effect during galvanoplastic plating, and thickness of coating is uneven, and defect is many, no It is suitable for having deep hole, complicated part;Chemical plating is similar to plating, and coating is poor with basal body binding force, and easy peeling comes off also And can produce substantial amounts of sewage, and the harm of intractability height is big;When spraying process is for processing the magnet of small volume, difficulty is high, Paint waste is serious, and these protective layers there is also the problem such as loosely of the combination with magnet, once protective layer part or complete Portion comes off, and its decay resistance will decline rapidly;Although vacuum ion plating can improve the adhesion of coating and matrix, But it is big to there is equipment investment in this technique, and production efficiency is low, it is impossible to the shortcoming processing complex parts.
Summary of the invention
It is an object of the invention to provide a kind of method improving Sintered NdFeB magnet antiseptic property, the method is simple to operate, Pollution-free, and the neodymium iron boron magnetic body decay resistance processed is strong.The present invention is achieved through the following technical solutions:
A kind of method improving Sintered NdFeB magnet antiseptic property, comprises the following steps:
The first step: pretreatment, carries out neodymium iron boron magnetic body polishing, cleaning;
Second step: preservative treatment, is placed in heat treated under blanket of nitrogen, Surface Creation one layer by neodymium iron boron magnetic body Anti-corrosion layer.
A kind of described method improving Sintered NdFeB magnet antiseptic property, pretreatment is polished on 800~2000 mesh sand paper Carrying out, first use acetone soln ultrasonic cleaning after polishing, followed in turn by dehydrated alcohol ultrasonic cleaning, nitrogen dries up standby.
A kind of described method improving Sintered NdFeB magnet antiseptic property, anticorrosion treatment technology is, pretreated Neodymium iron boron magnetic body is put into vacuum drying oven and is sealed, and by vacuum pump extracting vacuum, when stove internal gas pressure drops to below 20pa, is filled with 0.1~0.2Mpa nitrogen, then evacuation, carry out gas washing 2~3 times the most repeatedly.Then heating up vacuum drying oven, temperature reaches After 400~750 DEG C, being filled with nitrogen, its pressure is maintained at 1 × 103~1 × 105The scope of pa, the process time controls 2~24h, Making nitrogen react with top layer neodymium iron boron, forming thickness is the compound that 1~50 μm contain nitrogen element.After preservative treatment to be done, Constant at holding furnace intracavity nitrogen pressure or again furnace chamber can be carried out furnace cooling on the basis of evacuation process.
Compared with prior art, the invention has the advantages that: simple to operate, the size and shape for magnet does not limit, It is suitable for batch production, and nitrogen can be passed through in NbFeB sintered end temperature-fall period carries out preservative treatment, save energy Source, pollution-free, and the neodymium iron boron magnetic body decay resistance processed is strong.
Detailed description of the invention
Below in conjunction with being embodied as, the present invention will be further described in detail:
Embodiment 1: select the iron boron magnet not magnetized, uses following methods to carry out this neodymium iron boron magnetic body at surface anticorrosion Reason, improves its decay resistance.
A kind of method improving Sintered NdFeB magnet antiseptic property, comprises the following steps:
The first step: pretreatment: polish on 800 mesh sand paper, first uses acetone soln ultrasonic cleaning, subsequently after polishing Using dehydrated alcohol ultrasonic cleaning again, nitrogen dries up standby.
Second step: preservative treatment: pretreated neodymium iron boron magnetic body is put into vacuum drying oven and seals, extracted by vacuum pump Vacuum, when stove internal gas pressure drops to 10pa, is filled with 0.15Mpa nitrogen, then evacuation, the most repeatedly carries out gas washing 3 times. Then vacuum drying oven is heated up, after temperature reaches 500 DEG C, be filled with nitrogen so that it is pressure is maintained at 2 × 104Pa, processes the time For 24h.After completing preservative treatment, furnace cooling on the basis of holding furnace intracavity nitrogen pressure is constant.
Corrosion-resistant test experiments illustrates that this technique can make neodymium iron boron magnetic body decay resistance significantly improve: under room temperature, 0.5mol/L H2SO410 × 10 × 10mm in solution3Sample etches rate test result is as follows:
Embodiment 2: select the iron boron magnet not magnetized, uses following methods to carry out this neodymium iron boron magnetic body at surface anticorrosion Reason, improves its decay resistance.
A kind of method improving Sintered NdFeB magnet antiseptic property, comprises the following steps:
The first step: pretreatment: polish on 1500 mesh sand paper, first uses acetone soln ultrasonic cleaning after polishing, with After use dehydrated alcohol ultrasonic cleaning again, nitrogen dries up standby.
Second step: preservative treatment: pretreated neodymium iron boron magnetic body is put into vacuum drying oven and seals, extracted by vacuum pump Vacuum, when stove internal gas pressure drops to 20pa, is filled with 0.2Mpa nitrogen, then evacuation, the most repeatedly carries out gas washing 2~3 times. Then vacuum drying oven is heated up, after temperature reaches 400 DEG C, be filled with nitrogen so that it is pressure is maintained at 1 × 105Pa, processes the time For 12h, after completing preservative treatment, furnace cooling on the basis of holding furnace intracavity nitrogen pressure is constant.
Under room temperature, at 0.5mol/L H2SO410 × 10 × 10mm in solution3Sample weight loss rate test result is as follows:

Claims (3)

1. the method improving Sintered NdFeB magnet antiseptic property, it is characterised in that include following Step:
The first step: pretreatment
Carry out neodymium iron boron magnetic body polishing, cleaning;
Second step: preservative treatment
Pretreated neodymium iron boron magnetic body is put into vacuum drying oven seal, by vacuum pump extracting vacuum, When stove internal gas pressure drops to below 20pa, it is filled with 0.1~0.2Mpa nitrogen, then evacuation, the most repeatedly Carry out gas washing 2~3 times;Then vacuum drying oven is heated up, after temperature reaches 400~750 DEG C, is filled with nitrogen, Its pressure is made to be maintained at 1 × 103~1 × 105The scope of pa, the process time controls 2~24h, to be done anti- After rotten process, furnace cooling, one layer of anti-corrosion layer of Surface Creation.
A kind of method improving Sintered NdFeB magnet antiseptic property the most according to claim 1, It is characterized in that: pretreatment is, polishing is carried out on 800~2000 mesh sand paper, first uses acetone after polishing Solution ultrasonic cleaning, followed in turn by dehydrated alcohol ultrasonic cleaning, nitrogen dries up standby.
A kind of method improving Sintered NdFeB magnet antiseptic property the most according to claim 1, It is characterized in that: the anti-corrosion layer thickness of formation is 1~50 μm.
CN201610237819.9A 2016-04-17 2016-04-17 Method for improving anticorrosion performance of sintered neodymium-iron-boron magnet Pending CN105839045A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110983395A (en) * 2019-12-17 2020-04-10 广东小天才科技有限公司 Magnet, preparation method and wearable device
CN111755236A (en) * 2020-06-23 2020-10-09 安泰科技股份有限公司 Bluing anti-corrosion method for sintered neodymium-iron-boron magnet
CN112786301A (en) * 2020-12-30 2021-05-11 包头天和磁材科技股份有限公司 Corrosion-resistant neodymium-iron-boron magnet, surface treatment method and application of hydroxyl compound
CN114875353A (en) * 2022-04-27 2022-08-09 宁波同创强磁材料有限公司 Preparation method of high-corrosion-resistance sintered neodymium-iron-boron magnet

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06145705A (en) * 1992-11-11 1994-05-27 Seiko Epson Corp Rare earth magnet powder, rare earth bond magnet and composition for rare earth bond magnet
CN1103987A (en) * 1993-12-17 1995-06-21 陶一飞 Method for mfg. micro crystalline magnetic powder
WO2003034451A1 (en) * 2001-10-15 2003-04-24 Kabushiki Kaisha Toshiba Bonded magnet and method for production thereof
CN202948803U (en) * 2012-08-20 2013-05-22 烟台正海磁性材料股份有限公司 Neodymium iron boron magnetic body
CN103956244A (en) * 2014-05-14 2014-07-30 辽宁五寰科技发展有限公司 Preparation method for high-coercivity sintered neodymium-iron-boron

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06145705A (en) * 1992-11-11 1994-05-27 Seiko Epson Corp Rare earth magnet powder, rare earth bond magnet and composition for rare earth bond magnet
CN1103987A (en) * 1993-12-17 1995-06-21 陶一飞 Method for mfg. micro crystalline magnetic powder
WO2003034451A1 (en) * 2001-10-15 2003-04-24 Kabushiki Kaisha Toshiba Bonded magnet and method for production thereof
CN202948803U (en) * 2012-08-20 2013-05-22 烟台正海磁性材料股份有限公司 Neodymium iron boron magnetic body
CN103956244A (en) * 2014-05-14 2014-07-30 辽宁五寰科技发展有限公司 Preparation method for high-coercivity sintered neodymium-iron-boron

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110983395A (en) * 2019-12-17 2020-04-10 广东小天才科技有限公司 Magnet, preparation method and wearable device
CN111755236A (en) * 2020-06-23 2020-10-09 安泰科技股份有限公司 Bluing anti-corrosion method for sintered neodymium-iron-boron magnet
CN112786301A (en) * 2020-12-30 2021-05-11 包头天和磁材科技股份有限公司 Corrosion-resistant neodymium-iron-boron magnet, surface treatment method and application of hydroxyl compound
CN114875353A (en) * 2022-04-27 2022-08-09 宁波同创强磁材料有限公司 Preparation method of high-corrosion-resistance sintered neodymium-iron-boron magnet
CN114875353B (en) * 2022-04-27 2024-03-19 宁波同创强磁材料有限公司 Preparation method of high-corrosion-resistance sintered NdFeB magnet

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Application publication date: 20160810