CN103556208A - Treating agent and electro-deposition method for forming rare earth hydride particle coating - Google Patents
Treating agent and electro-deposition method for forming rare earth hydride particle coating Download PDFInfo
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Abstract
The invention relates to a treating agent and an electro-deposition method for forming a rare earth hydride particle coating, and belongs to the technical field of magnetic materials. Rare earth hydride particles are dispersed in a dispersing agent, wherein n-hexane or n-heptane is taken as the dispersing agent; the rare earth is at least one element of Pr, Nd, Tb, Dy and Ho. The hydride particles are deposited on the surface of a sintered NdFeB rare earth magnet by using the electro-deposition method so as to form the uniform and dense coating with controllable thickness. The rare earth hydride particle coating can be used for obviously improving the magnetic property of the sintered NdFeB rare earth magnet and especially the coercivity of the magnet. As the method is adopted, the usage amounts of heavy rare earths in the sintered NdFeB rare earth is decreased on the premise of guaranteeing good magnetic property of the magnet, so that the manufacturing cost of the magnet with high coercivity is reduced.
Description
Technical field
The present invention relates to a kind of novel method that forms rare earth hydride particulate coating, the present invention is used for improving sintered NdFeB (NdFeB) magnet institute coercive force, belongs to technical field of magnetic materials.
Background technology
Sintered Nd Fe B is the strongest permanent magnet material of magnetic up to now, be widely used in the numerous areas ，Shi world todays such as electronics, electromechanics, instrument and medical treatment with fastest developing speed, 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 ℃, and therefore the application in fields such as high-temperature electric machines is greatly limited.In recent years, hybrid vehicle (HEV) is developed rapidly because of the advantage of its energy-saving and environmental protection, as the permanent-magnet machine of key part wherein, from quantity and temperature stability (working temperature is more than 200 ℃) two aspects, again sintered Nd Fe B has been proposed to urgent demand.National governments, relevant enterprise and investigator are also to this extensive concern.
At present, by add more Dy or Tb in sintered NdFeB magnet, can significantly improve the coercive force of alloy, and then improve the temperature profile of alloy.Although this is a kind of effective way that has realized industrialization, exist following deficiency: first, due to the saturation magnetization that adds membership loss magnet of Dy or Tb, thereby 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 inventor invents a kind of method that forms rare earth hydride nanoparticle coating and heat-treat applying magnet in magnet surface in earlier stage.Specifically nano particle is formed to solution, then magnet is dipped in solution and is taking out, surface forms particulate coating.Then the magnet after applying is heat-treated.Adopt this patented technology can effectively improve the coercive force increase rate obvious (this patent is authorized at present, patent No. ZL201210241737.4) of the comprehensive magnetic energy, particularly magnet of magnet.But there are 2 deficiencies in this invention technically: first, this technology is difficult to control for thickness and the distributing homogeneity of hydride nano-particle coating, therefore causes coating effect unstable, and then have 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 the industrialization of this technology, must adopt new method to prepare even compact, the coating that surface quality is good, and control and enhance productivity by automatization.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the application proposes to form on Sintered NdFeB magnet surface by electro-deposition method the new technology of rare earth hydride coating.First a kind for the treatment of agent that is used to form rare earth hydride coating is provided, then in magnet surface, forms evenly, densification and the regulatable rare earth hydride nanoparticle coating of thickness.Finally, by thermal treatment process, prepare high magnetic characteristics Sintered NdFeB magnet.
The treatment agent that is used to form rare earth hydride particulate coating of the present invention, it is characterized in that, described treatment agent is in dispersion agent, to be dispersed with rare earth hydride particle, the selected dispersion agent for the treatment of 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, preferably 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, be formed for the treatment agent of rare earth hydride particulate coating.
Of the present invention another to the effect that utilizes the above-mentioned treatment agent that is used to form rare earth hydride particulate coating, and a kind of method that forms rare earth hydride particulate coating on body surface needing top coat to process is provided.Adopt present method, can on the surface of reguline metal magnet, add the top coat that comprises rare earth hydride particle, by having formed the magnet of rare earth hydride particulate coating on effects on surface, carry out secondary thermal treatment, can significantly improve the coercive force of the magnetic property, particularly magnet of magnet.
Adopt above-mentioned treatment agent to prepare the method that forms 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 that forms rare earth hydride top coat, treatment agent is inserted in galvanic deposition cell, and constantly stir and make it to form suspension, 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 to treatment agent suspension and carry out galvanic deposit, in neodymium-iron-boron surface, obtain rare earth hydride granular layer, afterwards the magnet that deposits rare earth hydride granular layer is taken out, air-dry, then with nickel foil, magnet pack is wrapped, at the temperature of 790 ℃-870 ℃, carry out one-level thermal treatment, time 5-7 hour, and then at the temperature of 500 ℃, carry out secondary thermal treatment, 3 hours time.
Above-mentioned galvanic deposit is preferred, and neodymium iron boron magnetic body glazed surface is over against 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 is controlled at 1-5cm, preferably 2.5cm.Galvanic deposit voltage 50-300v, electric current 10-100mA, preferred voltage 150v, electric current 40mA, by the different time of galvanic deposit (10-220 second), forms the rare earth hydride particulate coating of different thickness.To cover afterwards cated magnet and take out, the dispersion agent in air-dry coat.After thermal treatment, can significantly improve the magnetic property of magnet, particularly the coercive force of magnet be promoted obviously.
In the present invention, related magnet is that the magnet of any material containing rare earth is as sintered NdFeB magnet.Each embodiment passes through the standby neodymium iron boron magnetic body of electrodeposited coating legal system under different experimental conditions below, and the thickness of magnet surface coating (the hydrogenation dysprosium particle of take is example) is as shown in table 1 with the variation of electrodeposition time.By having tested every magnetic parameter of magnet after different process thermal treatment.For convenient contrast, the raw magnetic of magnet before processing can also provide (in Table 2) in the lump.
Adopt electro-deposition method by above-mentioned hydride particle on sintered Nd Fe B rare-earth magnet surface, form evenly, densification and the controlled coating of thickness.Described rare earth hydride particulate coating can obviously improve the coercive force of the magnetic property, particularly magnet of sintered Nd Fe B rare-earth magnet.Adopt the inventive method guaranteeing that magnet has under the prerequisite of good magnetic property, reduce the usage quantity of heavy rare earths in sintered Nd Fe B rare earth, thereby reduce the manufacturing cost of high-coercive force 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
The rare earth hydrogenation dysprosium particle 20g of particle diameter 100 nanometers is evenly mixed with the n-heptane solution of 1000ml, make hydrogenation dysprosium be dispersed in uniformly in normal heptane, and adopt induction stirring to guarantee that in electrolyzer, concentration is consistent everywhere, prepare the suspension liquid that is used to form hydrogenation dysprosium particulate coating, its concentration be 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 No. 1 magnet in 2) is prepared into the small pieces of physical dimension 10 * 10 * 3.5mm, and polished finish is carried out in its surface.Magnet after processing is connected to negative electrode, and anode adopts area to be slightly larger than magnet over against the stainless steel substrates of area, and cathode and anode spacing is controlled at 2.5cm left and right, 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, with nickel is thin, magnet pack is wrapped.Afterwards, by being surrounded by neodymium iron boron magnetic body that nickel is thin, to be placed in vacuum tightness be 1 * 10
-4in the heat treatment furnace of Pa, one-level thermal treatment temp is 810 ℃, 5 hours; Secondary thermal treatment temp is 500 ℃, 3 hours.After processing, the final magnetic property parameter of magnet is in Table No. 2 magnets in 2.
Embodiment 2
The rare earth hydrogenation terbium particle 10g of particle diameter 100 nanometers is evenly mixed with the n-heptane solution of 1000ml, make hydrogenation terbium be dispersed in uniformly in normal heptane, and adopt induction stirring to guarantee that in electrolyzer, concentration is consistent everywhere, prepare the suspension liquid that is used to form hydrogenation terbium particulate coating, its concentration is 0.01g/ml.
Sintered NdFeB magnet (its magnetic property parameter is in Table No. 1 magnet in 2) is prepared into the small pieces of physical dimension 10 * 10 * 3.5mm, and polished finish is carried out in its surface.Magnet after processing is connected to negative electrode, and anode adopts area to be slightly larger than magnet over against the stainless steel substrates of area, and cathode and anode spacing is controlled at 2.5cm left and right, 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, with nickel is thin, magnet pack is wrapped.Afterwards, by being surrounded by neodymium iron boron magnetic body that nickel is thin, to be placed in vacuum tightness be 1 * 10
-4in the heat treatment furnace of Pa, one-level thermal treatment temp is 790 ℃, 5 hours; Secondary thermal treatment temp is 500 ℃, 3 hours.After processing, the final magnetic property parameter of magnet is in Table No. 3 magnets in 2.
Embodiment 3
The rare earth praseodymium hydride particle 60g of particle diameter 150 nanometers is evenly mixed with the n-heptane solution of 1000ml, make praseodymium hydride be dispersed in uniformly in normal heptane, and adopt induction stirring to guarantee that in electrolyzer, concentration is consistent everywhere, prepare the suspension liquid that is used to form praseodymium hydride particulate coating, its concentration is 0.06g/ml.
Sintered NdFeB magnet (its magnetic property parameter is in Table No. 1 magnet in 2) is prepared into the small pieces of physical dimension 10 * 10 * 3.5mm, and polished finish is carried out in its surface.Magnet after processing is connected to negative electrode, and anode adopts area to be slightly larger than magnet over against the stainless steel substrates of area, and cathode and anode spacing is controlled at 2.5cm left and right, 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, with nickel is thin, magnet pack is wrapped.Afterwards, by being surrounded by neodymium iron boron magnetic body that nickel is thin, to be placed in vacuum tightness be 1 * 10
-4in the heat treatment furnace of Pa, one-level thermal treatment temp is 870 ℃, 7 hours; Secondary thermal treatment temp is 500 ℃, 3 hours.After processing, the final magnetic property parameter of magnet is in Table No. 4 magnets in 2.
Embodiment 4
The rare earth neodymium hydride particle 80g of particle diameter 150 nanometers is evenly mixed with the hexane solution of 1000ml, make neodymium hydride be dispersed in uniformly in normal hexane, and adopt magnetic agitation to guarantee that in electrolyzer, concentration is consistent everywhere, prepare the suspension liquid that is used to form neodymium hydride particulate coating, its concentration is 0.08g/ml.
Sintered NdFeB magnet (its magnetic property parameter is in Table No. 1 magnet in 2) is prepared into the small pieces of physical dimension 10 * 10 * 3.5mm, and polished finish is carried out in its surface.Magnet after processing is connected to negative electrode, and anode adopts area to be slightly larger than magnet over against the stainless steel substrates of area, and cathode and anode spacing is controlled at 2.5cm left and right, 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, with nickel is thin, magnet pack is wrapped.Afterwards, by being surrounded by neodymium iron boron magnetic body that nickel is thin, to be placed in vacuum tightness be 1 * 10
-4in the heat treatment furnace of Pa, one-level thermal treatment temp is 850 ℃, 6 hours; Secondary thermal treatment temp is 500 ℃, 3h.After processing, the final magnetic property parameter of magnet is in Table No. 5 magnets in 2.
Embodiment 5
The rare earth hydrogenation holmium particle 100g of particle diameter 200 nanometers is evenly mixed with the hexane solution of 1000ml, make hydrogenation holmium be dispersed in uniformly in normal hexane, and adopt magnetic agitation to guarantee that in electrolyzer, concentration is consistent everywhere, prepare the suspension liquid that is used to form hydrogenation holmium particulate coating, its concentration is 0.1g/ml.
Sintered NdFeB magnet (its magnetic property parameter is in Table No. 1 magnet in 2) is prepared into the small pieces of physical dimension 10 * 10 * 3.5mm, and polished finish is carried out in its surface.Magnet after processing is connected to negative electrode, and anode adopts area to be slightly larger than magnet over against the stainless steel substrates of area, and cathode and anode spacing is controlled at 2.5cm left and right, 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, with nickel is thin, magnet pack is wrapped.Afterwards, by being surrounded by neodymium iron boron magnetic body that nickel is thin, to be placed in vacuum tightness be 1 * 10
-4in the heat treatment furnace of Pa, one-level thermal treatment temp is 830 ℃, 7 hours; Secondary thermal treatment temp is 500 ℃, 3h.After processing, the final magnetic property parameter of magnet is in Table No. 6 magnets in 2.
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 times obtain
| Time/second | 10 | 20 | 40 | 80 | 150 | 220 |
| Coat-thickness/μ m | 138.96 | 166.48 | 169.77 | 274.08 | 415.71 | 452.10 |
Table 2
Claims (10)
1. the treatment agent of a rare earth hydride particle, it is characterized in that, described treatment agent is in dispersion agent, to be dispersed with rare earth hydride particle, and the selected dispersion agent for the treatment of agent is normal hexane or normal heptane, and described rare earth is at least one in Pr, Nd, Tb, Dy, Ho.
2. according to the treatment agent of a kind of rare earth hydride particle of claim 1, it is characterized in that, the scope of the average particulate diameter of rare earth hydride is between 100-500 nanometer.
3. 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.
4. 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.
5. according to the treatment agent of any rare earth hydride particle described in claim 1-4, for galvanic deposit, prepare rare earth hydride particulate coating.
6. any treatment agent described in employing claim 1-4 is prepared 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 that forms rare earth hydride top coat, treatment agent is inserted in galvanic deposition cell, and constantly stir and make 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 to treatment agent suspension and carry out galvanic deposit, in neodymium-iron-boron surface, obtain rare earth hydride granular layer, afterwards the magnet that deposits rare earth hydride granular layer is taken out, air-dry, then with nickel foil, magnet pack is wrapped, at the temperature of 790 ℃-870 ℃, carry out one-level thermal treatment, time 5-7 hour, and then at the temperature of 500 ℃, carry out secondary thermal treatment, 3 hours time.
7. according to the method for claim 6, it is characterized in that, neodymium iron boron magnetic body glazed surface is over against stainless steel substrates, and the area of stainless steel substrates is slightly larger than neodymium iron boron magnetic body glazed surface area.
8. according to the method for claim 6, it is characterized in that, cathode and anode spacing is controlled at 1-5cm, galvanic deposit voltage 50-300v, electric current 10-100mA.
9. according to the method for claim 6, it is characterized in that cathode and anode spacing 2.5cm, galvanic deposit voltage 150v, electric current 40mA.
10. according to the method for claim 6, it is characterized in that electrodeposition time 10-220 second forms the rare earth hydride particulate coating of different thickness.
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| 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 |
| 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 |
| 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 |
| 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 |
| CN106319441A (en) * | 2016-08-31 | 2017-01-11 | 浙江凯文磁业有限公司 | Dysprosium permeating process capable of improving performances of neodymium iron boron |
| 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 |
| CN108461272A (en) * | 2018-03-20 | 2018-08-28 | 北京工业大学 | A technique for being used to form hydride nano-particle face coat |
| CN108597840A (en) * | 2018-04-04 | 2018-09-28 | 北京工业大学 | A kind of the diffusion into the surface method and its device of nano particle |
| CN110556243A (en) * | 2019-08-19 | 2019-12-10 | 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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| 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 |
| 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 |
| 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 |
| 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 |
| CN106319441A (en) * | 2016-08-31 | 2017-01-11 | 浙江凯文磁业有限公司 | Dysprosium permeating process capable of improving performances of neodymium iron boron |
| 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 |
| CN108461272A (en) * | 2018-03-20 | 2018-08-28 | 北京工业大学 | A technique for being used to form hydride nano-particle face coat |
| CN108597840A (en) * | 2018-04-04 | 2018-09-28 | 北京工业大学 | A kind of the diffusion into the surface method and its device of nano particle |
| CN108597840B (en) * | 2018-04-04 | 2020-07-03 | 北京工业大学 | Surface diffusion method and device for nano particles |
| CN110556243A (en) * | 2019-08-19 | 2019-12-10 | 安徽省瀚海新材料股份有限公司 | neodymium iron boron surface dysprosium penetration method |
| 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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Effective date of registration: 20230705 Address after: 100124 No. 100 Chaoyang District Ping Tian Park, Beijing Patentee after: Beijing University of Technology Patentee after: EARTH-PANDA ADVANCE MAGNETIC MATERIAL Co.,Ltd. Address before: 100124 No. 100 Chaoyang District Ping Tian Park, Beijing Patentee before: Beijing University of Technology |