CN101266858A - A processing method for sintering neodymium-iron-boron magnetic material - Google Patents
A processing method for sintering neodymium-iron-boron magnetic material Download PDFInfo
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- CN101266858A CN101266858A CNA2008100190814A CN200810019081A CN101266858A CN 101266858 A CN101266858 A CN 101266858A CN A2008100190814 A CNA2008100190814 A CN A2008100190814A CN 200810019081 A CN200810019081 A CN 200810019081A CN 101266858 A CN101266858 A CN 101266858A
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Abstract
The invention relates to a processing method for a sintering neodymium ferroboron permanent magnet material, comprising the steps of: cleaning and confecting raw materials, melting and preparing the alloy, crushing the alloy into powder and forming in a magnetic field, and then sintering and performing a heat treatment; the alloy is respectively a main phase whose ingredient is close to positive Nd<2>Fe<14>B ingredient; liquid phase 1: Re50-65Fe remaining B 0-1.5, M 0-2, liquid phase 2: Re80-100Fe remaining M 0-10; the ingredient Re28-38M after mixing remains B 1-1.5. Re is one or more of rare earth elements consisting of La or Ce or Pr or Nd or Eu or Gd or Tb or Dy or Ho or Er, M is the metal alloy of Co, Fe, Ni, Al, Zr, Ga. The processing method of the invention can obtain a neodymium ferroboron magnet with high coercive force, low temperature coefficient, and great abilities to resist the high temperature and corrosion.
Description
Technical field
The present invention relates to a kind of method for metal working, be specifically related to a kind of improvement of sintered NdFeB processing method.
Background technology
In recent years, whole world neodymium iron boron output on average reaches the growth rate in year 25%, and China has become big country, the power that produces neodymium iron boron magnetic body, and annual production accounts for world's total amount nearly 80%.But, China's rare earth permanent-magnetic material technology of preparing and magnet performance aspect with certain gap is abroad arranged.Along with the continuous expansion of neodymium iron boron magnetic body application, more and more higher to its performance demands.Particularly high temperature resistant, high-coercive force neodymium iron boron magnetic body will be more and more wider in the application of machine field.The serviceability temperature key that improves the NdFeB magnet is to improve its Curie temperature Tc and HCJ Hcj.Improving the coercitive main path of NdFeB magnet at present is the alloying means, comprises being aided with suitable heat treatment.The technology of alloying is by smelting technology, makes it be smelted directly into multicomponent alloy.Mainly contain: 1. single alloy preparation method has been used for the large-scale production Sintered NdFeB magnet.2. the two-phase alloys method adopts and approaches Nd at composition
2Fe
14Add the higher parafacies alloy of content of rare earth in the B main-phase alloy and produce high-performance neodymium-iron-boron magnet.But adopt the resulting neodymium iron boron magnetic body of above processing method lower than the performance that present single alloy preparation method obtains, the high-coercive force magnet remanent magnetism of acquisition descends bigger.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, designed and developed out a kind of processing method that can process high-coercive force, low-temperature coefficient, high temperature resistant, high anti-corrosion neodymium iron boron magnetic body.
The present invention is achieved by the following technical solutions:
A kind of processing method of sintered Nd-Fe-B magnetic material, comprise raw material is cleaned, carry out preparation raw material by composition, and prepare alloy with induction furnace melting, with the broken powder process of alloy and mixing back moulding in magnetic field, through sintering and heat treatment promptly, described alloy is respectively the alloy of three kinds of different content of rare earth again, and wherein a kind of composition is near just dividing Nd
2Fe
14The principal phase of B composition; Two kinds of alloy liquid phase compositions are respectively in addition: the surplus B0-1.5M0-2 of liquid phase 1:Re50-65Fe, the surplus M0-10 of liquid phase 2:Re80-100Fe; More than three kinds of alloys broken and mix after shared separately weight ratio, liquid phase 1 is 1%～10%, liquid phase 2 is 0.5%～5%, all the other are principal phase; Mix the surplus B1-1.5 of back composition Re28-38M, Re is a rare earth element, and M is the metal alloy of Co, Fe, Ni, Al, Zr, Ga.
A kind of processing method of sintered Nd-Fe-B magnetic material, described Re is one or more in La or Ce or Pr or Nd or Eu or Gd or Tb or Dy or Ho or the Er rare earth element.
A kind of processing method of sintered Nd-Fe-B magnetic material, described melting is the method melting preparation with vacuum induction melting.
A kind of processing method of sintered Nd-Fe-B magnetic material, the broken powder process of described alloy is broken for the explosion of employing hydrogen, airflow milling powder process.
A kind of processing method of sintered Nd-Fe-B magnetic material, described alloy powder mixes and mixes under inert gas shielding.
A kind of processing method of sintered Nd-Fe-B magnetic material, described alloy powder mixes and mixes under the normal temperature state.
A kind of processing method of sintered Nd-Fe-B magnetic material describedly is sintered to vacuum-sintering.
The present invention adopts " principal phase+biliquid phase alloy " technology, by adding element, has improved the remanent magnetism and the coercitive temperature coefficient of neodymium iron boron magnetic body; Adopt biliquid phase alloy sintering process, dissimilar and alloy element quantity are directly introduced magnet intergranular zone, make it in sintering and subsequently ag(e)ing process, metallurgical reaction take place mutually with original intergranular, the interfacial structure of the character that changes the intergranular phase and distribution and intergranular and principal phase, thereby improve the coercive force of magnet, produce the high-coercive force Sintered NdFeB magnet.
Biliquid phase technology is to improve the coercitive effective way of magnet, and main-phase alloy and crystal-boundary phase alloy are prepared respectively, mixes by certain proportioning, and crystal boundary is dispersed in around the principal phase mutually, and by prepared such as sintering, tempering.So both reduced crystal boundary separating out in principal phase, and can reduce it again in the reunion that crystal boundary hands over the corner to locate, and made principal phase more reasonable with crystal boundary composition mutually, the content of rare earth of principal phase can be more near Nd simultaneously
2Fe
14B is just dividing ratio, also can obtain higher H
CJTherefore biliquid phase alloy technology can guarantee to also have enough crystal boundaries to exist mutually when very low content of rare earth, guarantees that alloy has high H
CJ
Adopt biliquid phase alloy sintering process to improve the corrosion resistance and the resistance to elevated temperatures of magnet.Result of study shows, is the main existence zone of block rich Nd phase near the boundary corner of neodymium iron boron magnetic body inside, also is the higher relatively zone of surface energy, also is the easiest zone that is corroded of magnet therefore.Also having some studies show that, also is the zone of the easier formation of nuclei of reversed domain near the crystal boundary corner.Therefore, our research emphasis that will improve the neodymium iron boron magnetic body corrosion resistance has been placed on chemical composition and the configuration aspects of optimizing the crystal boundary corner.
Consider that rich Nd finishes the back except being present in the grain boundary at sintering, some mainly is present in the crystal boundary corner.If can reduce crystal boundary corner place rich Nd phase amount or by the chemical composition that changes the rich Nd phase in crystal boundary corner place its chemism is reduced, then just might significantly increase the corrosion resistance of magnet.Therefore, we have designed biliquid phase alloy sintering process.The main feature of this technology is: principal phase powder and two kinds of liquid phase powder are mixed the back pressing under magnetic field by a certain percentage, carry out sintering and heat treatment then, having produced magnetic property is the prescription and a whole set of production technology of resistant to elevated temperatures Sintered NdFeB magnet.
Studies show that, also be the zone of the easier formation of nuclei of reversed domain near the crystal boundary corner.Consider that rich Nd finishes the back except being present in the grain boundary at sintering, some mainly is present in the crystal boundary corner.By the microstructure of single liquid phase magnet and biliquid phase alloy magnet is discovered, the boundary structure of the magnet of producing with new sintering process is more regular and complete more than the grain boundary structure of the magnet of producing with conventional liquid sintering technology.
The crystal boundary corner of the neodymium iron boron magnetic body of producing with new sintering process is size little than the magnet of producing with conventional single liquid sintering technology not only, and become regular more.We think that this may be that the magnet of biliquid phase alloy sintering process production is than having higher corrosion resistance and durothermic reason with the magnet of conventional single liquid sintering technology production.
Experiment embodiment data and result
Adopt the magnetic property such as the following table of the 33EH high-coercive force Sintered NdFeB magnet of this explained hereafter:
| Title | Unit | 33EH |
| Residual magnetic flux density Br | mT(KGs) | 1130-1180 (11.3-11.8) |
| Coercivity H b | KA/m(KOe) | ≥812(≥10.2) |
| HCJ Hcj | KA/m(KOe) | ≥2388(≥30) |
| Maximum magnetic energy product (BH) max | KJ/m 3(MGOe) | 247-271(31-34) |
| Remanent magnetism temperature coefficient α Br | ％/℃ | ≤-0.09 |
| Coercive force temperature coefficient α Hcj | ％/℃ | ≤-0.48 |
| Maximum operation (service) temperature | ℃ | 200 |
Description of drawings
Accompanying drawing is the flow process chart of the inventive method.
Embodiment
Embodiment 1
The processing method of sintered Nd-Fe-B magnetic material; at first raw material is cleaned; carry out preparation raw material by composition; and prepare alloy with the method melting of vacuum induction melting; adopt the hydrogen explosion broken alloy, airflow milling powder process and under inert gas shielding the normal temperature state mix back moulding in magnetic field, more promptly through vacuum-sintering and heat treatment; alloy is respectively the alloy of three kinds of different content of rare earth, and wherein a kind of composition is the approaching Nd that just dividing
2Fe
14The principal phase of B composition; Two kinds of alloy liquid phase compositions are respectively in addition: the surplus B0-1.5M0-2 of liquid phase 1:La50-65Fe, the surplus M0-10 of liquid phase 2:La 80-100Fe; More than three kinds of alloys broken and mix after shared separately weight ratio, liquid phase 1 is 1%～10%, liquid phase 2 is 0.5%～5%, all the other are principal phase; Mix the surplus B1-1.5 of back composition La 28-38M, M is the metal alloy of Co, Fe, Ni, Al, Zr, Ga.
Embodiment 2
The surplus B0-1.5M0-2 of liquid phase 1:Ce50-65Fe, the surplus M0-10 of liquid phase 2:Ce 80-100Fe; Mix the surplus B1-1.5 of back composition Ce 28-38M.All the other are with embodiment 1.
Embodiment 3
The surplus B0-1.5M0-2 of liquid phase 1:Pr50-65Fe, the surplus M0-10 of liquid phase 2:Pr 80-100Fe; Mix the surplus B1-1.5 of back composition Pr 28-38M.All the other are with embodiment 1.
Embodiment 4
The surplus B0-1.5M0-2 of liquid phase 1:Nd50-65Fe, the surplus M0-10 of liquid phase 2:Nd 80-100Fe; Mix the surplus B1-1.5 of back composition Nd 28-38M.All the other are with embodiment 1.
Embodiment 5
The surplus B0-1.5M0-2 of liquid phase 1:Eu50-65Fe, the surplus M0-10 of liquid phase 2:Eu 80-100Fe; Mix the surplus B1-1.5 of back composition Eu 28-38M.All the other are with embodiment 1.
Embodiment 6
The surplus B0-1.5M0-2 of liquid phase 1:Dy50-65Fe, the surplus M0-10 of liquid phase 2:Dy 80-100Fe; Mix the surplus B1-1.5 of back components D y 28-38M.All the other are with embodiment 1.
Embodiment 7
The surplus B0-1.5M0-2 of liquid phase 1:DyEr50-65Fe, the surplus M0-10 of liquid phase 2:DyEr 80-100Fe; Mix the surplus B1-1.5 of back components D yEr 28-38M.All the other are with embodiment 1.
Claims (7)
1, a kind of processing method of sintered Nd-Fe-B magnetic material, comprise raw material is cleaned, carry out preparation raw material by composition, and prepare alloy with induction furnace melting, with the broken powder process of alloy and mixing back moulding in magnetic field, through sintering and heat treatment promptly, it is characterized in that described alloy is respectively the alloy of three kinds of different content of rare earth again, wherein a kind of composition is near just dividing Nd
2Fe
14The principal phase of B composition; Two kinds of alloy liquid phase compositions are respectively in addition: the surplus B0-1.5M0-2 of liquid phase 1:Re50-65Fe, the surplus M0-10 of liquid phase 2:Re80-100Fe; More than three kinds of alloys broken and mix after shared separately weight ratio, liquid phase 1 is 1%～10%, liquid phase 2 is 0.5%～5%, all the other are principal phase; Mix the surplus B1-1.5 of back composition Re28-38M; Re is a rare earth element, and M is the metal alloy of Co, Fe, Ni, Al, Zr, Ga.
2, the processing method of a kind of sintered Nd-Fe-B magnetic material according to claim 1 is characterized in that described Re is one or more in La or Ce or Pr or Nd or Eu or Gd or Tb or Dy or Ho or the Er rare earth element.
3, the processing method of a kind of sintered Nd-Fe-B magnetic material according to claim 1 is characterized in that described melting is the method melting preparation with vacuum induction melting.
4, the processing method of a kind of sintered Nd-Fe-B magnetic material according to claim 1 is characterized in that the broken powder process of described alloy is broken for the explosion of employing hydrogen, airflow milling powder process.
5, the processing method of a kind of sintered Nd-Fe-B magnetic material according to claim 1 is characterized in that described alloy powder mixing mixes under inert gas shielding.
6, a kind of processing method of sintered Nd-Fe-B magnetic material according to claim 1 or 5, it is characterized in that described alloy powder mixes mixes under the normal temperature state.
7, the processing method of a kind of sintered Nd-Fe-B magnetic material according to claim 1 is characterized in that the described vacuum-sintering that is sintered to.
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| CN102211192A (en) * | 2011-06-09 | 2011-10-12 | 天津一阳磁性材料有限责任公司 | Method for preparing high-performance neodymium iron boron by using secondary recycled materials |
| CN101728041B (en) * | 2008-10-24 | 2012-06-13 | 北京中科三环高技术股份有限公司 | Manufacturing method of ring-shaped sintered neodymium-iron-boron magnet |
| CN102856029A (en) * | 2012-04-20 | 2013-01-02 | 漯河市三鑫稀土永磁材料有限责任公司 | High (BH)max quick quenching magnetic powder and preparation method thereof |
| CN103100977A (en) * | 2013-01-29 | 2013-05-15 | 中国地质大学（北京） | Preparation method of high-strength diamond grinding wheel dressing pen |
| CN103280290A (en) * | 2013-06-09 | 2013-09-04 | 钢铁研究总院 | Cerium-containing low-melting-point rare-earth permanent magnet liquid phase alloy and production method of permanent magnet comprising same |
| CN103996522A (en) * | 2014-05-11 | 2014-08-20 | 沈阳中北通磁科技股份有限公司 | Manufacturing method for Ce-containing NdFeB rare earth permanent magnet |
| CN103996523A (en) * | 2014-05-11 | 2014-08-20 | 沈阳中北通磁科技股份有限公司 | Method for manufacturing La-contained high-performance neodymium iron boron rare earth permanent magnet |
| WO2015103905A1 (en) * | 2014-01-07 | 2015-07-16 | 中国科学院宁波材料技术与工程研究所 | Method for improving magnetic performance of sintered neodymium-iron-boron permanent magnet |
| CN104966607A (en) * | 2015-06-18 | 2015-10-07 | 安徽大地熊新材料股份有限公司 | Sintered Nd-Fe-B permanent magnet producing method |
| CN105598434A (en) * | 2015-11-12 | 2016-05-25 | 苏州萨伯工业设计有限公司 | Method for preparing rare earth permanent magnetic material by adding liquid phase nano europium to magnetic steel waste |
| CN106356175A (en) * | 2016-08-29 | 2017-01-25 | 四川省有色冶金研究院有限公司 | Double-main-phase Nd2Fe14B-Ce2Fe14B composite permanent magnet and preparation method thereof |
| CN107958760A (en) * | 2016-10-17 | 2018-04-24 | 中国科学院宁波材料技术与工程研究所 | A kind of rare earth permanent-magnetic material and preparation method thereof |
| CN110202324A (en) * | 2019-06-05 | 2019-09-06 | 浙江鑫盛永磁科技有限公司 | Ndfeb magnet manufacturing process |
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| CN101728041B (en) * | 2008-10-24 | 2012-06-13 | 北京中科三环高技术股份有限公司 | Manufacturing method of ring-shaped sintered neodymium-iron-boron magnet |
| CN102211192B (en) * | 2011-06-09 | 2012-12-26 | 天津一阳磁性材料有限责任公司 | Method for preparing high-performance neodymium iron boron by using secondary recycled materials |
| CN102211192A (en) * | 2011-06-09 | 2011-10-12 | 天津一阳磁性材料有限责任公司 | Method for preparing high-performance neodymium iron boron by using secondary recycled materials |
| CN102856029A (en) * | 2012-04-20 | 2013-01-02 | 漯河市三鑫稀土永磁材料有限责任公司 | High (BH)max quick quenching magnetic powder and preparation method thereof |
| CN103100977B (en) * | 2013-01-29 | 2015-05-06 | 中国地质大学（北京） | Preparation method of high-strength diamond grinding wheel dressing pen |
| CN103100977A (en) * | 2013-01-29 | 2013-05-15 | 中国地质大学（北京） | Preparation method of high-strength diamond grinding wheel dressing pen |
| CN103280290A (en) * | 2013-06-09 | 2013-09-04 | 钢铁研究总院 | Cerium-containing low-melting-point rare-earth permanent magnet liquid phase alloy and production method of permanent magnet comprising same |
| CN103280290B (en) * | 2013-06-09 | 2016-03-02 | 钢铁研究总院 | Containing cerium low melting point rare earth permanent magnetic liquid phase alloy and permanent magnet preparation method thereof |
| WO2015103905A1 (en) * | 2014-01-07 | 2015-07-16 | 中国科学院宁波材料技术与工程研究所 | Method for improving magnetic performance of sintered neodymium-iron-boron permanent magnet |
| CN103996522B (en) * | 2014-05-11 | 2016-06-15 | 沈阳中北通磁科技股份有限公司 | A kind of manufacture method of the Fe-B rare-earth permanent magnet containing Ce |
| CN103996523A (en) * | 2014-05-11 | 2014-08-20 | 沈阳中北通磁科技股份有限公司 | Method for manufacturing La-contained high-performance neodymium iron boron rare earth permanent magnet |
| CN103996522A (en) * | 2014-05-11 | 2014-08-20 | 沈阳中北通磁科技股份有限公司 | Manufacturing method for Ce-containing NdFeB rare earth permanent magnet |
| CN103996523B (en) * | 2014-05-11 | 2016-05-25 | 沈阳中北通磁科技股份有限公司 | A kind of manufacture method of the high-performance Ne-Fe-B rare-earth permanent magnet containing La |
| CN104966607A (en) * | 2015-06-18 | 2015-10-07 | 安徽大地熊新材料股份有限公司 | Sintered Nd-Fe-B permanent magnet producing method |
| CN104966607B (en) * | 2015-06-18 | 2017-03-01 | 安徽大地熊新材料股份有限公司 | A kind of preparation method of sintered Nd-Fe-B permanent magnet |
| CN105598434A (en) * | 2015-11-12 | 2016-05-25 | 苏州萨伯工业设计有限公司 | Method for preparing rare earth permanent magnetic material by adding liquid phase nano europium to magnetic steel waste |
| CN106356175A (en) * | 2016-08-29 | 2017-01-25 | 四川省有色冶金研究院有限公司 | Double-main-phase Nd2Fe14B-Ce2Fe14B composite permanent magnet and preparation method thereof |
| CN106356175B (en) * | 2016-08-29 | 2018-11-02 | 四川省有色冶金研究院有限公司 | A kind of double main phase Nd2Fe14B-Ce2Fe14B composite permanent magnets and preparation method thereof |
| CN107958760A (en) * | 2016-10-17 | 2018-04-24 | 中国科学院宁波材料技术与工程研究所 | A kind of rare earth permanent-magnetic material and preparation method thereof |
| CN110202324A (en) * | 2019-06-05 | 2019-09-06 | 浙江鑫盛永磁科技有限公司 | Ndfeb magnet manufacturing process |
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Application publication date: 20080917 |