CN102554240A - Preparation method for bonded neodymium iron boron permanent magnet granular material - Google Patents
Preparation method for bonded neodymium iron boron permanent magnet granular material Download PDFInfo
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- CN102554240A CN102554240A CN2010106169369A CN201010616936A CN102554240A CN 102554240 A CN102554240 A CN 102554240A CN 2010106169369 A CN2010106169369 A CN 2010106169369A CN 201010616936 A CN201010616936 A CN 201010616936A CN 102554240 A CN102554240 A CN 102554240A
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Abstract
The invention discloses a preparation method for a bonded neodymium iron boron permanent magnet granular material suitable for processes of injection molding and extrusion molding. First, rapid-quenching neodymium iron boron permanent magnetic powder is treated by coupling, then, 85-95wt% of neodymium iron boron magnetic powder after coupling treatment, 2-14 wt% of thermoplastic resin, 1-5wt% of metal antioxidant and 0-2wt% of other processing additives are fully mixed in a high-speed mixer, the evenly mixed magnetic power mixture is simultaneously filled with a protective gas by means of a same-direction meshing parallel double-screw muller for mulling at a certain temperature and then cut into the granular material after cooling. The preparation method effectively resolves the problems that metal magnetic powder is prone to oxidation and loss of magnetic powder coercive force is large during a conventional high-temperature mulling process and effectively improves magnetic performance of a magnetic body.
Description
Technical field
The present invention relates to a kind of preparation method of boned neodymium iron boron permanent magnet particulate material, refer to a kind of preparation method who is suitable for the Agglutinate neodymium-iron-boron permanent magnetism powder particles material of injection moulding or extrusion molding explained hereafter especially.
Background technology
Boned neodymium iron boron permanent magnet has and has excellent magnetic characteristics, and advantages such as dimensional accuracy is high, freedom shape is big, mechanical strength good, automated production continuously in enormous quantities, properties of product high conformity are widely used in computer hard disc; CD-ROM drive; Game machine, printer, automobile micro machine; In the Magnetic Sensor, be indispensable functional device in the said equipment.
The production technology of boned neodymium iron boron permanent magnet mainly contains compression molding, injection moulding, extrusion molding, four kinds of calendaring moldings etc.Injection moulding bonded permanent magnet production technology is that process is broken, and the fast quenching NdFeB permanet magnetic powder of classification mixes with biaxial mixing machine under the temperature that is higher than the binding resin fusing point with after a certain proportion of binding resin and processing aid mix; Granulation is cut off in cooling then; To pass through the particulate material that forms after the granulation puts in the injector; Be heated to uniform temperature and make the particulate material fusion, be injected in the die cavity through an aperture with the magnetic material of screw rod with fusion, magnetic is squeezed into required form in die cavity; And in die cavity, cool off and curing, obtain the Agglutinate neodymium-iron-boron magnet of required size and shape.
Extrusion molding technology and injection molding process are similar; All need use particulate material in process of production through forming behind the biaxial mixing; The composition of particulate material; The size of particle, uniformity coefficient etc. all can have influence on the properties of product of final shaping, so this granulation process is one of critical process of above-mentioned two kinds of production technologies.Yet in the granulation process of reality, owing to there is high-temperature heating process, coat not sternly so occur binding agent and magnetic easily, magnetic is prone to oxidation, and the coercivity of magnetic loses phenomenons such as big, has a strong impact on the quality of final products.
The preparation method of a Chinese invention patent ZL200710066788.4 NdFeB/PPS injection moulding particle material; The production method of a kind of PPS resin as the injection moulding particle material of binding agent proposed, at first will be O.5～dissolving of 2 mass parts coupling agents usefulness alcohol, add 100 mass parts NdFeB magnetics then; Mixing; Dry under 40～60 ℃ then, grind broken, screening, acquisition coupling NdFeB magnetic; Be dissolved in the polyvinyl alcohol of mass parts O.5～2 and form clear solution in the deionized water, in solution, add a certain proportion of coupling NdFeB magnetic and PPS resin, mix, fully dry cooling, take out grind broken, sieve and process particulate material; Particulate material is mixing, pelletizing obtains the NdFeB/PPS injection moulding particle material.
The particulate material that this invention is produced has solved the problem of evenly mixing of NdFeB magnetic and PPS resin, but the mix problem of oxidation of the NdFeB magnetic that takes place in the process of high temperature is not effectively solved, and the particulate material coercivity that utilizes this method to produce simultaneously loses bigger.
Summary of the invention
Mix and metal powder takes place in the process be prone to oxidation in order to solve high temperature, the problem that the loss of magnetic coercivity is big the invention provides a kind of injection moulding that is suitable for, the production method of the boned neodymium iron boron permanent magnet particulate material that extrusion molding technology is used.
Production method of the present invention comprises the steps.
Step 1: coupling processing: get 0.2～1 mass parts coupling agent, to use be that the absolute ethyl alcohol of 2～10 mass parts stirs coupling agent is fully dissolved; The fast quenching NdFeB permanet magnetic powder of solution and 20～100 mass parts in low speed mixer; Stir; Then NdFeB magnetic powder is after treatment carried out drying under 50 ℃～60 ℃ temperature, more above-mentioned block NdFeB magnetic powder through coupling processing is pulverized after the cooling.
Step 2: mixed processing: the NdFeB magnetic powder 85～95wt%, thermoplastic resin 2～14 wt%, metal antioxidant 1～5 wt% and other processing additives 0～2wt% that get after step 1 coupling processing fully mix at high-speed mixer.
Step 3: the processing of mixing: will pass through the magnetic mixture after step 2 is handled, and in the muller that meshes parallel double-screw in the same way, mix.
Step 4: granulation: cut into particulate material after the magnetic amalgam cooling after will mixing.
Wherein, in the step 3, the magnetic mixture mixes having under the protective atmosphere.
Of the present inventionly further be improved to: in the step 1, coupling agent, absolute ethyl alcohol, the three's of magnetic weight ratio is 1:10:100.
Of the present inventionly further be improved to: in the step 1, described coupling agent is silane coupler or titanate coupling agent.
Of the present inventionly further be improved to: in the step 2; Described thermoplastic resin is nylon or PPS; Described metal antioxidant is the mixture of phenols antioxidant or phenols antioxidant and phosphorous acid esters antioxidant, and described processing aid is plasticizer and lubricant.
Of the present inventionly further be improved to: described plasticizer is a phthalate compound, and described lubricant is silicone oil or wax liquid.
Of the present inventionly further be improved to: in the step 3, described protective atmosphere is a nitrogen.
Of the present inventionly further be improved to: in the step 3, when thermoplastic resin was nylon, melting temperature was between 200 ℃～300 ℃, and thermoplastic resin is between 290 ℃～350 ℃ of the temperature of mixing of PPS.
Of the present inventionly further be improved to:, the size of the particulate material after step 4 cutting is φ 3.5～4.5mm, length 2～4mm.
Of the present inventionly further be improved to:, in the step 1, described Agglutinate neodymium-iron-boron permanent magnetism powder is the fast quenching NdFeB permanet magnetic powder.
Of the present inventionly further be improved to: the iHc of described boned neodymium iron boron permanent magnet particulate material is 9200 Oe～9600 Oe.
The manufacturing approach of Agglutinate neodymium-iron-boron magnet particulate material of the present invention charges into protective gas when high temperature mixes, solved the technical barrier of magnetic easy oxidation in high temperature mixes process; Traditional technology of mixing; The iHc of particulate material generally at 8500 Oe～9300 Oe, mixes in protective atmosphere, and the iHc of particulate material is 9200 Oe～9600 Oe; Reduce the coercivity loss of magnetic to a great extent, efficiently solved the technical barrier that exists in the prior art.
The specific embodiment
In order to make those skilled in the art understand spirit of the present invention clearer, accurately, elaborate below in conjunction with the specific embodiment specific embodiments of the invention.
Preparation method of the present invention comprises the steps:
Step 1: coupling processing: get 0.5～1 mass parts coupling agent, to use be that the absolute ethyl alcohol of 5～10 mass parts stirs coupling agent is fully dissolved; In low speed mixer, stir the fast quenching NdFeB permanet magnetic powder of solution and 50～100 mass parts, generally speaking, coupling agent, absolute ethyl alcohol, when the three's of magnetic weight ratio was the ratio of 1:10:100, effect was best.Then NdFeB magnetic powder is after treatment carried out drying under 50 ℃～60 ℃ temperature, more above-mentioned block NdFeB magnetic powder through coupling processing is pulverized after the cooling.
Coupling agent is silane coupler or titanate coupling agent among the present invention, in specific embodiment of the present invention, adopts the KH550 silane coupler.
Described Agglutinate neodymium-iron-boron permanent magnetism powder is the fast quenching NdFeB permanet magnetic powder, the fast quenching NdFeB permanet magnetic powder that the specific embodiment of the invention all uses MQI to produce, and granularity preferably is distributed between 10 μ m～100 μ m.
Step 2: mixed processing: the NdFeB magnetic powder 85～95wt%, thermoplastic resin 2～14 wt%, metal antioxidant 1～5 wt% and other processing additives 0～2wt% that get after step 1 coupling processing fully mix at high-speed mixer; General incorporation time 10 min～15min reach mixed uniformly effect and get final product.
Described thermoplastic resin is nylon or PPS; Described metal antioxidant is the mixture of phenols antioxidant or phenols antioxidant and phosphorous acid esters antioxidant; Said anti-oxidant is that phenolic compound can be selected IRGANOX1010, IRGANOX1098 and IRGANOX245 for use, and described phenolic compound and phosphite antioxidant blend are IRGANOX B225 and IRGANOX B1171.Described processing aid is plasticizer and lubricant.Among the present invention, plasticizer is a phthalate compound, like dibutyl phthalate; The phthalic acid n-octyl, the different monooctyl ester of phthalic acid, diisooctyl phthalate; Diisononyl phthalate and diisooctyl phthalate etc., lubricant are silicone oil or wax liquid.
Step 3: the processing of mixing: will pass through the magnetic mixture after step 2 is handled, and in the muller that meshes parallel double-screw in the same way, mix.Among the present invention,, charge into protectiveness gas gas to prevent the oxidation at high temperature of magnetic mixture in the operation of mixing.In a concrete embodiment, protective gas is a nitrogen.
Temperature when mixing should be so that resin fully be molten into suitable.According to the variety classes of resin, select the suitable temperature of mixing.When thermoplastic resin was nylon, melting temperature was between 200 ℃～300 ℃, and thermoplastic resin is between 290 ℃～350 ℃ of the temperature of mixing of PPS.
Step 4: granulation: cut into size after the magnetic amalgam cooling after will mixing and be φ 3.5～4.5mm, the particulate material of length 2～4mm.
Through the boned neodymium iron boron permanent magnet particulate material that said method obtains, its intrinsic coercivity iHc is 9200 Oe～9600 Oe.
The manufacturing approach of Agglutinate neodymium-iron-boron magnet particulate material of the present invention;, high temperature charges into protective gas when mixing; Efficiently solve the technical barrier of magnetic easy oxidation in high temperature mixes process, the coercivity of magnetic loss simultaneously is little, efficiently solves the technical barrier that exists in the prior art.
Embodiment 1:
The NdFeB permanet magnetic powder 10kg of the coupling processing of learning from else's experience, nylon 12 quality are 890g, metal antioxidant 167g; Plasticizer 30g, wax liquid 25g mixes through meshing parallel double-screw in the same way; The process of mixing charges into nitrogen protection, and 250 ℃ of the temperature of mixing cut into size after the magnetic amalgam cooling after will mixing and are φ 3.5mm; The particulate material of length 2.5mm, the intrinsic coercivity iHc of particulate material is 9415 Oe.
Embodiment 2:
The NdFeB permanet magnetic powder 10kg of the coupling processing of learning from else's experience, nylon 6 quality 1646g, metal antioxidant 118g; Plasticizer 15g, silicone oil 10g mixes through meshing parallel double-screw in the same way; The process of mixing charges into nitrogen protection, and 280 ℃ of the temperature of mixing cut into size after the magnetic amalgam cooling after will mixing and are φ 3.5mm; The particulate material of length 3.5mm, the intrinsic coercivity iHc of particulate material is 9200 Oe.
Embodiment 3:
The NdFeB permanet magnetic powder 10kg of the coupling processing of learning from else's experience, nylon 612 quality 1150g, metal antioxidant 287g; Plasticizer 30g, wax liquid 27g mixes through meshing parallel double-screw in the same way; The process of mixing charges into nitrogen protection, and 220 ℃ of the temperature of mixing cut into size after the magnetic amalgam cooling after will mixing and are φ 3.5mm; The particulate material of length 2.5mm, the intrinsic coercivity iHc of particulate material is 9600 Oe.
Embodiment 4:
The NdFeB permanet magnetic powder 10kg of the coupling processing of learning from else's experience, NYLON610 quality 940g, metal antioxidant 588g; Plasticizer 100g, wax liquid 135g mixes through meshing parallel double-screw in the same way; The process of mixing charges into nitrogen protection, and 290 ℃ of the temperature of mixing cut into size after the magnetic amalgam cooling after will mixing and are φ 3.5mm; The particulate material of length 2.5mm, the intrinsic coercivity iHc of particulate material is 9300 Oe.
Embodiment 5:
The NdFeB permanet magnetic powder 10kg of the coupling processing of learning from else's experience, NYLON610 quality 900g, metal antioxidant 112g; Plasticizer 25g, silicone oil 25g mixes through meshing parallel double-screw in the same way; The process of mixing charges into nitrogen protection, and 200 ℃ of the temperature of mixing cut into size after the magnetic amalgam cooling after will mixing and are φ 3.5mm; The particulate material of length 2.5mm, the intrinsic coercivity iHc of particulate material is 9520 Oe.
Embodiment 6:
The NdFeB permanet magnetic powder 10kg of the coupling processing of learning from else's experience, the quality 540g of PPS, metal antioxidant 217g; Plasticizer 50g, wax liquid 59g mixes through meshing parallel double-screw in the same way; The process of mixing charges into nitrogen protection, and 320 ℃ of the temperature of mixing cut into size after the magnetic amalgam cooling after will mixing and are φ 3.5mm; The particulate material of length 2.5mm, the intrinsic coercivity iHc of particulate material is 9315 Oe.
Embodiment 7:
The NdFeB permanet magnetic powder 10kg of the coupling processing of learning from else's experience, the quality 316g of PPS, metal antioxidant 210g; Plasticizer 10g, silicone oil 15g mixes through meshing parallel double-screw in the same way; The process of mixing charges into nitrogen protection, and 350 ℃ of the temperature of mixing cut into size after the magnetic amalgam cooling after will mixing and are φ 3.5mm; The particulate material of length 2.5mm, the intrinsic coercivity iHc of particulate material is 9200 Oe.
Embodiment 8:
The NdFeB permanet magnetic powder 10kg of the coupling processing of learning from else's experience, the quality 538g of PPS, metal antioxidant 161g; Plasticizer 20g, wax liquid 34g mixes through meshing parallel double-screw in the same way; The process of mixing charges into nitrogen protection, and 290 ℃ of the temperature of mixing cut into size after the magnetic amalgam cooling after will mixing and are φ 3.5mm; The particulate material of length 2.5mm, the intrinsic coercivity iHc of particulate material is 9370 Oe.
Embodiment 9:
The NdFeB permanet magnetic powder 10kg of the coupling processing of learning from else's experience, nylon 317g, metal antioxidant 190g; Plasticizer 20g, wax liquid 33g mixes through meshing parallel double-screw in the same way; The process of mixing charges into nitrogen protection, and 320 ℃ of the temperature of mixing cut into size after the magnetic amalgam cooling after will mixing and are φ 3.5mm; The particulate material of length 2.5mm, the intrinsic coercivity iHc of particulate material is 9400 Oe.
Claims (10)
1. boned neodymium iron boron permanent magnet particulate material preparation method comprises the steps:
Step 1: coupling processing: get the coupling agent of 0.2～1 mass parts, use is that the absolute ethyl alcohol of 2～10 mass parts stirs coupling agent is fully dissolved; The fast quenching NdFeB permanet magnetic powder of solution and 20～100 mass parts in low speed mixer; Stir; Then NdFeB magnetic powder is after treatment carried out drying under 50 ℃～60 ℃ temperature, more above-mentioned block NdFeB magnetic powder through coupling processing is pulverized after the cooling;
Step 2: mixed processing: the NdFeB magnetic powder 85～95wt%, thermoplastic resin 2～14 wt%, metal antioxidant 1～5 wt% and other processing additives 0～2wt% that get after step 1 coupling processing fully mix at high-speed mixer;
Step 3: the processing of mixing: will pass through the magnetic mixture after step 2 is handled, and in the muller that meshes parallel double-screw in the same way, mix;
Step 4: granulation: cut into particulate material after the magnetic amalgam cooling after will mixing;
It is characterized in that in the step 3, the magnetic mixture mixes having under the protective atmosphere.
2. boned neodymium iron boron permanent magnet particulate material preparation method as claimed in claim 1 is characterized in that: in the step 1, and coupling agent, absolute ethyl alcohol, the three's of magnetic weight ratio is 1:10:100.
3. boned neodymium iron boron permanent magnet particulate material preparation method as claimed in claim 1 is characterized in that: in the step 1, described coupling agent is silane coupler or titanate coupling agent.
4. boned neodymium iron boron permanent magnet particulate material preparation method as claimed in claim 1; It is characterized in that: in the step 2; Described thermoplastic resin is nylon or PPS; Described metal antioxidant is the mixture of phenols antioxidant or phenols antioxidant and phosphorous acid esters antioxidant, and described processing aid is plasticizer and lubricant.
5. boned neodymium iron boron permanent magnet particulate material preparation method as claimed in claim 4 is characterized in that: described plasticizer is a phthalate compound, and described lubricant is silicone oil or wax liquid.
6. boned neodymium iron boron permanent magnet particulate material preparation method as claimed in claim 1 is characterized in that: in the step 3, described protective atmosphere is a nitrogen.
7. boned neodymium iron boron permanent magnet particulate material preparation method as claimed in claim 1 is characterized in that: in the step 3, when thermoplastic resin was nylon, melting temperature was between 200 ℃～300 ℃, and thermoplastic resin is between 290 ℃～350 ℃ of the temperature of mixing of PPS.
8. boned neodymium iron boron permanent magnet particulate material preparation method as claimed in claim 1 is characterized in that: the size of the particulate material after step 4 cutting is φ 3.5～4.5mm, length 2～4mm.
9. boned neodymium iron boron permanent magnet particulate material preparation method as claimed in claim 1 is characterized in that: in the step 1, described Agglutinate neodymium-iron-boron permanent magnetism powder is the fast quenching NdFeB permanet magnetic powder.
10. like each described boned neodymium iron boron permanent magnet particulate material preparation method of claim 1～9, it is characterized in that: the iHc of described boned neodymium iron boron permanent magnet particulate material is 9200 Oe～9600 Oe.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102965115A (en) * | 2012-11-21 | 2013-03-13 | 中国计量学院 | Ternary antioxidant and application thereof |
| CN102969116A (en) * | 2012-07-20 | 2013-03-13 | 横店集团东磁股份有限公司 | UV (ultraviolet) solidified bonding magnet and preparation method thereof |
| CN103578683A (en) * | 2013-09-29 | 2014-02-12 | 浙江省东阳市诚基电机有限公司 | Rubber magnetic strip used under low temperature and preparation method thereof |
| CN103862052A (en) * | 2012-12-17 | 2014-06-18 | 北京中科三环高技术股份有限公司 | Method for forming isotropic neodymium-iron-boron magnet |
| CN105655077A (en) * | 2016-04-13 | 2016-06-08 | 烟台正海磁性材料股份有限公司 | Manufacturing method of high-coercive-force neodymium iron boron |
| CN107603220A (en) * | 2017-09-14 | 2018-01-19 | 横店集团东磁股份有限公司 | A kind of PPS rare earth permanent magnets injection particle masterbatch and preparation method thereof |
| CN115673328A (en) * | 2022-11-15 | 2023-02-03 | 绵阳西磁磁业有限公司 | Method and device for ball milling powder preparation by rare earth permanent magnet dry method |
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| CN1937111A (en) * | 2006-09-19 | 2007-03-28 | 北京大学 | Method for preparing rolling anisotropic magnetic powder and magnet |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102969116A (en) * | 2012-07-20 | 2013-03-13 | 横店集团东磁股份有限公司 | UV (ultraviolet) solidified bonding magnet and preparation method thereof |
| CN102965115A (en) * | 2012-11-21 | 2013-03-13 | 中国计量学院 | Ternary antioxidant and application thereof |
| CN102965115B (en) * | 2012-11-21 | 2014-06-04 | 中国计量学院 | Ternary antioxidant and application thereof |
| CN103862052A (en) * | 2012-12-17 | 2014-06-18 | 北京中科三环高技术股份有限公司 | Method for forming isotropic neodymium-iron-boron magnet |
| CN103578683A (en) * | 2013-09-29 | 2014-02-12 | 浙江省东阳市诚基电机有限公司 | Rubber magnetic strip used under low temperature and preparation method thereof |
| CN103578683B (en) * | 2013-09-29 | 2016-02-03 | 浙江省东阳市诚基电机有限公司 | A kind of low temperature rubber magnetic stripe and preparation method thereof |
| CN105655077A (en) * | 2016-04-13 | 2016-06-08 | 烟台正海磁性材料股份有限公司 | Manufacturing method of high-coercive-force neodymium iron boron |
| CN107603220A (en) * | 2017-09-14 | 2018-01-19 | 横店集团东磁股份有限公司 | A kind of PPS rare earth permanent magnets injection particle masterbatch and preparation method thereof |
| CN115673328A (en) * | 2022-11-15 | 2023-02-03 | 绵阳西磁磁业有限公司 | Method and device for ball milling powder preparation by rare earth permanent magnet dry method |
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Application publication date: 20120711 |