CN103556208B - The electro-deposition method of a kind for the treatment of agent for the formation of rare earth hydride particulate coating and formation coating - Google Patents
The electro-deposition method of a kind for the treatment of agent for the formation of rare earth hydride particulate coating and formation coating Download PDFInfo
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Abstract
For the formation of the treatment agent of rare earth hydride particulate coating and an electro-deposition method for formation coating, belong to technical field of magnetic materials.Be dispersed with rare earth hydride particle in dispersion agent, dispersion agent is normal hexane or normal heptane, and rare earth is at least one in Pr, Nd, Tb, Dy, Ho.Adopt electro-deposition method to be deposited to by above-mentioned hydride particle to be formed evenly on sintered Nd Fe B rare-earth magnet surface, the fine and close and coating that thickness is controlled.Rare earth hydride particulate coating obviously can improve the coercive force of the magnetic property, particularly magnet of sintered Nd Fe B rare-earth magnet.Adopt the inventive method under ensureing that magnet has the prerequisite of good magnetic property, the usage quantity of heavy rare earths in sintered Nd Fe B rare earth can be reduced, thus reduce the manufacturing cost of high-coercivity magnet.
Description
Technical field
The present invention relates to a kind of novel method forming rare earth hydride particulate coating, the present invention, for improving sintered NdFeB (NdFeB) magnet institute coercive force, belongs to technical field of magnetic materials.
Background technology
Sintered Nd Fe B is the permanent magnet material that magnetic is the strongest up to now, and being widely used in the numerous areas such as electronics, electromechanics, instrument and medical treatment, is with fastest developing speed in the world today, the permanent magnet material that market outlook are best.But the temperature stability of sintered Nd Fe B is poor, working temperature is usually less than 100 DEG C, is therefore greatly limited in the application in the fields such as high-temperature electric machine.In recent years, hybrid vehicle (HEV) is developed rapidly because of the advantage of its energy-saving and environmental protection, and the permanent-magnet machine as key part wherein proposes urgent demand to sintered Nd Fe B again from quantity and temperature stability (working temperature more than 200 DEG C) two aspects.National governments, relevant enterprise and investigator are also to this extensive concern.
At present, by adding more Dy or Tb in sintered NdFeB magnet, the coercive force of alloy can be significantly improved, and then improve the temperature profile of alloy.Although this is a kind of effective way having realized industrialization, there is following deficiency: first, due to the saturation magnetization adding membership loss magnet of Dy or Tb, thus cause the decline of magnet remanent magnetism and magnetic energy product.Secondly, due to Dy and Tb scarcity of resources, price, far above Nd element, therefore can cause the significantly raising of alloy raw material cost.
To this, the present inventor invents a kind of method of heat-treating in magnet surface formation rare earth hydride nanoparticle coating and to coating magnet early stage.Specifically nano particle is formed solution, be then dipped into by magnet in taking-up in solution, surface forms particulate coating.Then the magnet after coating is heat-treated.Adopt this patented technology effectively can improve the coercive force increase rate of the comprehensive magnetic energy, particularly magnet of magnet obviously (this patent is authorized at present, patent No. ZL201210241737.4).But this invention exists 2 deficiencies technically: first, this technology is difficult to manipulation for the thickness of hydride nano-particle coating and distributing homogeneity, therefore causes coating effect unstable, and then has influence on the magnetic property of final magnet.The second, this technology is manual operation, and working efficiency is low.In other words, foregoing invention technology is only limited to the short run research of laboratory scope, wants to realize this technological industrialization, new method must be adopted to prepare even compact, the coating that surface quality is good, and be enhanced productivity by Automated condtrol.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the application proposes the new technology being formed rare earth hydride coating by electro-deposition method on Sintered NdFeB magnet surface.First a kind for the treatment of agent for the formation of rare earth hydride coating is provided, is then formed evenly in magnet surface, the fine and close and rare earth hydride nanoparticle coating that thickness is regulatable.Finally, high magnetic characteristics Sintered NdFeB magnet is prepared by thermal treatment process.
Treatment agent for the formation of rare earth hydride particulate coating of the present invention, it is characterized in that, described treatment agent is be dispersed with rare earth hydride particle in dispersion agent, dispersion agent selected by treatment agent is normal hexane or normal heptane, described rare earth is Pr, Nd, Tb, Dy, at least one in Ho, the scope of the average particulate diameter of rare earth hydride is between 100-500 nanometer, preferred average particulate diameter is in 100-200 nanometer, above-mentioned rare earth hydride particle is mixed with normal hexane or normal heptane solvent, rare earth hydride is dispersed in normal hexane or normal heptane solvent uniformly and forms suspension liquid, dispersion liquid concentration 0.01-0.1g/ml, form the treatment agent being used for rare earth hydride particulate coating.
Of the present invention another to the effect that utilizes the above-mentioned treatment agent for the formation of rare earth hydride particulate coating, provides a kind of method forming rare earth hydride particulate coating on the body surface needing surface coated treatment.Adopt present method, the top coat comprising rare earth hydride particle can be added on the surface of reguline metal magnet, carry out secondary thermal treatment by magnet effects on surface having been formed rare earth hydride particulate coating, significantly can improve the coercive force of the magnetic property, particularly magnet of magnet.
Above-mentioned treatment agent is adopted to prepare the method forming rare earth hydride particulate coating, it is characterized in that, adopt the method for galvanic deposit, concrete steps comprise: be first ready for the treatment agent forming rare earth hydride top coat, treatment agent is inserted in galvanic deposition cell, and constantly stirring makes it to form suspension, to guarantee in galvanic deposition cell that concentration is everywhere consistent, neodymium iron boron magnetic body after surface finish is connected to negative electrode, anode adopts stainless steel substrates, neodymium iron boron magnetic body and stainless steel substrates are placed in treatment agent suspension and carry out galvanic deposit, rare earth hydride granular layer is obtained in neodymium-iron-boron surface, afterwards the magnet depositing rare earth hydride granular layer is taken out, air-dry, then with nickel foil, magnet is wrapped up, one-level thermal treatment is carried out at the temperature of 790 DEG C-870 DEG C, time 5-7 hour, and then at the temperature of 500 DEG C, carry out secondary thermal treatment, 3 hours time.
Above-mentioned galvanic deposit is preferred, and neodymium iron boron magnetic body glazed surface is just to stainless steel substrates, and the area of stainless steel substrates is slightly larger than neodymium iron boron magnetic body glazed surface area.Cathode and anode spacing controls at 1-5cm, preferred 2.5cm.Galvanic deposit voltage 50-300v, electric current 10-100mA, preferred voltage 150v, electric current 40mA, by the time (10-220 second) that galvanic deposit is different, forms the rare earth hydride particulate coating of different thickness.Cated magnet will be covered afterwards take out, the dispersion agent in air-dry coat.Significantly can improve the magnetic property of magnet after thermal treatment, particularly the coercive force of magnet be promoted obviously.
Magnet involved in the present invention is that the magnet of any material containing rare earth is as sintered NdFeB magnet.Each embodiment is neodymium iron boron magnetic body standby by electrodeposited coating legal system under different experimental conditions below, and the thickness (for hydrogenation dysprosium particle) of magnet surface coating is as shown in table 1 with the change of electrodeposition time.By testing every magnetic parameter of magnet after different process thermal treatment.Conveniently contrast, magnet raw magnetic before treatment can also provide (see table 2) in the lump.
Adopt electro-deposition method to be formed evenly on sintered Nd Fe B rare-earth magnet surface by above-mentioned hydride particle, the fine and close and coating that thickness is controlled.Described rare earth hydride particulate coating obviously can improve the coercive force of the magnetic property, particularly magnet of sintered Nd Fe B rare-earth magnet.Adopt the inventive method under ensureing that magnet has the prerequisite of good magnetic property, the usage quantity of heavy rare earths in sintered Nd Fe B rare earth can be reduced, thus reduce the manufacturing cost of high-coercivity magnet.
Embodiment
Below in conjunction with embodiment, the present invention will be further described, but the present invention is not limited to following examples.
Embodiment 1
By the n-heptane solution Homogeneous phase mixing of rare earth hydrogenation dysprosium particle 20g and the 1000ml of particle diameter 100 nanometer, hydrogenation dysprosium is dispersed in normal heptane uniformly, and concentration is consistent everywhere in electrolyzer to adopt induction stirring to guarantee, prepare the suspension liquid for the formation of hydrogenation dysprosium particulate coating, its concentration is 0.02g/ml(because the volume of gained suspension liquid and dispersion agent is basically identical, lower with).
Sintered NdFeB magnet (its magnetic property parameter is in table 2 No. 1 magnet) is prepared into the small pieces of physical dimension 10 × 10 × 3.5mm, and polished finish is carried out to its surface.Magnet after process is connected to negative electrode, the stainless steel substrates that anode adopts area to amass slightly larger than magnet right opposite, cathode and anode spacing controls at about 2.5cm, galvanic deposit voltage control is at 150v, galvanic deposit current control is at 40mA, and galvanic deposit is taken out air-dry after 180 seconds, is wrapped by magnet with nickel is thin.Afterwards, by being surrounded by the thin neodymium iron boron magnetic body of nickel, to be placed in vacuum tightness be 1 × 10
-4in the heat treatment furnace of Pa, one-level thermal treatment temp is 810 DEG C, 5 hours; Secondary thermal treatment temp is 500 DEG C, 3 hours.After process, the final magnetic property parameter of magnet is in table 2 No. 2 magnet.
Embodiment 2
By the n-heptane solution Homogeneous phase mixing of rare earth hydrogenation terbium particle 10g and the 1000ml of particle diameter 100 nanometer, hydrogenation terbium is dispersed in normal heptane uniformly, and concentration is consistent everywhere in electrolyzer to adopt induction stirring to guarantee, prepare the suspension liquid for the formation of hydrogenation terbium particulate coating, its concentration is 0.01g/ml.
Sintered NdFeB magnet (its magnetic property parameter is in table 2 No. 1 magnet) is prepared into the small pieces of physical dimension 10 × 10 × 3.5mm, and polished finish is carried out to its surface.Magnet after process is connected to negative electrode, the stainless steel substrates that anode adopts area to amass slightly larger than magnet right opposite, cathode and anode spacing controls at about 2.5cm, galvanic deposit voltage control is at 150v, galvanic deposit current control is at 40mA, and galvanic deposit is taken out air-dry after 220 seconds, is wrapped by magnet with nickel is thin.Afterwards, by being surrounded by the thin neodymium iron boron magnetic body of nickel, to be placed in vacuum tightness be 1 × 10
-4in the heat treatment furnace of Pa, one-level thermal treatment temp is 790 DEG C, 5 hours; Secondary thermal treatment temp is 500 DEG C, 3 hours.After process, the final magnetic property parameter of magnet is in table 2 No. 3 magnet.
Embodiment 3
By the n-heptane solution Homogeneous phase mixing of rare earth praseodymium hydride particle 60g and the 1000ml of particle diameter 150 nanometer, praseodymium hydride is dispersed in normal heptane uniformly, and concentration is consistent everywhere in electrolyzer to adopt induction stirring to guarantee, prepare the suspension liquid for the formation of praseodymium hydride particulate coating, its concentration is 0.06g/ml.
Sintered NdFeB magnet (its magnetic property parameter is in table 2 No. 1 magnet) is prepared into the small pieces of physical dimension 10 × 10 × 3.5mm, and polished finish is carried out to its surface.Magnet after process is connected to negative electrode, the stainless steel substrates that anode adopts area to amass slightly larger than magnet right opposite, cathode and anode spacing controls at about 2.5cm, galvanic deposit voltage control is at 150v, galvanic deposit current control is at 40mA, and galvanic deposit is taken out air-dry after 100 seconds, is wrapped by magnet with nickel is thin.Afterwards, by being surrounded by the thin neodymium iron boron magnetic body of nickel, to be placed in vacuum tightness be 1 × 10
-4in the heat treatment furnace of Pa, one-level thermal treatment temp is 870 DEG C, 7 hours; Secondary thermal treatment temp is 500 DEG C, 3 hours.After process, the final magnetic property parameter of magnet is in table 2 No. 4 magnet.
Embodiment 4
By the hexane solution Homogeneous phase mixing of rare earth neodymium hydride particle 80g and the 1000ml of particle diameter 150 nanometer, neodymium hydride is dispersed in normal hexane uniformly, and concentration is consistent everywhere in electrolyzer to adopt magnetic agitation to guarantee, prepare the suspension liquid for the formation of neodymium hydride particulate coating, its concentration is 0.08g/ml.
Sintered NdFeB magnet (its magnetic property parameter is in table 2 No. 1 magnet) is prepared into the small pieces of physical dimension 10 × 10 × 3.5mm, and polished finish is carried out to its surface.Magnet after process is connected to negative electrode, the stainless steel substrates that anode adopts area to amass slightly larger than magnet right opposite, cathode and anode spacing controls at about 2.5cm, galvanic deposit voltage control is at 150v, galvanic deposit current control is at 40mA, and galvanic deposit is taken out air-dry after 40 seconds, is wrapped by magnet with nickel is thin.Afterwards, by being surrounded by the thin neodymium iron boron magnetic body of nickel, to be placed in vacuum tightness be 1 × 10
-4in the heat treatment furnace of Pa, one-level thermal treatment temp is 850 DEG C, 6 hours; Secondary thermal treatment temp is 500 DEG C, 3h.After process, the final magnetic property parameter of magnet is in table 2 No. 5 magnet.
Embodiment 5
By the hexane solution Homogeneous phase mixing of rare earth hydrogenation holmium particle 100g and the 1000ml of particle diameter 200 nanometer, hydrogenation holmium is dispersed in normal hexane uniformly, and concentration is consistent everywhere in electrolyzer to adopt magnetic agitation to guarantee, prepare the suspension liquid for the formation of hydrogenation holmium particulate coating, its concentration is 0.1g/ml.
Sintered NdFeB magnet (its magnetic property parameter is in table 2 No. 1 magnet) is prepared into the small pieces of physical dimension 10 × 10 × 3.5mm, and polished finish is carried out to its surface.Magnet after process is connected to negative electrode, the stainless steel substrates that anode adopts area to amass slightly larger than magnet right opposite, cathode and anode spacing controls at about 2.5cm, galvanic deposit voltage control is at 150v, galvanic deposit current control is at 40mA, and galvanic deposit is taken out air-dry after 10 seconds, is wrapped by magnet with nickel is thin.Afterwards, by being surrounded by the thin neodymium iron boron magnetic body of nickel, to be placed in vacuum tightness be 1 × 10
-4in the heat treatment furnace of Pa, one-level thermal treatment temp is 830 DEG C, 7 hours; Secondary thermal treatment temp is 500 DEG C, 3h.After process, the final magnetic property parameter of magnet is in table 2 No. 6 magnet.
The coat-thickness that when table 1 treatment agent concentration 0.06g/ml, two interelectrode distance 2.5cm, galvanic deposit voltage 150v, electric current 40mA, different electrodeposition time obtains
| Time/second | 10 | 20 | 40 | 80 | 150 | 220 |
| Coat-thickness/μm | 138.96 | 166.48 | 169.77 | 274.08 | 415.71 | 452.10 |
Table 2
Claims (9)
1. the treatment agent of a rare earth hydride particle, it is characterized in that, described treatment agent is be dispersed with rare earth hydride particle in dispersion agent, and the dispersion agent selected by treatment agent is normal hexane or normal heptane, and described rare earth is at least one in Pr, Nd, Tb, Dy, Ho; The scope of the average particulate diameter of rare earth hydride is between 100-500 nanometer.
2. according to the treatment agent of a kind of rare earth hydride particle of claim 1, it is characterized in that, the average particulate diameter of rare earth hydride is in 100-200 nanometer.
3., according to the treatment agent of a kind of rare earth hydride particle of claim 1, it is characterized in that, treatment agent concentration 0.01-0.1g/ml.
4. be used for galvanic deposit according to the treatment agent of any one the rare earth hydride particle described in claim 1-3 and prepare rare earth hydride particulate coating.
5. adopt any one treatment agent described in claim 1-3 to prepare the method for rare earth hydride top coat, it is characterized in that, adopt the method for galvanic deposit, concrete steps comprise: be first ready for the treatment agent forming rare earth hydride top coat, treatment agent is inserted in galvanic deposition cell, and constantly stirring makes it to form suspension, neodymium iron boron magnetic body after surface finish is connected to negative electrode, anode adopts stainless steel substrates, neodymium iron boron magnetic body and stainless steel substrates are placed in treatment agent suspension and carry out galvanic deposit, obtain rare earth hydride granular layer in neodymium-iron-boron surface; Afterwards the magnet depositing rare earth hydride granular layer is taken out, air-dry, then with nickel foil, magnet is wrapped up, one-level thermal treatment is carried out at the temperature of 790 DEG C-870 DEG C, time 5-7 hour, and then at the temperature of 500 DEG C, carry out secondary thermal treatment, 3 hours time.
6. according to the method for claim 5, it is characterized in that, neodymium iron boron magnetic body glazed surface is just to stainless steel substrates, and the area of stainless steel substrates is slightly larger than neodymium iron boron magnetic body glazed surface area.
7. according to the method for claim 5, it is characterized in that, cathode and anode spacing controls at 1-5cm, galvanic deposit voltage 50-300V, electric current 10-100mA.
8. according to the method for claim 5, it is characterized in that, cathode and anode spacing 2.5cm, galvanic deposit voltage 150V, electric current 40mA.
9. according to the method for claim 5, it is characterized in that, electrodeposition time 10-220 second, form the rare earth hydride particulate coating of different thickness.
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| CN104036946A (en) * | 2014-06-11 | 2014-09-10 | 北京工业大学 | Method for using magnetic steel of waste permanent magnet motor to prepare high-performance high-coercivity regenerated sintered neodymium iron boron (NdFeB) magnet |
| CN104036945A (en) * | 2014-06-11 | 2014-09-10 | 北京工业大学 | Method for manufacturing high-temperature stable regenerated sintered neodymium-iron-boron magnet by waste permanent-magnet motor magnet steel |
| CN104036948A (en) * | 2014-06-11 | 2014-09-10 | 北京工业大学 | Method for using magnetic steel of waste permanent magnet motor to prepare high-performance regenerated sintered neodymium iron boron (NdFeB) magnet |
| CN104036949A (en) * | 2014-06-11 | 2014-09-10 | 北京工业大学 | Method for using bulk sintered neodymium iron boron (NdFeB) machining waste to prepare high-performance regenerated NdFeB magnet |
| CN106319441B (en) * | 2016-08-31 | 2019-07-30 | 浙江凯文磁业有限公司 | A kind of infiltration dysprosium technique improving neodymium iron boron performance |
| CN107492430A (en) * | 2017-08-09 | 2017-12-19 | 江西金力永磁科技股份有限公司 | A kind of neodymium iron boron magnetic body and preparation method thereof |
| CN108461272B (en) * | 2018-03-20 | 2020-05-22 | 北京工业大学 | Technology for forming hydride nanoparticle surface coating |
| CN108597840B (en) * | 2018-04-04 | 2020-07-03 | 北京工业大学 | Surface diffusion method and device for nano particles |
| CN110556243B (en) * | 2019-08-19 | 2021-07-02 | 安徽省瀚海新材料股份有限公司 | Neodymium iron boron surface dysprosium penetration method |
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| CN101908397A (en) * | 2010-07-30 | 2010-12-08 | 北京工业大学 | Rare earth hydride surface coating treating agent, application thereof and method for forming rare earth hydride surface coating |
| WO2012100863A1 (en) * | 2011-01-26 | 2012-08-02 | Robert Bosch Gmbh | Synthesis of magnetic composites |
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| CN101492830A (en) * | 2008-01-25 | 2009-07-29 | 中国科学院宁波材料技术与工程研究所 | Process for producing nano-composite plate of neodymium iron boron material |
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| WO2012100863A1 (en) * | 2011-01-26 | 2012-08-02 | Robert Bosch Gmbh | Synthesis of magnetic composites |
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