CN103426621B - A kind of method and size conditioning agent regulating neodymium iron boron magnetic body size - Google Patents

A kind of method and size conditioning agent regulating neodymium iron boron magnetic body size Download PDF

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CN103426621B
CN103426621B CN201310243557.3A CN201310243557A CN103426621B CN 103426621 B CN103426621 B CN 103426621B CN 201310243557 A CN201310243557 A CN 201310243557A CN 103426621 B CN103426621 B CN 103426621B
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conditioning agent
size
iron boron
neodymium iron
powder
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CN103426621A (en
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金向阳
赵冶
卢燎花
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ZHEJIANG ZHONGYUAN MAGNETIC INDUSTRY Co Ltd
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ZHEJIANG ZHONGYUAN MAGNETIC INDUSTRY Co Ltd
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Abstract

The invention provides a kind of method regulating neodymium iron boron magnetic body size, neodymium iron boron powder is it is characterized in that fully to carry out batch mixing by adding size conditioning agent after airflow milling, then shaping in Magnetic field press, be heated to 300 DEG C of constant temperature by vacuum furnace after molded blank enters sintering furnace, conditioning agent is discharged from blank.Use size conditioning agent can also reduce friction between powder in the compacting of neodymium iron boron powder, there is lubricant.Because the zinc stearate in size conditioning agent composition originally, in molding neodymium iron boron process, can reduce the frictional force between magnetic powder particle, make the mobility of powder strengthen, the degree of orientation of magnet improves.Shaping pressing process is become the blank with certain density gradually along with the increase powder of pressure by loose state, when magnetic has higher density, add lubricant to overcoming the effect of magnetic coagulation not clearly, but to reducing the frictional force that has in the blank of certain density between powder, improving the degree of orientation and also having and act on very significantly.

Description

A kind of method and size conditioning agent regulating neodymium iron boron magnetic body size
Technical field
The invention belongs to magnetic auxiliary material and preparation method thereof, specifically a kind of method and size conditioning agent regulating neodymium iron boron magnetic body size.
Background technology
Nd-Fe-B permanent magnet is as third generation rare-earth permanent magnet, there is the price of excellent magnetic property, good processing characteristics and relative moderate, be widely used at numerous areas such as industrial automation, computer, household electrical appliances, communications, China's neodymium iron boron magnetic body industry is since 1984, through the development of more than 20 years, there is significant progress, achieved the achievement attracted attention in the world.The sintered NdFeB that China produces, Agglutinate neodymium-iron-boron etc. are all taken its place in the front ranks of the world.All higher level is reached in raw material supplying, output, variety and quality, technology, domestic application amount and market sales volume etc.Wherein the output of sintered NdFeB, application quantity and market sales volume are particularly outstanding at home and abroad, and the output calendar year 2001 of sintered NdFeB just exceedes Japan and ranks first in the world.Within 2010, China's Sintered NdFeB magnet output reaches nearly 80,000 tons, accounts for 80% of Gross World Product.
Through effort for many years, the magnetic property of sintered NdFeB product has had and has significantly improved, the sintered NdFeB maximum magnetic energy product prepared under experiment condition (BH) maxreach 474kJ/m 3(59.5MGOe), close to 93% of theoretical value.Many enterprises of China also can produce N52 ~ N54 trade mark ((BH) maxbe 52 ~ 54MGOe) high performance sintered NdFeB product.Because raw material (rare earth) rise in price of neodymium iron boron magnetic body is in recent years comparatively large, considers reduction production cost, reduce the waste of rare earth resources, control NbFeB sintered blank dimension as far as possible.And the requirement of client to the apparent size of product is in recent years also more and more tighter.So also adding year by year sternly the size tolerance requirements of neodymium iron boron manufacturer production blank.But Sintered NdFeB magnet shrinks in sintering process, there are many factors can have influence on the size (radial, longitudinal shrinkage) of product.And this radial direction, longitudinal shrinkage uncertain factor bring inconvenience to neodymium iron boron manufacturer to guarantee product specification.A lot of product man encounters this situation, and the properties of product everyway made well only because size does not reach requirement, can not be delivered.And can only more more mold exchange again produce to ensure the specification of product, thus add production cost, delay the delivery date of product.For above-mentioned phenomenon, research and development department of Zhejiang Zhongyuan Magnetic Material Co., Ltd. member is studied the factor affecting sintered NdFeB cylinder magnet length (or size of square), find granularity and the oxygen absorbed of powder in production process, the density of molded blank, sintering temperature has impact to small dimension cylinder magnet amount of contraction along its length, under normal circumstances, certain at formula, sintering process is certain, certain and the filler one of pressure Bear-grudge mould regularly, the oxygen absorbed of powder, the shaping density be press-fitted, when sintering temperature does not become research and development department of our company by a large amount of experimental formula adjustable neodymium-iron-boron steel dimensions conditioning agent (main component relates to the materials such as zinc stearate) in a kind of scope.Practice shows that adding a certain proportion of size conditioning agent can have larger adjustable range to neodymium iron boron magnetic body amount of contraction along its length, and the increasing along with addition occurs that cylinder length increases gradually, the radial trend reduced gradually.Carry out this discussing and inquiring into.
Summary of the invention
In order to solve the problems of the technologies described above, the invention provides a kind of method and the size conditioning agent that regulate neodymium iron boron magnetic body size.
A kind of method regulating neodymium iron boron magnetic body size, neodymium iron boron powder is it is characterized in that fully to carry out batch mixing by adding size conditioning agent after airflow milling, then shaping in Magnetic field press, be heated to 300 DEG C of constant temperature by vacuum furnace after molded blank enters sintering furnace, conditioning agent is discharged from blank.
A kind of described method regulating neodymium iron boron magnetic body size, is characterized in that the interpolation weight of described size conditioning agent is 0.2 ‰-0.5 ‰ of neodymium iron boron powder weight.
Regulate a size conditioning agent for neodymium iron boron magnetic body size, it is characterized in that it is made up of the raw material of following weight percentage: zinc stearate 15-30%; Oxirane alkyl ether 10-20%; Oleic acid 0.1-5%; Nano zircite 0.05%-0.5%; Benzinum 30-65%.
Described a kind of size conditioning agent regulating neodymium iron boron magnetic body size, is characterized in that other mixtures also comprising 5-10% weight percentage in described raw material.
Use size conditioning agent can also reduce friction between powder in the compacting of neodymium iron boron powder, there is lubricant.Because the zinc stearate in size conditioning agent composition originally, in molding neodymium iron boron process, can reduce the frictional force between magnetic powder particle, make the mobility of powder strengthen, the degree of orientation of magnet improves.Shaping pressing process is become the blank with certain density gradually along with the increase powder of pressure by loose state, when magnetic has higher density, add lubricant to overcoming the effect of magnetic coagulation not clearly, but to reducing the frictional force that has in the blank of certain density between powder, improving the degree of orientation and also having and act on very significantly.
Embodiment
For determining the impact of the interpolation of size conditioning agent on sintering blank dimension, the experiment adopted is as follows: after airflow milling, neodymium-iron-boron powder adds 0.2 ‰ respectively, 0.3 ‰, the even batch mixing of 0.5 ‰ size conditioning agent and the material not adding conditioning agent contrast, be pressed into blank through overmolding, again through oversintering and heat treatment, the sintering blank dimension obtained is as shown in the table.In table, short transverse size can claim opaque amount to control by regulating.Experiment shows, along with the increase of conditioning agent content, sintering direction of orientation shrinkage reduces.Regulate sintering shrinkage, be conducive to the NdFeB blank obtaining different size with same compacting tool set, size difference can reach 10%, and the production for neodymium iron boron brings very large convenience.Substantially increase the size rate of finished products of neodymium iron boron product, improve the delivery rate that product hands over the phase.Reduce manufacturing cost and the rework cost of mould.
Table 1 different size conditioning agent addition is on the impact of sintering nominal dimension
As can be seen from Table 1; , along with the raising of conditioning agent addition, the direction of orientation length of product has larger increase, increase volume amplitude and conditioning agent addition number relevant.The above results represents, reduce product from the direction of orientation amount of contraction macroscopically showing as product elongated, pressing direction amount of contraction increases miscellaneous goods size and diminishes, and it is elongated that fore-and-aft direction amount of contraction reduces product a little.Under square one, it is relatively more remarkable that direction of orientation change shows.Short transverse size can control and make up product amount of contraction by the input amount increasing powder and cause greatly product size to change.Thus reach the object regulating product direction of orientation size in certain limit.But too much adds lubricant (when being increased to 0.08%), the remanent magnetism of magnet and magnetic property will be affected and can decrease on the contrary, although this is because the addition of increase conditioning agent can make the degree of orientation increase, but lubricant too much in magnet is difficult to haul out completely when sintering, cause C content in magnet higher, sintered magnet density reduces, and the remanent magnetism of magnet and magnetic energy product is not only improved, declines on the contrary.
Add conditioning agent in addition to improve the degree of orientation of product and the density of product and also have and act on significantly.After not adding lubricant sintering, the microstructure of magnet compares, and the magnet intercrystalline not adding lubricant exists cavity; The magnet adding lubricant is fine and close obviously good than un-added, and the sintered magnet not adding lubricant occurs that cavity is the flowing of the frictional force obstruction powder between powder, the arch formation of appearance.When the addition of lubricant is increased to 0.05% by 0.02%, remanent magnetism is increased to 1.365T by 1.35T, relative increase is 1.1%, magnetic energy product also has corresponding increase, suitably increases the degree of orientation that additivated addition can improve magnet, remanent magnetism and magnetic energy product, in an experiment, when lubricant addition is 0.05%, whole powder sufficient lubrication can be made, magnet remanent magnetism and comprehensive permanent magnetism performance best while also reach and regulate the object of product size.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., be all included within protection scope of the present invention.

Claims (1)

1. one kind regulates the method for neodymium iron boron magnetic body size, neodymium iron boron powder is it is characterized in that fully to carry out batch mixing by adding size conditioning agent after airflow milling, then shaping in Magnetic field press, be heated to 300 DEG C of constant temperature by vacuum furnace after molded blank enters sintering furnace, conditioning agent is discharged from blank; Size conditioning agent is made up of the raw material of following weight percentage: zinc stearate 15-30%; Oxirane alkyl ether 10-20%; Oleic acid 0.1-5%; Nano zircite 0.05%-0.5%; Benzinum 30-65%; The interpolation weight of described size conditioning agent is 0.2 ‰-0.5 ‰ of neodymium iron boron powder weight.
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CN110369713B (en) * 2019-08-21 2020-03-10 济南市冶金科学研究所有限责任公司 Method for controlling size of hard alloy hobbing cutter product
CN112768170B (en) * 2020-12-30 2022-11-01 烟台正海磁性材料股份有限公司 Rare earth permanent magnet and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5634189A (en) * 1993-11-11 1997-05-27 Mtu Motoren-Und Turbinen Union Munchen Gmbh Structural component made of metal or ceramic having a solid outer shell and a porous core and its method of manufacture
CN1450569A (en) * 2003-04-28 2003-10-22 宁波韵升(集团)股份有限公司 Method for mfg of sintered Nd-Fe-B
CN1909124A (en) * 2006-08-23 2007-02-07 北京科技大学 Magnetic field gel injection molding method for large scale rare-earth sintering magnet
CN102240805A (en) * 2011-07-27 2011-11-16 湖南航天工业总公司 Method for preparing anisotropic bonded rare-earth permanent magnet
CN102982992A (en) * 2012-08-02 2013-03-20 横店集团东磁股份有限公司 Manufacturing method of room temperature wet pressing molding anisotropic bonding NdFeB magnet

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5634189A (en) * 1993-11-11 1997-05-27 Mtu Motoren-Und Turbinen Union Munchen Gmbh Structural component made of metal or ceramic having a solid outer shell and a porous core and its method of manufacture
CN1450569A (en) * 2003-04-28 2003-10-22 宁波韵升(集团)股份有限公司 Method for mfg of sintered Nd-Fe-B
CN1909124A (en) * 2006-08-23 2007-02-07 北京科技大学 Magnetic field gel injection molding method for large scale rare-earth sintering magnet
CN102240805A (en) * 2011-07-27 2011-11-16 湖南航天工业总公司 Method for preparing anisotropic bonded rare-earth permanent magnet
CN102982992A (en) * 2012-08-02 2013-03-20 横店集团东磁股份有限公司 Manufacturing method of room temperature wet pressing molding anisotropic bonding NdFeB magnet

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Denomination of invention: A method for adjusting the size of NdFeB magnet and size regulator

Effective date of registration: 20221127

Granted publication date: 20151223

Pledgee: ZHEJIANG DONGYANG RURAL COMMERCIAL BANK Co.,Ltd.

Pledgor: ZHEJIANG ZHONGYUAN MAGNETIC MATERIAL CO.,LTD.

Registration number: Y2022330003219