WO2022198539A1 - Procédé de préparation d'un noyau de poudre magnétique revêtue de sol-gel modifié par broyage à billes - Google Patents

Procédé de préparation d'un noyau de poudre magnétique revêtue de sol-gel modifié par broyage à billes Download PDF

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Publication number
WO2022198539A1
WO2022198539A1 PCT/CN2021/082877 CN2021082877W WO2022198539A1 WO 2022198539 A1 WO2022198539 A1 WO 2022198539A1 CN 2021082877 W CN2021082877 W CN 2021082877W WO 2022198539 A1 WO2022198539 A1 WO 2022198539A1
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WIPO (PCT)
Prior art keywords
magnetic powder
ball
ball milling
gel
powder core
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PCT/CN2021/082877
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English (en)
Chinese (zh)
Inventor
张勉团
皮金斌
毛圣华
陈俊杰
温余远
金鑫
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江西艾特磁材有限公司
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Priority to PCT/CN2021/082877 priority Critical patent/WO2022198539A1/fr
Publication of WO2022198539A1 publication Critical patent/WO2022198539A1/fr

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/20—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder
    • H01F1/22—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together
    • H01F1/24—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets

Definitions

  • the invention relates to the technical field of magnetic powder core preparation, in particular to a method for ball milling modified sol-gel coating magnetic powder core.
  • Soft magnetic composites are mostly coated with inorganic and organic layers.
  • patent US2783208 filed by Katz reports that the bilayer coating is phosphoric acid and thermosetting phenolic resin; while patent US5063011 by Rutz uses iron phosphate and thermoplastic resin.
  • the patent US4601765 of Soileau et al. reported that the alkali metal silicate was used to coat first, and then the siloxane resin was coated. Double cladding can better meet the requirements of various properties (magnetic, mechanical, chemical, thermal properties, etc.).
  • Al 2 O 3 is an insulating material with high resistivity and heat resistance, and is the preferred coating for soft magnetic composite powders.
  • Chinese patent 201310351622.4 reports that nano-Al 2 O 3 is uniformly and densely coated on metal magnetic powder by sol-gel combined with high temperature heat treatment, and the coated powder is used to prepare metal soft magnetic composite material.
  • the particle size and surface morphology of the powder are uncontrollable and cannot be adapted to magnetic powder cores with different performance requirements.
  • the heat treatment temperature is too high. Due to the problems of high requirements and high energy consumption, the present invention provides a method for ball-milling modified sol-gel to coat magnetic powder cores.
  • a method for ball milling modified sol-gel coating magnetic powder core which is characterized by comprising the following steps:
  • step S4 mixing the AlOOH sol obtained in step S3 with the metal magnetic powder, and the weight of the sol is 0.5-3% of the weight of the metal magnetic powder;
  • step S6 the powder obtained in step S5 is ball milled with a ball mill;
  • step S8 First coat the silane coupling agent on the metal magnetic powder obtained in step S7, let stand for 30-60 min, then coat the silicone resin, and heat and dry the mixed material at 120-180 °C for 120-180 min to obtain coated powder;
  • the ball milling time of the ball mill in the step S6 is set to 4 to 12 hours, the diameter of the grinding balls is 10 to 100 mm, and the ball milling speed is 20 to 50 r/min.
  • the diameter and thickness of the grinding ball in the step S6 are matched: 25%, 75%; or 30%, accounted for 60%, accounted for 10%.
  • the temperature of the high-temperature heat treatment in the step S7 is 600-800° C.
  • the holding time is 30-180 minutes.
  • the molar ratio of the added amounts of aluminum isopropoxide, deionized water and HNO 3 in the steps S1 and S2 is 1:80-100:0.3-0.5.
  • the metal magnetic powder in the step S4 is composed of one or more of pure Fe, FeSi, FeSiAl, FeSiNi, FeNi, FeNiMo or FeNiCr, and the average particle size of the metal magnetic powder is 20-100 ⁇ m.
  • the metal magnetic powder in step S8 accounts for 97.5-99 wt % of the total composition
  • the silane coupling agent accounts for 0.3-1.0 wt % of the total composition
  • the silicone resin accounts for 0.5-1.5 wt % of the total composition.
  • the lubricant in the step S10 is a mixture of one or more of KP-11, stearic acid, zinc stearate or lithium stearate, and the lubricant content is 0.1-1.0% by weight of the mixture.
  • the press forming process of the step S11 is to press into a ring shape, an E shape or a U shape under a pressure of 1000-2300 MPa.
  • the process parameters of the annealing heat treatment in the step S12 are: a temperature of 500-800° C., a holding time of 30-120 min, and an atmosphere of N 2 or H 2 atmosphere.
  • the powder is coated with ball-milled AlOOH gel to obtain a nano- ⁇ -Al 2 O 3 coated inorganic layer, so that the coated layer is thin, more uniform and dense, and has excellent insulation;
  • the temperature of powder heat treatment after ball milling only needs to be 600-800 °C, which greatly reduces energy consumption and reduces equipment requirements;
  • the soft magnetic composite material prepared by the present invention has high magnetic permeability and lower core loss, and has good frequency stability. small magnetic loss;
  • the preparation equipment of the present invention is simple, easy to operate, and low in cost, and is especially suitable for industrialized mass production and large-scale production.
  • FIG. 1 is a process flow diagram of a coated magnetic powder core according to an embodiment of the present invention
  • Fig. 2 is the SME photo after FeSiAl magnetic powder core annealing treatment of the present invention
  • 3 is a graph showing the change of magnetic properties of the magnetic powder core obtained when the ball milling time of the present invention is 4h, 6h, 8h, 10h and 12h;
  • 4 is a graph showing the change of magnetic properties of the magnetic powder core obtained when the ball milling speed of the present invention is 20r/min, 30r/min, 40r/min and 50r/min.
  • the weight of the sol is 1% of the aerosolized FeSi magnetic powder; then the mixture is kept in a drying oven at 150 °C for 150 min to obtain AlOOH gel-coated powder; the obtained powder is then ball-milled in a ball mill, using and Two grinding balls, and The grinding ball ratio was 1:3, the ball milling speed was 20 r/min, and the ball milling was performed for 12 hours.
  • the ball-milled powder was heated to 600°C for 90min in a H2 atmosphere to obtain a magnetic powder coated with nano- ⁇ -Al 2 O 3 ; then the heat-treated mixture was added with 0.6% of the total mass of silane coupling 1.1% of the total mass of silicone resin was added and mixed evenly; the mixed material was placed in a drying box at 150°C for drying for 2 hours, and after cooling, the material was crushed and passed through a 100-mesh sieve. The obtained powder is added with 0.8% content of zinc stearate lubricant and mixed uniformly, and then pressed under 2300MPa pressure into ring.
  • Comparative Example 1 is the FeSi magnetic powder core prepared by the prior art.
  • the detection data from Table 1 and Table 2 show that the FeSi magnetic powder core of the present invention has better frequency characteristics of magnetic permeability compared with the existing FeSi magnetic powder core, and the magnetic permeability decreases with the increase of frequency. Very small; less magnetic loss at high frequencies.
  • AlOOH gel-coated powder is then ball-milled in a ball mill, using and Two grinding balls, and The grinding ball ratio was 3:1, the ball milling speed was 50 r/min, and the ball milling was performed for 4 hours.
  • the ball-milled powder was heated to 800° C. for 80 min in a N 2 atmosphere to obtain a magnetic powder coated with nano- ⁇ -Al 2 O 3 ; then the heat-treated mixture was added with 0.5% of the total mass of silane
  • the joint agent is mixed evenly, and 1.2% of the total mass of silicone resin is added and mixed evenly; the mixed material is put into a drying box for drying at 150 ° C for 2 hours, and after cooling, the material is crushed and passed through a 100-mesh sieve; the obtained powder is added with 0.7%
  • the content of zinc stearate lubricant is mixed evenly, and then pressed into a 2300MPa pressure ring.
  • the obtained samples were heat-treated at 720°C in a sintering furnace in a pure N2 atmosphere for 60 minutes, and finally the magnetic properties of the samples were tested on a VR152 tester. The properties of the obtained samples are shown in Table 3 and Table 4.
  • the detection data in Table 3 and Table 4 show that compared with the FeSiAl magnetic powder core of the present invention, the magnetic powder core prepared by the present invention has better magnetic permeability frequency characteristics. With the increase of frequency, the magnetic permeability Attenuation is small; less magnetic loss at high frequencies.
  • the weight of the sol is 0.5% of the gas atomized FeSiAl magnetic powder; then the mixture is kept in a drying oven at 150 ° C for 120 min to obtain AlOOH gel-coated powder; the obtained powder is then ball-milled in a ball mill, using and Three grinding balls, The ratio of grinding balls is 3:6:1, the ball milling speed is 35r/min, and the ball milling is 8 hours.
  • the ball-milled powder was heated to 700°C for 90min in a H 2 atmosphere to obtain a magnetic powder coated with nano- ⁇ -Al 2 O 3 ; then the heat-treated mixture was added with 0.5% of the total mass of silane
  • the joint agent is mixed evenly, and 1.2% of the total mass of silicone resin is added and mixed evenly; the mixed material is put into a drying box for drying at 150 ° C for 2 hours, and after cooling, the material is crushed and passed through a 100-mesh sieve; the obtained powder is added with 0.7%
  • the content of zinc stearate lubricant is mixed uniformly, and then pressed into a 1500MPa pressure ring.
  • the obtained samples were heat-treated at 800 °C in a sintering furnace in a pure H2 atmosphere for 60 min, and finally the magnetic properties of the samples were tested on a VR152 tester. The properties of the obtained samples are shown in Table 5 and Table 6.
  • the detection data from Table 5 and Table 6 show that the FeSiAl magnetic powder core of the present invention has better magnetic permeability frequency characteristics compared with the FeSiAl magnetic powder core of the prior art, and the magnetic permeability decays with the increase of the frequency. Very small; less magnetic loss at high frequencies.
  • the weight is 2% of the gas atomized FeNi magnetic powder; then the mixture is kept in a drying oven at 140 °C for 150 min to obtain AlOOH gel-coated powder; the obtained powder is then ball-milled in a ball mill, using and Three grinding balls, The ratio of grinding balls is 3:6:1, the ball milling speed is 40r/min, and the ball milling is performed for 10 hours.
  • the ball-milled powder was heated to 800°C for 60 min in an H 2 atmosphere to obtain a magnetic powder coated with nano- ⁇ -Al 2 O 3 ; then the heat-treated mixture was added with 1% of the total mass of silane
  • the joint agent is mixed evenly, and 1.5% of the total mass of silicone resin is added and mixed evenly; the mixed material is placed in a drying box at 150 ° C for drying for 2 hours, and after cooling, the material is crushed and passed through a 100-mesh sieve; the obtained powder is added with 0.8%
  • the content of zinc stearate lubricant is mixed uniformly, and then pressed into a 1900MPa pressure ring.
  • the obtained samples were heat-treated at 720°C in a sintering furnace in a pure H2 atmosphere for 60 minutes, and finally the magnetic properties of the samples were tested on a VR152 tester. The properties of the obtained samples are shown in Table 4.
  • the detection data from Table 7 and Table 8 show that the FeNi magnetic powder core of the present invention has better magnetic permeability frequency characteristics compared with the FeNi magnetic powder core of the prior art, and the magnetic permeability decreases with the increase of frequency. Very small; less magnetic loss at high frequencies.
  • the present invention can obtain magnetic powder cores with different performance requirements by controlling the ball milling time and ball milling speed.

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Powder Metallurgy (AREA)

Abstract

La présente invention concerne un procédé de préparation d'un noyau de poudre magnétique revêtue de sol-gel modifié par broyage à billes. La poudre revêtue de gel d'AlOOH est soumise à un broyage à billes et à un traitement thermique à haute température, de sorte qu'un nano α-Al2O3 plus uniforme et compact peut être obtenu pour revêtir un noyau de poudre magnétique. Selon la présente invention, la poudre revêtue de gel d'AlOOH est soumise au broyage à billes pour obtenir une couche de revêtement nano α-Al2O3, de sorte que la couche de revêtement est mince et plus uniforme et compacte, et présente une excellente capacité d'isolation. La température du traitement thermique pour la poudre après le broyage à billes est seulement comprise entre 600 et 800 °C, ce qui réduit considérablement la consommation d'énergie, ainsi que les exigences imposées au dispositif. La distribution granulométrique et la morphologie de poudre de la poudre revêtue peuvent être commandées en commandant le temps de broyage à billes, le diamètre des billes de broyage, de la vitesse de rotation du broyage à billes et d'autres paramètres de traitement, ce qui permet d'obtenir des noyaux de poudre magnétique présentant des exigences de performance différentes. Selon la présente invention, le dispositif de préparation est simple, facile à utiliser et à faible coût, et est particulièrement approprié pour une production industrielle de masse et une production à grande échelle.
PCT/CN2021/082877 2021-03-25 2021-03-25 Procédé de préparation d'un noyau de poudre magnétique revêtue de sol-gel modifié par broyage à billes WO2022198539A1 (fr)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116631764A (zh) * 2023-07-24 2023-08-22 通友微电(四川)有限公司 无机包覆软磁粉体的制备方法
CN116666101A (zh) * 2023-07-24 2023-08-29 通友微电(四川)有限公司 有机包覆软磁粉体的制备方法
CN116825466A (zh) * 2023-08-16 2023-09-29 中南大学 一种FeSiAl软磁复合材料及其制备方法

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CN101619177A (zh) * 2009-07-31 2010-01-06 孝感学院 一种纳米二氧化钛包覆纳米三氧化二铝的制备方法
CN104368807A (zh) * 2013-08-13 2015-02-25 东睦新材料集团股份有限公司 一种金属软磁复合材料用粉末的包覆方法及磁体的制备方法
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CN112185642A (zh) * 2020-09-23 2021-01-05 江西艾特磁材有限公司 一种球磨改性溶胶－凝胶包覆磁粉芯的方法

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JP2009099853A (ja) * 2007-10-18 2009-05-07 Hitachi Metals Ltd 高耐食性ｒ−ｔ−ｂ系希土類磁石
CN101619177A (zh) * 2009-07-31 2010-01-06 孝感学院 一种纳米二氧化钛包覆纳米三氧化二铝的制备方法
CN104368807A (zh) * 2013-08-13 2015-02-25 东睦新材料集团股份有限公司 一种金属软磁复合材料用粉末的包覆方法及磁体的制备方法
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116631764A (zh) * 2023-07-24 2023-08-22 通友微电(四川)有限公司 无机包覆软磁粉体的制备方法
CN116666101A (zh) * 2023-07-24 2023-08-29 通友微电(四川)有限公司 有机包覆软磁粉体的制备方法
CN116631764B (zh) * 2023-07-24 2023-10-27 通友微电(四川)有限公司 无机包覆软磁粉体的制备方法
CN116666101B (zh) * 2023-07-24 2024-03-08 通友微电(四川)有限公司 有机包覆软磁粉体的制备方法
CN116825466A (zh) * 2023-08-16 2023-09-29 中南大学 一种FeSiAl软磁复合材料及其制备方法

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