CN102139369B - Preparation method of mixture of superfine neodymium, iron and boron powder and mixture - Google Patents
Preparation method of mixture of superfine neodymium, iron and boron powder and mixture Download PDFInfo
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- CN102139369B CN102139369B CN201010623551.5A CN201010623551A CN102139369B CN 102139369 B CN102139369 B CN 102139369B CN 201010623551 A CN201010623551 A CN 201010623551A CN 102139369 B CN102139369 B CN 102139369B
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Abstract
The invention discloses a preparation method of a mixture of superfine neodymium, iron and boron powder, which is characterized in that: the preparation method comprises the following steps of: (1) pretreating raw materials: preparing spherically sintered neodymium, iron and boron magnets and zirconium oxide as spheres used in a ball mill, and preparing a coating agent; (2) weighing materials: weighing 88-97wt% of neodymium, iron and boron powder, 0-5wt% of metallocene polyolefin elastomer, 1-5wt% of rubber and 1-2wt% of coating agent; (3) performing surface coating treatment; (4) mixing and grinding solid and liquid; and (5) filtering and sealing the mixture for storage to obtain the mixture of the superfine neodymium, iron and boron powder. The invention also discloses the mixture of the superfine neodymium, iron and boron powder prepared by the preparation method, and the preparation method can be widely applied to producing flexible plastic and magnetic products.
Description
Technical field
The present invention relates to macromolecule compound mixture, be specifically related to one and mould magnetic product for the manufacture of high-performance flexible, adopt preparation method and the mixture of the ultra-fine neodymium iron boron powder mixture of nanometer technology.
Background technology
Along with the development of society, particularly the developing rapidly of the technology such as various electric automobile, magnetic suspension train, high-performance motor, generator, makes the demand of high performance magnetic product increasing, also more and more higher to the characteristic requirements of product.
In prior art, bonded rare earth magnet processing method many employings mold pressing, injection and expressing technique, obtained magnet is all that rigidity is inelastic, and adopt mold pressing, injection molding technique more to need the mould of a large amount of different size, and need to carry out machined to size in the later stage, be unfavorable for the change of magnet specification, processing cost is higher.Although simultaneously rigidity magnet has higher magnetic property and certain freedom shape, the shortcoming such as automaticity not high, assembling inconvenience when there is motor application, and also the magnet being made into ultrathin (being less than 1.0mm) has certain difficulty.
Flexible bonding rare-earth magnet is a kind of new product of bonded rare earth magnet, be different from the rigid bond rare-earth magnet that injection moulding and mould pressing process are produced, take rubber as binding agent, employing rubber processing is produced, do not need a large amount of mould development expenses, production efficiency high, can free bend ftracture, product size can change arbitrarily, thickness can be less than 1 millimeter, be convenient to client assembles use, meet small and special electric machine to small-sized, ultra-thin, at a high speed, the requirement of high accuracy and low noise future development, market prospects are had an optimistic view of.Flexible adhesion permanent magnet has been widely used in the fields such as household electrical appliances, automobile, office automation, is in great demand.
In existing mass production techniques, the magnetic majority adopted is ferrite, although this type of ferrite bonded permanent magnet has certain antioxidant anticorrosive performance and good mechanical performance, magnetic property is lower, can not meet the application requirements such as high-performance small and special electric machine.Ndfeb magnet is the magnet finding that commercialization performance is the highest at present, is called magnetic king by people, has its maximum magnetic energy product of high magnetic property (BHmax) and exceeds more than 10 times, ferrite (Ferrite).Itself machining property is also suitable good, and operating temperature reaches as high as 200 degrees Celsius, and its quality is hard, and stable performance has good cost performance, therefore its application is extremely extensive.But because its chemism is very strong, so must to its surface coated treatment, as plating Zn, Ni, electrophoresis, passivation etc., technique be quite complicated, and manufacturing cost is higher.
Neodymium iron boron (Nd-Fe-B) material is a kind of novel third generation permanent-magnet material that domestic and international development in recent years is got up.Nd Fe B alloys chemical property is active, in process of production, often there is nature and catch fire or explosion phenomenon in its dusty material, this phenomenon even also likely occurs under low-temperature condition, have again the danger of blast when containing certain alloyed powder dust concentration in air, the normal production of safety of iron B permanent magnetic material by the emperor himself in serious threat.
In prior art, the neodymium iron boron powder of institute's production and selling, its granularity mostly is 100 ~ 200 orders, and it can meet the production of Sintered NdFeB magnet, and cannot meet the production of bonded permanent magnet, particularly can not meet the Production requirement of high-performance plastic magnetic product.Existingly mould magnetic product, all many-sides such as its pliability, impact resistance, resistance to elevated temperatures all also exist deficiency, and the product thickness produced is comparatively large, usually at more than 1mm, cannot meet the demand of the product such as micro motor, small and special electric machine.
Summary of the invention
Object of the present invention, exactly for overcoming the above-mentioned deficiency of prior art, the preparation method of the ultra-fine neodymium iron boron powder mixture of nanometer providing a kind of applicable industrialization to produce, multiple ball milling step concentrates in a ball mill and carries out by it, by the selection of the material to abrading-ball, the own loss that it is produced becomes the active ingredient of neodymium iron boron powder mixture;
The present invention also aims to, provide a kind of ultra-fine neodymium iron boron powder mixture adopting said method to prepare, it can be widely used in the manufacture that various flexibility moulds magnetic product.
For achieving the above object, technical scheme provided by the invention is:
A preparation method for ultra-fine neodymium iron boron powder mixture, is characterized in that, comprise the following steps:
(1) pretreatment of raw material:
(11) spherical sintered NdFeB magnetic patch and zirconia is prepared, as the spheroid used in ball mill;
Prepared sizes be commodity neodymium iron boron powder impurity elimination between 100 ~ 200 orders, dry after for subsequent use;
(12) covering is prepared
(121) silane coupler 80 ~ 90wt% is taken
Take diluent acetone 10 ~ 20wt%
(122) by silane coupler and diluent Homogeneous phase mixing, obtained covering;
(2) material is weighed:
Raw material is taken according to following percentage by weight:
(3) Surface coating process: under the protection of nitrogen argon gas atmosphere, neodymium iron boron powder mixture and the covering for preparing are added ball mill grinding 2 ~ 5 hours, carrying out mixed grinding makes neodymium iron boron powder mixture form cladded type particulate, namely its Surface coating has one deck covering, until each powder granularity reaches 100 ~ 300 nanometers;
(4) solid-liquid mixed grinding:
Under the protection of nitrogen argon gas atmosphere, natural rubber, metallocene polyolefin elastomers are added ball mill grinding 2 ~ 5 hours, carry out mixed grinding and make it form mixing cladded type particulate, until each powder granularity reaches 10 ~ 50 nanometers;
(5) filter, and sealed storage, obtained ultra-fine neodymium iron boron powder mixture mixture.
Spherical ndfeb magnet in described step (1), its diameter is 60 ~ 95mm; The diameter of described zirconia spheroid is 5 ~ 30mm; The weight ratio of its loading is neodymium iron boron: zirconia=3: 1.
Metallocene polyolefin elastomers in described step (2) is propylene-octene Copolymer.
Described step (3), (4), be carry out in alternating magnetic field, accelerate ball milling under magnetic stirring.
Described step (4), also comprises and ball mill and compound is evenly warmed up to 85 ~ 120 DEG C, pressurization 3 ~ 8MPa, and pressurize is to grinding end, leaves standstill and is cooled to room temperature.
The ultra-fine neodymium iron boron powder mixture adopting preceding method to prepare, is characterized in that, comprises following raw material components weight portion:
Surplus is the neodymium iron boron produced in process of lapping that comprises in finished product and Zirconium powder.
Described metallocene polyolefin elastomers is propylene-octene Copolymer.
Described rubber is one or more in natural rubber, Oppanol, silicon rubber, EP rubbers, butyl rubber.
Preparation method provided by the invention, adopts special abrading-ball, carries out sorting without the need to the impurity produced abrading-ball, and it is suitable for industrialization and produces, and in process of production, operating mode easily controls, constant product quality; Owing to have employed pretreatment of raw material and precise finiss process two step, reduce the needs of preparation process for equipment and place, and preparation speed is fast, efficiency is high; Also directly can purchase through pretreated raw material, be directly used in production; By neodymium iron boron powder and covering, rubber and metallocene polyolefin elastomers mixed grinding; adopt the gas shield of nitrogen argon gas complex protection simultaneously; powder in process of lapping can be realized avoid contacting with air; thus avoid powder to be oxidized, explode and sharply temperature rise, make process stable, efficient.
Ultra-fine neodymium iron boron powder mixture provided by the invention have employed high performance neodymium iron boron powder simultaneously, dynamical covering, the flexible rubber of product can be improved, the metallocene polyolefin elastomers of product anti-impact force and high-temperature behavior can be improved, make this mixture when being prepared as further and moulding magnetic product, thickness low (0.1mm can be reached) can be produced, pliability is good, tension resistance to compression, good springiness, magnetic behavior is remarkable, thickness be 1mm magnetic sheet after tested its magnetic energy product be 8 ~ 12MGOe, the hot strength of magnetic sheet is more than 4MPa, the high temperature of less than 200 DEG C can be tolerated and not loss of excitation.
Below in conjunction with embodiment, the present invention is further described.
Detailed description of the invention
Embodiment 1: the preparation method of ultra-fine neodymium iron boron powder mixture provided by the invention, comprises the following steps:
(1) pretreatment of raw material:
(11) spherical sintered NdFeB magnetic patch and zirconia is prepared, as the spheroid used in ball mill;
Prepared sizes be commodity neodymium iron boron powder impurity elimination between 100 ~ 200 orders, dry after for subsequent use;
(12) covering is prepared
(121) silane coupler 80 ~ 90wt% is taken
Take diluent acetone 10 ~ 20wt%
(122) by silane coupler and diluent Homogeneous phase mixing, obtained covering;
(2) material is weighed:
Raw material is taken according to following percentage by weight:
(3) Surface coating process: under the protection of nitrogen argon gas atmosphere, neodymium iron boron powder mixture and the covering for preparing are added ball mill grinding 2 ~ 5 hours, carrying out mixed grinding makes neodymium iron boron powder mixture form cladded type particulate, namely its Surface coating has one deck covering, until each powder granularity reaches 100 ~ 300 nanometers;
(4) solid-liquid mixed grinding:
Under the protection of nitrogen argon gas atmosphere, natural rubber, metallocene polyolefin elastomers are added ball mill grinding 2 ~ 5 hours, carry out mixed grinding and make it form mixing cladded type particulate, until each powder granularity reaches 10 ~ 50 nanometers;
(5) filter, and sealed storage, obtained ultra-fine neodymium iron boron powder mixture.
Spherical NbFeB sintered magnetic patch in described step (1), its diameter is 60 ~ 95mm; The diameter of described zirconia spheroid is 5 ~ 30mm; The weight ratio of its loading is neodymium iron boron: zirconia=3: 1.
Adopting the collocation of this abrading-ball, is consider that neodymium iron boron and zirconia are magnetic material, and its powder that self produces in process of lapping, can as a part for inventive mixture, and without the need to screening, reject operation again to it; Meanwhile, the density of neodymium iron boron is large and hardness is slightly low, and zirconic hardness is large and density is slightly low, the lapping mode that both employings combine, and can accelerate the grinding rate to powder various in mixture; Simultaneously, the weight ratio of its loading in ball mill is neodymium iron boron: zirconia=3: 1, and the diameter of neodymium iron boron abrading-ball is much larger than zirconia, also be consider that the content of neodymium iron boron in mix ingredients can be slightly large, zirconia needs less than normal, and neodymium iron boron density is large, grinding impulsive force is large, be suitable for the corase grind in large space, zirconia is then suitable for the fine grinding in little space, by the two is reasonably combined, work together, can greatly improve grinding efficiency and grinding precision, obtain nano level mix ingredients.
Metallocene polyolefin elastomers in described step (2) is propylene-octene Copolymer.
Described step (3), (4), be carry out in alternating magnetic field, accelerate ball milling under magnetic stirring.
Described step (4), also comprises and ball mill and compound is evenly warmed up to 85 ~ 120 DEG C, pressurization 3 ~ 8MPa, and pressurize is to grinding end, leaves standstill and is cooled to room temperature.
The ultra-fine neodymium iron boron powder mixture adopting preceding method to prepare, comprises following raw material components weight portion:
Surplus is the neodymium iron boron produced in process of lapping that comprises in finished product and Zirconium powder.
Described metallocene polyolefin elastomers is propylene-octene Copolymer.
Described rubber is one or more in natural rubber, Oppanol, silicon rubber, EP rubbers, butyl rubber.
Improving in weatherability and pliability, impact resistance, present invention employs metallocene polyolefin elastomers POE, polyene elastomer is a kind of propylene-octene Copolymer, it has superior mobility, there is the heat aging property of excellent mechanical property, processing characteristics and excellence, with metal oxide with the use of the characteristic that can get at excellent heat ageing, compressibility and resistance to sky marquis.
In heat endurance, chemical stability and mechanical stability, the present invention adopts micro-oxidation zirconium, insulate under its normal temperature, thermal conductivity is low, linear expansion coefficient is large, thermal structure intensity is high, chemical stability is good, less than 2000 DEG C inoperative to multiple motlten metal, silicate, glass etc., and solution and the zirconia of caustic alkali, carbonate and various acid (concentrated sulfuric acid and hydrofluoric acid except) are inoperative, also improve the combination property of mixture.
Process equipment used in the present invention, can use high speed ball mill, friction mill, vibrations mill, planetary mills, the devices such as micronizer, sorting unit can be micropowder sorter etc.
Mixture provided by the invention, there is thinner granularity and mobile performance, the modes such as doping micro-oxidation zirconium, metallocene polyolefin elastomers POE are adopted to obtain more superior composite performance, after tested, thickness be 1mm magnetic sheet after tested its magnetic energy product be 8 ~ 12MGOe, the hot strength of magnetic sheet is more than 4MPa, can tolerate the high temperature of less than 200 DEG C and not loss of excitation.It is the thinnest can produce the magnetic sheet that thickness is 0.1mm, and combination property is significantly superior to existing common powder magnetic sheet.
Embodiment 2: the preparation method that this enforcement provides and mixture, substantially identical with embodiment 1, its difference is:
A preparation method for ultra-fine neodymium iron boron powder mixture, comprises the following steps:
(1) pretreatment of raw material:
(11) spherical sintered NdFeB magnetic patch and zirconia is prepared, as the spheroid used in ball mill;
Prepared sizes are for subsequent use after 100 ~ 150 object commodity neodymium iron boron powder impurity eliminations, drying;
(12) covering is prepared
(121) silane coupler 80wt% is taken
Take diluent acetone 20wt%
(122) by silane coupler and diluent Homogeneous phase mixing, obtained covering;
(2) material is weighed:
Raw material is taken according to following percentage by weight:
(3) Surface coating process: under the protection of nitrogen argon gas atmosphere, neodymium iron boron powder mixture and the covering for preparing are added ball mill grinding 2 ~ 5 hours, carrying out mixed grinding makes neodymium iron boron powder mixture form cladded type particulate, namely its Surface coating has one deck covering, until each powder granularity reaches 100 ~ 200 nanometers;
(4) solid-liquid mixed grinding:
Under the protection of nitrogen argon gas atmosphere, natural rubber, metallocene polyolefin elastomers are added ball mill grinding 2 ~ 5 hours, carry out mixed grinding and make it form mixing cladded type particulate, until each powder granularity reaches 25 ~ 50 nanometers;
(5) filter, and sealed storage, obtained ultra-fine neodymium iron boron powder mixture.
Spherical NbFeB sintered magnetic patch wherein, its diameter is 60mm; The diameter of described zirconia spheroid is 5mm;
Described step (4), also comprises and ball mill and compound is evenly warmed up to 85 DEG C ~ 100 DEG C, pressurization 8MPa, and pressurize is to grinding end, leaves standstill and is cooled to room temperature.
The ultra-fine neodymium iron boron powder mixture adopting preceding method to prepare, comprises following raw material components weight portion:
Surplus is the neodymium iron boron produced in process of lapping that comprises in finished product and Zirconium powder.
Described rubber, employing be natural rubber.
Embodiment 3: the preparation method that this enforcement provides and mixture, substantially with embodiment 1,2 identical, its difference is, in the step of its preparation method:
(1) pretreatment of raw material:
(11) spherical sintered NdFeB magnetic patch and zirconia is prepared, as the spheroid used in ball mill;
Prepared sizes be commodity neodymium iron boron powder impurity elimination between 150 ~ 200 orders, dry after for subsequent use;
(12) covering is prepared
(121) silane coupler 90wt% is taken
Take diluent acetone 10wt%
(122) by silane coupler and diluent Homogeneous phase mixing, obtained covering;
(2) material is weighed:
Raw material is taken according to following percentage by weight:
(3) Surface coating process: under the protection of nitrogen argon gas atmosphere, neodymium iron boron powder mixture and the covering for preparing are added ball mill grinding 2 ~ 5 hours, carrying out mixed grinding makes neodymium iron boron powder mixture form cladded type particulate, namely its Surface coating has one deck covering, until each powder granularity reaches 200 ~ 300 nanometers;
(4) solid-liquid mixed grinding:
Under the protection of nitrogen argon gas atmosphere, natural rubber, metallocene polyolefin elastomers are added ball mill grinding 2 ~ 5 hours, carry out mixed grinding and make it form mixing cladded type particulate, until each powder granularity reaches 10 ~ 25 nanometers;
Spherical NbFeB sintered magnetic patch wherein, its diameter is 95mm; The diameter of described zirconia spheroid is 30mm;
Described step (4), also comprises and ball mill and compound is evenly warmed up to 100 ~ 120 DEG C, pressurization 3 ~ 5MPa, and pressurize is to grinding end, leaves standstill and is cooled to room temperature.
The ultra-fine neodymium iron boron powder mixture adopting preceding method to prepare, comprises following raw material components weight portion:
Surplus is the neodymium iron boron produced in process of lapping that comprises in finished product and Zirconium powder, amounts to the 1wt% accounting for finished product.
Described rubber is Oppanol.
Embodiment 4: the preparation method that this enforcement provides and mixture, substantially with embodiment 1,2,3 identical, its difference is, in the step of its preparation method:
(1) pretreatment of raw material:
(11) spherical sintered NdFeB magnetic patch and zirconia is prepared, as the spheroid used in ball mill;
Prepared sizes be commodity neodymium iron boron powder impurity elimination between 100 ~ 120 orders, dry after for subsequent use;
(12) covering is prepared
(121) silane coupler 85wt% is taken
Take diluent acetone 15wt%
(122) by silane coupler and diluent Homogeneous phase mixing, obtained covering;
(2) material is weighed:
Raw material is taken according to following percentage by weight:
(3) Surface coating process: under the protection of nitrogen argon gas atmosphere, neodymium iron boron powder mixture and the covering for preparing are added ball mill grinding 2 ~ 5 hours, carrying out mixed grinding makes neodymium iron boron powder mixture form cladded type particulate, namely its Surface coating has one deck covering, until each powder granularity reaches 100 ~ 300 nanometers;
(4) solid-liquid mixed grinding:
Under the protection of nitrogen argon gas atmosphere, natural rubber, metallocene polyolefin elastomers are added ball mill grinding 2 ~ 5 hours, carry out mixed grinding and make it form mixing cladded type particulate, until each powder granularity reaches 20 ~ 30 nanometers;
Spherical NbFeB sintered magnetic patch in described step (1), its diameter is 80mm; The diameter of described zirconia spheroid is 20mm;
Described step (4), also comprises and ball mill and compound is evenly warmed up to 95 ~ 110 DEG C, pressurization 5 ~ 6MPa, and pressurize is to grinding end, leaves standstill and is cooled to room temperature.
The ultra-fine neodymium iron boron powder mixture adopting preceding method to prepare, comprises following raw material components weight portion:
Surplus is the neodymium iron boron produced in process of lapping that comprises in finished product and Zirconium powder, about 1.5%.
Described rubber is one or more in silicon rubber, EP rubbers, butyl rubber.
The present invention is not limited to above-mentioned embodiment, and every all similar or equivalent embodiment that can realize the object of the invention, all within protection scope of the present invention.
Claims (8)
1. a preparation method for ultra-fine neodymium iron boron powder mixture, is characterized in that, comprise the following steps:
(1) pretreatment of raw material:
(11) spherical sintered NdFeB magnetic patch and zirconia is prepared, as the spheroid used in ball mill;
Prepared sizes be commodity neodymium iron boron powder impurity elimination between 100 ~ 200 orders, dry after for subsequent use;
(12) covering is prepared
(121) silane coupler 80 ~ 90wt% is taken
Take diluent acetone 10 ~ 20wt%
(122) by silane coupler and diluent Homogeneous phase mixing, obtained covering;
(2) material is weighed:
Raw material is taken according to following percentage by weight:
(3) Surface coating process: under the protection of nitrogen argon gas atmosphere, neodymium iron boron powder and the covering for preparing are added ball mill grinding 2 ~ 5 hours, carrying out mixed grinding makes Nd-Fe-B powder body form cladded type particulate, namely its Surface coating has one deck covering, until each powder granularity reaches 100 ~ 300 nanometers;
(4) solid-liquid mixed grinding:
Under the protection of nitrogen argon gas atmosphere, rubber, metallocene polyolefin elastomers are added ball mill grinding 2 ~ 5 hours, carry out mixed grinding and make it form mixing cladded type particulate, until each powder granularity reaches 10 ~ 50 nanometers;
(5) filter, and sealed storage, obtained ultra-fine neodymium iron boron powder mixture.
2. the preparation method of ultra-fine neodymium iron boron powder mixture according to claim 1, it is characterized in that, the spherical ndfeb magnet in described step (1), its diameter is 60 ~ 95mm; The diameter of described zirconia spheroid is 5 ~ 30mm; The weight ratio of its loading is neodymium iron boron: zirconia=3: 1.
3. the preparation method of ultra-fine neodymium iron boron powder mixture according to claim 1, it is characterized in that, the metallocene polyolefin elastomers in described step (2) is propylene-octene Copolymer.
4. the preparation method of ultra-fine neodymium iron boron powder mixture according to claim 1, is characterized in that described step (3), (4) are carry out in alternating magnetic field, accelerate ball milling under magnetic stirring.
5. the preparation method of ultra-fine neodymium iron boron powder mixture according to claim 1, is characterized in that, described step (4), also comprise and ball mill and compound are evenly warmed up to 85 ~ 120 DEG C, pressurization 3 ~ 8MPa, and pressurize is to grinding end, leaves standstill and is cooled to room temperature.
6. adopt a ultra-fine neodymium iron boron powder mixture prepared by the described method of one of Claims 1 to 5, it is characterized in that, comprise following raw material components weight portion:
Surplus is the neodymium iron boron produced in process of lapping that comprises in finished product and Zirconium powder.
7. ultra-fine neodymium iron boron powder mixture according to claim 6, is characterized in that, described metallocene polyolefin elastomers is propylene-octene Copolymer.
8. ultra-fine neodymium iron boron powder mixture according to claim 6, is characterized in that, described rubber, is one or more in natural rubber, Oppanol, silicon rubber, EP rubbers, butyl rubber.
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