CN102139369A - 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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- CN102139369A CN102139369A CN2010106235515A CN201010623551A CN102139369A CN 102139369 A CN102139369 A CN 102139369A CN 2010106235515 A CN2010106235515 A CN 2010106235515A CN 201010623551 A CN201010623551 A CN 201010623551A CN 102139369 A CN102139369 A CN 102139369A
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- boron powder
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- 239000000203 mixture Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 42
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title abstract description 15
- 229910052742 iron Inorganic materials 0.000 title abstract description 7
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 title abstract 6
- 229910052779 Neodymium Inorganic materials 0.000 title abstract 6
- BDDGCXUIIBADED-UHFFFAOYSA-N neodymium Chemical compound [Nd].[Nd].[Nd].[Nd] BDDGCXUIIBADED-UHFFFAOYSA-N 0.000 title abstract 5
- 238000000227 grinding Methods 0.000 claims abstract description 43
- 229920006124 polyolefin elastomer Polymers 0.000 claims abstract description 29
- 229920001971 elastomer Polymers 0.000 claims abstract description 27
- 239000005060 rubber Substances 0.000 claims abstract description 26
- 238000005303 weighing Methods 0.000 claims abstract description 26
- 239000002994 raw material Substances 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 238000003860 storage Methods 0.000 claims abstract description 5
- 229910001172 neodymium magnet Inorganic materials 0.000 claims description 83
- 239000000843 powder Substances 0.000 claims description 77
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 claims description 75
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 44
- 238000000034 method Methods 0.000 claims description 22
- 239000007789 gas Substances 0.000 claims description 14
- PWKWDCOTNGQLID-UHFFFAOYSA-N [N].[Ar] Chemical compound [N].[Ar] PWKWDCOTNGQLID-UHFFFAOYSA-N 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 12
- 239000003085 diluting agent Substances 0.000 claims description 12
- 229910000077 silane Inorganic materials 0.000 claims description 12
- 244000043261 Hevea brasiliensis Species 0.000 claims description 10
- 229920003052 natural elastomer Polymers 0.000 claims description 10
- 229920001194 natural rubber Polymers 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 7
- 229920001577 copolymer Polymers 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 7
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 6
- 230000008030 elimination Effects 0.000 claims description 6
- 238000003379 elimination reaction Methods 0.000 claims description 6
- 229920005987 OPPANOL® Polymers 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 4
- 229920005549 butyl rubber Polymers 0.000 claims description 4
- 238000011068 loading method Methods 0.000 claims description 4
- 229920002379 silicone rubber Polymers 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 3
- 240000007594 Oryza sativa Species 0.000 claims 1
- 235000007164 Oryza sativa Nutrition 0.000 claims 1
- 235000009566 rice Nutrition 0.000 claims 1
- 239000011248 coating agent Substances 0.000 abstract 3
- 229910052796 boron Inorganic materials 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 229920002457 flexible plastic Polymers 0.000 abstract 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 abstract 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 abstract 1
- 238000007789 sealing Methods 0.000 abstract 1
- 239000007787 solid Substances 0.000 abstract 1
- 229910001928 zirconium oxide Inorganic materials 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 11
- 230000018109 developmental process Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 229910052761 rare earth metal Inorganic materials 0.000 description 4
- 150000002910 rare earth metals Chemical class 0.000 description 4
- 229910000859 α-Fe Inorganic materials 0.000 description 4
- 238000003825 pressing Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 2
- 229910000521 B alloy Inorganic materials 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000003679 aging effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 238000001962 electrophoresis Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 229940074869 marquis Drugs 0.000 description 1
- 238000007567 mass-production technique Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 150000004291 polyenes Chemical class 0.000 description 1
- VBUNOIXRZNJNAD-UHFFFAOYSA-N ponazuril Chemical compound CC1=CC(N2C(N(C)C(=O)NC2=O)=O)=CC=C1OC1=CC=C(S(=O)(=O)C(F)(F)F)C=C1 VBUNOIXRZNJNAD-UHFFFAOYSA-N 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000010057 rubber processing Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Landscapes
- Hard Magnetic Materials (AREA)
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 the macromolecule compound mixture, be specifically related to a kind ofly be used to make high-performance flexible and mould the magnetic product, adopt the ultra-fine neodymium iron boron powder preparation process of mixture and the mixture of nanometer technology.
Background technology
Along with the development of society, technology rapid development such as particularly various electric automobiles, magnetic suspension train, high-performance motor, generator make that the demand of high performance magnetic product is increasing, and are also more and more higher to the characteristic requirement of product.
In the prior art, bonding rare earth magnet processing method adopts mold pressing, injection and expressing technique more, prepared magnet all is that rigidity is inelastic, and adopt mold pressing, injection molding technique more to need the mould of a large amount of different sizes, and need carry out machined to size in the later stage, be unfavorable for the change of magnet specification, processing cost is higher.Though simultaneously the rigidity magnet has higher magnetic property and certain freedom shape, when having motor application automaticity not high, assemble shortcoming such as inconvenience, and the magnet that is made into ultrathin (less than 1.0mm) has certain difficulty.
The flexible bonding rare-earth magnet is a kind of new product of bonding rare earth magnet, be different from the rigidity bonding rare earth magnet that injection moulding and mould pressing process are produced, with rubber is binding agent, the employing rubber processing is produced, do not need that but a large amount of mould development expenses, production efficiency height free bend do not ftracture, product size can change arbitrarily, thickness can less than 1 millimeter, be convenient to the client and assemble use, satisfied small and special electric machine to small-sized, ultra-thin, at a high speed, the requirement that develops of high accuracy and low noise direction, market prospects are good.The flexible adhesion permanent magnet has been widely used in fields such as household electrical appliances, automobile, office automation, is in great demand.
In the existing mass production techniques, the magnetic that is adopted is most to be ferrite, though this type of ferrite bonded permanent magnet has certain antioxidant anticorrosive performance and mechanical performance preferably, magnetic property is lower, can not satisfy application requirements such as high-performance small and special electric machine.Ndfeb magnet is to find the highest magnet of commercialization performance at present, is called the magnetic king by people, has its maximum magnetic energy product of high magnetic property (BHmax) and exceeds ferrite (Ferrite) more than 10 times.Also suitable good of the machining property of itself, operating temperature reaches as high as 200 degrees centigrade, and its quality is hard, and stable performance has good cost performance, so its application is extremely extensive.But because its chemism is very strong, thus must handle its face coat, as plating Zn, Ni, electrophoresis, passivation etc., technology is 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.The Nd Fe B alloys chemical property is active, in process of production, its dusty material often takes place that nature catches fire or explosion phenomenon, this phenomenon even under low-temperature condition, also might take place, the danger of blast is arranged again when containing certain alloyed powder dust concentration in the air, and the safe ordinary production of iron B permanent magnetic material by the emperor himself in serious threat.
In the prior art, the neodymium iron boron powder of institute's production and selling, its granularity mostly is 100～200 orders, and it can satisfy the production of Sintered NdFeB magnet, and can't satisfy the production of bonded permanent magnet, particularly can not satisfy the production demand of high-performance plastic magnetic product.The existing magnetic product of moulding, all many-sides such as its pliability, impact resistance, resistance to elevated temperatures all exist deficiency, and the product thickness of being produced is bigger, more than 1mm, can't satisfy the demand of products such as micro motor, small and special electric machine usually.
Summary of the invention
Purpose of the present invention, exactly for overcoming the above-mentioned deficiency of prior art, the ultra-fine neodymium iron boron powder of the nanometer preparation process of mixture that provides a kind of suitable industrialization to produce, it concentrates on a plurality of ball milling steps in the ball mill and carries out, selection by to the material of abrading-ball makes the own loss of its generation become the active ingredient of neodymium iron boron powder mixture;
The present invention also aims to, a kind of ultra-fine neodymium iron boron powder mixture that adopts method for preparing is provided, it can be widely used in the manufacturing that various flexibilities are moulded the magnetic product.
For achieving the above object, technical scheme provided by the invention is:
A kind of ultra-fine neodymium iron boron powder preparation process of mixture is characterized in that, may further comprise the steps:
(1) pretreatment of raw material:
(11) spherical sintered NdFeB magnetic patch and the zirconia of preparation is as the spheroid that uses in the ball mill;
Prepared sizes are that the commodity neodymium iron boron powder impurity elimination between 100～200 orders, dry back are standby;
(12) preparation covering
(121) take by weighing silane coupler 80～90wt%
Take by weighing diluent acetone 10～20wt%
(122) silane coupler is evenly mixed with diluent, make covering;
(2) weighing material:
Take by weighing raw material according to following percentage by weight:
Neodymium iron boron powder 88～97wt%
Metallocene polyolefin elastomers 0～5wt% (propylene)
Rubber 1～5wt%
Covering 1～2wt%
(3) surface coats and handles: the protection of nitrogen argon gas atmosphere down, neodymium iron boron powder mixture and the covering for preparing were added ball mill grinding 2～5 hours, carrying out mixed grinding makes neodymium iron boron powder mixture form the cladded type particulate, be that its surface is coated with one deck covering, reach 100～300 nanometers until each powder granularity;
(4) solid-liquid mixed grinding:
The protection of nitrogen argon gas atmosphere added ball mill grinding 2～5 hours with natural rubber, metallocene polyolefin elastomers down, carried out mixed grinding and made it form mixing cladded type particulate, reached 10～50 nanometers until each powder granularity;
(5) filter, and sealed storage, make ultra-fine neodymium iron boron powder mixture mixture.
Spherical ndfeb magnet in the described step (1), its diameter are 60～95mm; The diameter of described zirconia spheroid is 5～30mm; The weight ratio of its loading is a neodymium iron boron: zirconia=3: 1.
Metallocene polyolefin elastomers in the described step (2) is propylene-octene copolymer.
Described step (4), (5) are to carry out in alternating magnetic field, quicken ball milling under magnetic agitation.
Described step (4) also comprises ball mill and compound evenly are warmed up to 85～120 ℃, pressurization 3～8MPa, and pressurize is left standstill and is cooled to room temperature to grinding end.
A kind of ultra-fine neodymium iron boron powder mixture that adopts the preceding method preparation is characterized in that, comprises following raw material components weight portion:
Neodymium iron boron powder 87～97wt%
Metallocene polyolefin elastomers 0～5wt%
Rubber 1～5wt%
Covering 1～2wt%
Surplus is neodymium iron boron that produces in process of lapping and the Zirconium powder that is comprised in the finished product.
Described metallocene polyolefin elastomers is propylene-octene copolymer.
Described rubber is in natural rubber, Oppanol, silicon rubber, EP rubbers, the butyl rubber one or more.
Preparation method provided by the invention adopts special abrading-ball, need not the impurity that abrading-ball produces is carried out sorting, and it is suitable for the industrialization generation, and in process of production, operating mode is controlled easily, constant product quality; Owing to adopted pretreatment of raw material and precise finiss to handle for two steps, reduced the needs of preparation process, and preparation speed be fast, efficient is high for equipment and place; Also can directly purchase through pretreated raw material, be directly used in production; With neodymium iron boron powder and covering, rubber and metallocene polyolefin elastomers mixed grinding; adopt the gas shield of nitrogen argon gas complex protection simultaneously; can realize that powder is avoided contacting with air in the process of lapping; thereby avoid powder generation oxidation, blast and rapid temperature rise, make process stable, efficient.
Ultra-fine neodymium iron boron powder mixture provided by the invention has adopted high performance neodymium iron boron powder simultaneously, dynamical covering, can improve the flexible rubber of product, can improve the metallocene polyolefin elastomers of product anti-impact force and high-temperature behavior, make this mixture further be prepared as mould the magnetic product in, can produce thickness low (can reach 0.1mm), pliability is good, the 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 the 4MPa, can tolerate high temperature below 200 ℃ and loss of excitation not.
The present invention is further described below in conjunction with embodiment.
The specific embodiment
Embodiment 1: ultra-fine neodymium iron boron powder preparation process of mixture provided by the invention may further comprise the steps:
(1) pretreatment of raw material:
(11) spherical sintered NdFeB magnetic patch and the zirconia of preparation is as the spheroid that uses in the ball mill;
Prepared sizes are that the commodity neodymium iron boron powder impurity elimination between 100～200 orders, dry back are standby;
(12) preparation covering
(121) take by weighing silane coupler 80～90wt%
Take by weighing diluent acetone 10～20wt%
(122) silane coupler is evenly mixed with diluent, make covering;
(2) weighing material:
Take by weighing raw material according to following percentage by weight:
Neodymium iron boron powder 88～97wt%
Metallocene polyolefin elastomers 0～5wt% (propylene)
Rubber 1～5wt%
Covering 1～2wt%
(3) surface coats and handles: the protection of nitrogen argon gas atmosphere down, neodymium iron boron powder mixture and the covering for preparing were added ball mill grinding 2～5 hours, carrying out mixed grinding makes neodymium iron boron powder mixture form the cladded type particulate, be that its surface is coated with one deck covering, reach 100～300 nanometers until each powder granularity;
(4) solid-liquid mixed grinding:
The protection of nitrogen argon gas atmosphere added ball mill grinding 2～5 hours with natural rubber, metallocene polyolefin elastomers down, carried out mixed grinding and made it form mixing cladded type particulate, reached 10～50 nanometers until each powder granularity;
(5) filter, and sealed storage, make ultra-fine neodymium iron boron powder mixture.
Spherical NbFeB sintered magnetic patch in the described step (1), its diameter are 60～95mm; The diameter of described zirconia spheroid is 5～30mm; The weight ratio of its loading is a neodymium iron boron: zirconia=3: 1.
Adopting the collocation of this abrading-ball, is to consider that neodymium iron boron and zirconia are magnetic material, and the powder that it self produces in process of lapping can be used as the part of mixture of the present invention, and need not again it to be screened, reject operation; Simultaneously, the density of neodymium iron boron is big and hardness is low slightly, and zirconic hardness is big and density is low slightly, adopts the lapping mode of the two combination, can accelerate the grinding rate to various powders in the mixture; Simultaneously, the weight ratio of its loading in ball mill is a neodymium iron boron: zirconia=3: 1, and the diameter of neodymium iron boron abrading-ball is much larger than zirconia, also be to consider that the content of neodymium iron boron in the mix ingredients can be big slightly, zirconia needs less than normal, and neodymium iron boron density is big, the grinding impulsive force is big, be suitable for the corase grind in large space, zirconia then is suitable for the correct grinding in the little space, by the two is reasonably combined, work together, can improve grinding efficiency and grinding precision greatly, obtain nano level mix ingredients.
Metallocene polyolefin elastomers in the described step (2) is propylene-octene copolymer.
Described step (4), (5) are to carry out in alternating magnetic field, quicken ball milling under magnetic agitation.
Described step (4) also comprises ball mill and compound evenly are warmed up to 85～120 ℃, pressurization 3～8MPa, and pressurize is left standstill and is cooled to room temperature to grinding end.
Adopt the ultra-fine neodymium iron boron powder mixture of preceding method preparation, comprise following raw material components weight portion:
Neodymium iron boron powder 87～88wt%
Metallocene polyolefin elastomers 0～5wt%
Rubber 1～5wt%
Covering 1～2wt%
Surplus is neodymium iron boron that produces in process of lapping and the Zirconium powder that is comprised in the finished product.
Described metallocene polyolefin elastomers is propylene-octene copolymer.
Described rubber is in natural rubber, Oppanol, silicon rubber, EP rubbers, the butyl rubber one or more.
Improving aspect weatherability and pliability, the impact resistance, the present invention has adopted metallocene polyolefin elastomers POE, the polyene elastomer is a kind of propylene-octene copolymer, it has superior flowability, have excellent mechanical property, processing characteristics and excellent heat aging property, be used the characteristic that can get at good heat ageing, compressibility and anti-day marquis with metal oxide.
Aspect heat endurance, chemical stability and mechanical stability, the present invention adopts micro-zirconia, its normal temperature insulate down, thermal conductivity is low, linear expansion coefficient is big, thermal structure intensity height, chemical stability is good, inoperative to multiple motlten metal, silicate, glass etc. below 2000 ℃, the solution and the zirconia of caustic alkali, carbonate and various acid (concentrated sulfuric acid and except for hydrofluoric acid) are inoperative, have also improved the combination property of mixture.
Process equipment used in the present invention can use high speed ball mill, friction mill, vibrations mill, planetary mills, and devices such as micronizer, sorting unit can be for the micro mist separators etc.
Mixture provided by the invention, have thinner granularity and mobile performance, adopt the modes such as micro-zirconia, metallocene polyolefin elastomers POE of mixing 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 the 4MPa, can tolerate high temperature below 200 ℃ and loss of excitation not.It is the thinnest can produce the magnetic sheet that thickness is 0.1mm, and combination property significantly is superior to existing common powder magnetic sheet.
Embodiment 2: preparation method that this enforcement provides and mixture, and identical with embodiment 1 basically, its difference is:
A kind of ultra-fine neodymium iron boron powder preparation process of mixture may further comprise the steps:
(1) pretreatment of raw material:
(11) spherical sintered NdFeB magnetic patch and the zirconia of preparation is as the spheroid that uses in the ball mill;
Prepared sizes are that 100～150 purpose commodity neodymium iron boron powder impurity eliminations, dry back are standby;
(12) preparation covering
(121) take by weighing silane coupler 80wt%
Take by weighing diluent acetone 20wt%
(122) silane coupler is evenly mixed with diluent, make covering;
(2) weighing material:
Take by weighing raw material according to following percentage by weight:
Neodymium iron boron powder 87wt%
Metallocene polyolefin elastomers 5wt%
Rubber 5wt%
Covering 2wt%
(3) surface coats and handles: the protection of nitrogen argon gas atmosphere down, neodymium iron boron powder mixture and the covering for preparing were added ball mill grinding 2～5 hours, carrying out mixed grinding makes neodymium iron boron powder mixture form the cladded type particulate, be that its surface is coated with one deck covering, reach 100～200 nanometers until each powder granularity;
(4) solid-liquid mixed grinding:
The protection of nitrogen argon gas atmosphere added ball mill grinding 2～5 hours with natural rubber, metallocene polyolefin elastomers down, carried out mixed grinding and made it form mixing cladded type particulate, reached 25～50 nanometers until each powder granularity;
(5) filter, and sealed storage, make ultra-fine neodymium iron boron powder mixture.
Spherical NbFeB sintered magnetic patch wherein, its diameter are 60mm; The diameter of described zirconia spheroid is 5mm;
Described step (4) also comprises ball mill and compound evenly are warmed up to 85 ℃～100 ℃, pressurization 8MPa, and pressurize is left standstill and is cooled to room temperature to grinding end.
A kind of ultra-fine neodymium iron boron powder mixture that adopts the preceding method preparation comprises following raw material components weight portion:
Neodymium iron boron powder 87wt%
Metallocene polyolefin elastomers 5wt%
Rubber 5wt%
Covering 2wt%
Surplus is neodymium iron boron that produces in process of lapping and the Zirconium powder that is comprised in the finished product.
Described rubber, employing be natural rubber.
Embodiment 3: preparation method that this enforcement provides and mixture, and identical with embodiment 1,2 basically, its difference is, in the step of its preparation method:
(1) pretreatment of raw material:
(11) spherical sintered NdFeB magnetic patch and the zirconia of preparation is as the spheroid that uses in the ball mill;
Prepared sizes are that the commodity neodymium iron boron powder impurity elimination between 150～200 orders, dry back are standby;
(12) preparation covering
(121) take by weighing silane coupler 90wt%
Take by weighing diluent acetone 10wt%
(122) silane coupler is evenly mixed with diluent, make covering;
(2) weighing material:
Take by weighing raw material according to following percentage by weight:
Neodymium iron boron powder 97wt%
Metallocene polyolefin elastomers 0%
Rubber 1wt%
Covering 1wt%
(3) surface coats and handles: the protection of nitrogen argon gas atmosphere down, neodymium iron boron powder mixture and the covering for preparing were added ball mill grinding 2～5 hours, carrying out mixed grinding makes neodymium iron boron powder mixture form the cladded type particulate, be that its surface is coated with one deck covering, reach 200～300 nanometers until each powder granularity;
(4) solid-liquid mixed grinding:
The protection of nitrogen argon gas atmosphere added ball mill grinding 2～5 hours with natural rubber, metallocene polyolefin elastomers down, carried out mixed grinding and made it form mixing cladded type particulate, reached 10～25 nanometers until each powder granularity;
Spherical NbFeB sintered magnetic patch wherein, its diameter are 95mm; The diameter of described zirconia spheroid is 30mm;
Described step (4) also comprises ball mill and compound evenly are warmed up to 100～120 ℃, pressurization 3～5MPa, and pressurize is left standstill and is cooled to room temperature to grinding end.
Adopt the ultra-fine neodymium iron boron powder mixture of preceding method preparation, comprise following raw material components weight portion:
Neodymium iron boron powder 97wt%
Metallocene polyolefin elastomers 0wt%
Rubber 1wt%
Covering 1wt%
Surplus is neodymium iron boron that produces in process of lapping and the Zirconium powder that is comprised in the finished product, amounts to the 1wt% that accounts for finished product.
Described rubber is Oppanol.
Embodiment 4: preparation method that this enforcement provides and mixture, and identical with embodiment 1,2,3 basically, its difference is, in the step of its preparation method:
(1) pretreatment of raw material:
(11) spherical sintered NdFeB magnetic patch and the zirconia of preparation is as the spheroid that uses in the ball mill;
Prepared sizes are that the commodity neodymium iron boron powder impurity elimination between 100～120 orders, dry back are standby;
(12) preparation covering
(121) take by weighing silane coupler 850wt%
Take by weighing diluent acetone 15wt%
(122) silane coupler is evenly mixed with diluent, make covering;
(2) weighing material:
Take by weighing raw material according to following percentage by weight:
Neodymium iron boron powder 90wt%
Metallocene polyolefin elastomers 5wt%
Rubber 2wt%
Covering 1.5wt%
(3) surface coats and handles: the protection of nitrogen argon gas atmosphere down, neodymium iron boron powder mixture and the covering for preparing were added ball mill grinding 2～5 hours, carrying out mixed grinding makes neodymium iron boron powder mixture form the cladded type particulate, be that its surface is coated with one deck covering, reach 100～300 nanometers until each powder granularity;
(4) solid-liquid mixed grinding:
The protection of nitrogen argon gas atmosphere added ball mill grinding 2～5 hours with natural rubber, metallocene polyolefin elastomers down, carried out mixed grinding and made it form mixing cladded type particulate, reached 20～30 nanometers until each powder granularity;
Spherical NbFeB sintered magnetic patch in the described step (1), its diameter are 80mm; The diameter of described zirconia spheroid is 20mm;
Described step (4) also comprises ball mill and compound evenly are warmed up to 95～110 ℃, pressurization 5～6MPa, and pressurize is left standstill and is cooled to room temperature to grinding end.
Adopt the ultra-fine neodymium iron boron powder mixture of preceding method preparation, comprise following raw material components weight portion:
Neodymium iron boron powder 90wt%
Metallocene polyolefin elastomers 5wt%
Rubber 2wt%
Covering 1.5wt%
Surplus is neodymium iron boron that produces in process of lapping and the Zirconium powder that is comprised in the finished product, about 1.5%.
Described rubber is in silicon rubber, EP rubbers, the butyl rubber one or more.
The present invention is not limited to above-mentioned embodiment, and every all similar or the be equal to embodiments that can realize the object of the invention are all within protection scope of the present invention.
Claims (8)
1. a ultra-fine neodymium iron boron powder preparation process of mixture is characterized in that, may further comprise the steps:
(1) pretreatment of raw material:
(11) spherical sintered NdFeB magnetic patch and the zirconia of preparation is as the spheroid that uses in the ball mill;
Prepared sizes are that the commodity neodymium iron boron powder impurity elimination between 100～200 orders, dry back are standby;
(12) preparation covering
(121) take by weighing silane coupler 80～90wt%
Take by weighing diluent acetone 10～20wt%
(122) silane coupler is evenly mixed with diluent, make covering;
(2) weighing material:
Take by weighing raw material according to following percentage by weight:
Neodymium iron boron powder 88～97wt%
Metallocene polyolefin elastomers 0～5wt%
Rubber 1～5wt%
Covering 1～2wt%
(3) surface coats and handles: the protection of nitrogen argon gas atmosphere down, neodymium iron boron powder mixture and the covering for preparing were added ball mill grinding 2～5 hours, carrying out mixed grinding makes neodymium iron boron powder mixture form the cladded type particulate, be that its surface is coated with one deck covering, reach 100～300 nanometers until each powder granularity;
(4) solid-liquid mixed grinding:
The protection of nitrogen argon gas atmosphere added ball mill grinding 2～5 hours with natural rubber, metallocene polyolefin elastomers down, carried out mixed grinding and made it form mixing cladded type particulate, reached rice in 10～50 until each powder granularity;
(5) filter, and sealed storage, make ultra-fine neodymium iron boron powder mixture.
2. according to the described ultra-fine neodymium iron boron powder preparation process of mixture of claim 1, it is characterized in that the spherical ndfeb magnet in the described step (1), its diameter are 60～95mm; The diameter of described zirconia spheroid is 5～30mm; The weight ratio of its loading is a neodymium iron boron: zirconia=3: 1.
3. according to the described ultra-fine neodymium iron boron powder preparation process of mixture of claim 1, it is characterized in that the metallocene polyolefin elastomers in the described step (2) is propylene-octene copolymer.
4. according to the described ultra-fine neodymium iron boron powder preparation process of mixture of claim 1, it is characterized in that described step (4), (5) are to carry out, and quicken ball milling under magnetic agitation in alternating magnetic field.
5. according to the described ultra-fine neodymium iron boron powder preparation process of mixture of claim 1, it is characterized in that described step (4), also comprise ball mill and compound evenly are warmed up to 85～120 ℃, pressurization 3～8MPa, and pressurize is left standstill and is cooled to room temperature to grinding end.
6. a ultra-fine neodymium iron boron powder mixture that adopts the described method preparation of one of claim 1～5 is characterized in that, comprises following raw material components weight portion:
Neodymium iron boron powder 87～97wt%
Metallocene polyolefin elastomers 0～5wt%
Rubber 1～5wt%
Covering 1～2wt%
Surplus is neodymium iron boron that produces in process of lapping and the Zirconium powder that is comprised in the finished product.
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 in natural rubber, Oppanol, silicon rubber, EP rubbers, the butyl rubber one or more.
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| CN107540902A (en) * | 2017-09-13 | 2018-01-05 | 扬州大学 | A kind of preparation method of flexible neodymium iron boron rubber magnet composite |
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| CN102139369B (en) | 2015-07-08 |
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