WO2022198539A1 - Method for preparing ball milling-modified sol-gel coated magnetic powder core - Google Patents

Method for preparing ball milling-modified sol-gel coated magnetic powder core Download PDF

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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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magnetic powder
ball
ball milling
gel
powder core
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PCT/CN2021/082877
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French (fr)
Chinese (zh)
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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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Publication of WO2022198539A1 publication Critical patent/WO2022198539A1/en

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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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Abstract

Disclosed in the present invention is a method for preparing a ball milling-modified sol-gel coated magnetic powder core. AlOOH gel coated powder is subjected to ball milling and high-temperature heat treatment, so that more uniform and compact nano α-Al2O3 can be obtained for coating a magnetic powder core. According to the present invention, the AlOOH gel coated powder is subjected to the ball milling to obtain a nano α-Al2O3 coating layer, so that the coating layer is thin and more uniform and compact, and has excellent insulativity; the temperature of the heat treatment for the powder after the ball milling is only 600-800°C, so that the energy consumption is greatly reduced, and the requirement on device is also reduced; and the particle size distribution and the powder morphology of the coated powder can be controlled by controlling the ball milling time, the diameter of grinding balls, the ball milling rotational speed, and other process parameters, so that magnetic powder cores having different performance requirements can be obtained. According to the present invention, the preparation device is simple, easy to operate and low in cost, and is particularly suitable for industrial mass production and large-scale production.

Description

一种球磨改性溶胶－凝胶包覆磁粉芯的方法A method for ball milling modified sol-gel coating magnetic powder core 技术领域technical field
本发明涉及磁粉芯制备技术领域，尤其涉及一种球磨改性溶胶－凝胶包覆磁粉芯的方法。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.
背景技术Background technique
软磁复合材料多采用无机物和有机物多层包覆。如Katz申请的专利US2783208报道的双层包覆层为磷酸和热固性酚醛树脂；而Rutz的专利US5063011则采用的是铁的磷酸盐和热塑性树脂。Soileau等的专利US4601765报道的是先采用碱金属硅酸盐包覆，然后再包覆硅氧烷树脂。双包覆层较能满足各种性能的要求(磁性、机械、化学、热性能等)。Soft magnetic composites are mostly coated with inorganic and organic layers. For example, 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.).
近年来，以超细甚至纳米金属氧化物(如Al 2O 3、TiO 2、SiO 2、MgO 2等)作为无机物包覆层得到普遍采用。欧洲专利EP434669报道在10-300μm的粉末中包覆一层不超过10μm的碱金属氧化物。中国发明专利200610040493.7报道了一种采用纳米SiO 2包覆羰基铁粉的制备方法。 In recent years, ultra-fine or even nano-metal oxides (such as Al 2 O 3 , TiO 2 , SiO 2 , MgO 2 , etc.) are widely used as inorganic coating layers. European Patent EP434669 reports the coating of powders of 10-300 μm with a layer of alkali metal oxide not exceeding 10 μm. Chinese invention patent 200610040493.7 reports a preparation method of carbonyl iron powder coated with nano-SiO 2 .
Al 2O 3是一种具有高电阻率和耐热性的绝缘材料，是软磁复合粉末的首选包覆物。中国专利201310351622.4报道采用溶胶-凝胶并结合高温热处理把纳米Al 2O 3均匀而致密地包覆在金属磁性粉末上，并采用此包覆粉末制备金属软磁复合材料。但该方法还存在一些不足：1)纳米Al 2O 3粉末粒径和表面形貌不可控，不能根据不同性能需求调整粉末粒径和表面形貌；2)对于性能要求很高的磁粉芯，纳米Al 2O 3包覆粉末还达不到要求；3)热处理温度太高，对设备要求高，不利于规模化生产，而且能耗大，不符合国家节能环保的方针。 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. However, this method still has some shortcomings: 1) The particle size and surface morphology of nano-Al 2 O 3 powder are uncontrollable, and the powder particle size and surface morphology cannot be adjusted according to different performance requirements; 2) For magnetic powder cores with high performance requirements, The nano-Al 2 O 3 coated powder can not meet the requirements; 3) The heat treatment temperature is too high, the equipment requirements are high, it is not conducive to large-scale production, and the energy consumption is large, which does not meet the national policy of energy conservation and environmental protection.
发明内容SUMMARY OF THE INVENTION
为了解决上述现有采用溶胶-凝胶把纳米Al 2O 3包覆金属磁性粉末，但粉末粒径和表面形貌不可控，不能适应不同性能要求的磁粉芯，同时热处理温度太高，对设备要求高，能耗大的问题，本发明提供了一种球磨改性溶胶－凝胶包覆磁粉芯的方法。 In order to solve the problem of the above-mentioned existing use of sol-gel to coat metal magnetic powder with nano-Al 2 O 3 , the particle size and surface morphology of the powder are uncontrollable and cannot be adapted to magnetic powder cores with different performance requirements. At the same time, 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.
本发明的技术方案是这样实现的：The technical scheme of the present invention is realized as follows:
一种球磨改性溶胶－凝胶包覆磁粉芯的方法，其特征在于包括以下步骤：A method for ball milling modified sol-gel coating magnetic powder core, which is characterized by comprising the following steps:
S1、把异丙醇铝和去离子水放入烧杯中并置于95～100℃水浴搅拌溶解60～90min；S1. Put aluminum isopropoxide and deionized water into a beaker and place it in a water bath at 95 to 100°C and stir to dissolve for 60 to 90 minutes;
S2、然后加入HN0 3,继续在95～100℃水浴中搅拌6～9.5h； S2, then add HN0 3 , and continue to stir in a water bath at 95 to 100° C. for 6 to 9.5 hours;
S3、随后在85-95℃水浴中静置陈化15～19.5h,然后过滤得到AlOOH溶胶；S3, then stand for 15-19.5 h in a water bath at 85-95 °C, and then filter to obtain AlOOH sol;
S4、将步骤S3得到的AlOOH溶胶与金属磁性粉末混合，溶胶重量为金属磁性粉末重量的0.5-3％；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;
S5、接着在120-150℃干燥120～180min得到AlOOH凝胶包覆的粉末；S5, then drying at 120-150° C. for 120-180 min to obtain AlOOH gel-coated powder;
S6、将步骤S5得到的粉末用球磨机球磨；S6, the powder obtained in step S5 is ball milled with a ball mill;
S7、将球磨后的粉末在H 2或N 2气氛下高温热处理，即得到纳米α-Al 2O 3包覆后的金属磁性粉末； S7, heat-treating the ball-milled powder at a high temperature in an atmosphere of H 2 or N 2 to obtain a metal magnetic powder coated with nano-α-Al 2 O 3 ;
S8、在步骤S7得到的金属磁性粉末上先包覆硅烷偶联剂，静置30～60min，再包覆硅树脂，并将混合好的物料于120-180℃保温干燥120～180min,即得到包覆粉末；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 ℃ for 120-180 min to obtain coated powder;
S9、将干燥后的包覆粉末采用80～200目筛进行过筛；S9, sieve the dried coated powder with an 80-200 mesh sieve;
S10、随后加入适量润滑剂后混合均匀；S10, then add an appropriate amount of lubricant and mix evenly;
S11、将混合料压制成形；S11, press the mixture into forming;
S12、最后将压坯进行退火热处理，即得到所需的球磨改性溶胶－凝胶包覆磁粉芯。S12. Finally, annealing and heat treatment is performed on the compact to obtain the desired ball-milled modified sol-gel coated magnetic powder core.
优选的，所述步骤S6中的球磨机球磨时间设为4～12小时，研磨球直径为10～100mm，球磨速度为20～50r/min。Preferably, 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.
优选的，所述步骤S6中的研磨球直径粗细搭配：
Figure PCTCN2021082877-appb-000001
占25％，
Figure PCTCN2021082877-appb-000002
占比75％；或者
Figure PCTCN2021082877-appb-000003
占30％，
Figure PCTCN2021082877-appb-000004
占比60％，
Figure PCTCN2021082877-appb-000005
Figure PCTCN2021082877-appb-000006
占比10％。 Preferably, the diameter and thickness of the grinding ball in the step S6 are matched:
Figure PCTCN2021082877-appb-000001
25%,
Figure PCTCN2021082877-appb-000002
75%; or
Figure PCTCN2021082877-appb-000003
30%,
Figure PCTCN2021082877-appb-000004
accounted for 60%,
Figure PCTCN2021082877-appb-000005
Figure PCTCN2021082877-appb-000006
accounted for 10%.
优选的，所述步骤S7中的高温热处理的温度为600～800℃,保温时间30～180min。Preferably, the temperature of the high-temperature heat treatment in the step S7 is 600-800° C., and the holding time is 30-180 minutes.
优选的，所述步骤S1、S2中的异丙醇铝、去离子水和HN0 3的加入量的摩尔比为1:80～100:0.3～0.5。 Preferably, 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.
优选的，所述步骤S4中的金属磁性粉末是由纯Fe、FeSi、FeSiAl、FeSiNi、FeNi、FeNiMo或FeNiCr中的一种或多种组成，金属磁性粉末平均粒度为20-100μm。Preferably, 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 μm.
优选的，步骤S8中的金属磁性粉末占总成分97.5～99wt％,硅烷偶联剂占总成分0.3～1.Owt％,硅树脂占总成分0.5～1.5wt％。Preferably, 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, and the silicone resin accounts for 0.5-1.5 wt % of the total composition.
优选的，所述步骤S10的润滑剂为KP-11、硬脂酸、硬脂酸锌或硬脂酸锂中的一种或几种混合,润滑剂含量为混合料重量的0.1～1.0％。Preferably, 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.
优选的，所述步骤S11的压制成形的工艺为在1000～2300MPa压力下压制成环形、E形或U形。Preferably, 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.
优选的，所述步骤S12的退火热处理的工艺参数为：温度500～800℃,保温时间30～120min,气氛为N 2或H 2气氛。 Preferably, 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.
与现有技术相比，本发明的有益效果是：Compared with the prior art, the beneficial effects of the present invention are:
1)采用球磨AlOOH凝胶包覆粉末，得到纳米α-Al 2O 3包覆无机物层，使包覆层薄且更加均匀致密,具有优良的绝缘性； 1) The powder is coated with ball-milled AlOOH gel to obtain a nano-α-Al 2 O 3 coated inorganic layer, so that the coated layer is thin, more uniform and dense, and has excellent insulation;
2)球磨后粉末热处理的温度只需要600-800℃，大大降低了能耗，也降低了对设备的要求；2) The temperature of powder heat treatment after ball milling only needs to be 600-800 ℃, which greatly reduces energy consumption and reduces equipment requirements;
3)通过对球磨时间、研磨球的直径和球磨转速等工艺参数的控制，可以控制包覆粉末粒度分布和粉末形貌，从而得到不同性能要求的磁粉芯；3) By controlling the process parameters such as the ball milling time, the diameter of the grinding ball and the ball milling speed, the particle size distribution and powder morphology of the coated powder can be controlled, so as to obtain magnetic powder cores with different performance requirements;
4)采用本发明所制备的软磁复合材料具有高的磁导率和更低的磁芯损耗,频率稳定性好，随着频率的提高，磁导率衰减很小，在高频下具有更小的磁损耗；4) 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;
5)本发明制备设备简单、易操作,成本低，特别适合于工业化大批量、大规模生产用。5) 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.
附图说明Description of drawings
图1为本发明实施例包覆磁粉芯工艺流程图；FIG. 1 is a process flow diagram of a coated magnetic powder core according to an embodiment of the present invention;
图2为本发明FeSiAl磁粉芯退火处理后的SME照片；Fig. 2 is the SME photo after FeSiAl magnetic powder core annealing treatment of the present invention;
图3为本发明球磨时间为4h、6h、8h、10h、12h时所得磁粉芯磁性能变化图；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;
图4为本发明球磨速度为20r/min、30r/min、40r/min、50r/min时所得磁粉芯磁性能变化图。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.
具体实施方式Detailed ways
下面结合具体实施例对本发明进行进一步描述，但本发明的保护范围并不仅限于此：The present invention is further described below in conjunction with specific embodiment, but the protection scope of the present invention is not limited to this:
实施例1：Example 1:
将异丙醇铝放入去离子水中经95℃水浴并磁力搅拌80min，随后滴入HNO3并继续磁力搅拌9.5h，异丙醇铝、去离子水和硝酸按摩尔比1:100:0.5配比；磁力搅拌结束后继续在95℃下水浴静置陈化19.5h；将过滤得到的AlOOH溶胶与平均粒径为30μm的气雾化FeSi(化学组成为铁94.5％、硅5.5％)磁粉混合均匀，溶胶重量为气雾化FeSi磁粉的1％；随后将混合料在干燥箱中150℃保温150min即得到AlOOH凝胶包覆的粉末；再将所得粉末在球磨机内进行球磨，采用
Figure PCTCN2021082877-appb-000007
和
Figure PCTCN2021082877-appb-000008
两种研磨球，
Figure PCTCN2021082877-appb-000009
和
Figure PCTCN2021082877-appb-000010
研磨球比例是1:3，球磨速度20r/min，球磨12小时。 Put aluminum isopropoxide into deionized water, go through a water bath at 95°C and stir magnetically for 80min, then drop in HNO3 and continue magnetic stirring for 9.5h. The molar ratio of aluminum isopropoxide, deionized water and nitric acid is 1:100:0.5. ; After the magnetic stirring, continue to stand in a water bath for 19.5 hours at 95°C; Mix the AlOOH sol obtained by filtration with the aerosolized FeSi (chemical composition: iron 94.5%, silicon 5.5%) magnetic powder with an average particle size of 30 μm. , 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
Figure PCTCN2021082877-appb-000007
and
Figure PCTCN2021082877-appb-000008
Two grinding balls,
Figure PCTCN2021082877-appb-000009
and
Figure PCTCN2021082877-appb-000010
The grinding ball ratio was 1:3, the ball milling speed was 20 r/min, and the ball milling was performed for 12 hours.
将球磨后的粉末在H2气氛中加热到600℃保温90min，即得到纳米α-Al 2O 3所包覆的磁性粉末；随后将热处理过的混合料中加入占总质量0.6％的硅烷偶联剂进行混合均匀，将占总质量1.1％硅树脂加入混合均匀；将混合好的物料放入烘干箱中150℃干燥2h，冷却后物料经解碎过100目筛。所得粉末加入0.8％含量的硬脂酸锌润滑剂混合均匀，随后经2300MPa压力压制成
Figure PCTCN2021082877-appb-000011
环。将得到的试样在纯H2气氛的烧结炉中700℃热处理，保温60min，最后在VR152测试仪上对样品进行磁性能测试。所得试样性能见表1、表2所示，对比例1为现有工艺所制备的FeSi磁粉芯。 The ball-milled powder was heated to 600°C for 90min in a H2 atmosphere to obtain a magnetic powder coated with nano-α-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
Figure PCTCN2021082877-appb-000011
ring. The obtained samples were heat-treated at 700°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 1 and Table 2. Comparative Example 1 is the FeSi magnetic powder core prepared by the prior art.
表1Table 1
Figure PCTCN2021082877-appb-000012
Figure PCTCN2021082877-appb-000012
表2Table 2
Figure PCTCN2021082877-appb-000013
Figure PCTCN2021082877-appb-000013
从表1、表2中检测数据显示本发明FeSi磁粉芯与现有FeSi磁粉芯相比，本发明制备的磁粉芯具有较好的磁导率频率特性，随着频率的提高，磁导率衰减很小；在高频下具有更小的磁损耗。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.
实施例2：Example 2:
将异丙醇铝放入去离子水中经100℃水浴并磁力搅拌60min，随后滴入HNO3并继续磁力搅拌6h，异丙醇铝、去离子水和硝酸按摩尔比1:90:0.4配比；磁力搅拌结束后继续在100℃下水浴静置陈化15h；将过滤得到的AlOOH溶胶与平均粒径为35μm的气雾化FeSiAl(化学组成为铁87.8％、硅6.8％和铝5.4％)磁粉混合均匀，溶胶重量为气雾化FeSiAl磁粉的3％；随后将混合料在干燥箱中120℃保温180min即得到AlOOH凝胶包覆的粉末；再将所得粉末在球磨机内进行球磨，采用
Figure PCTCN2021082877-appb-000014
和
Figure PCTCN2021082877-appb-000015
两种研磨球，
Figure PCTCN2021082877-appb-000016
和
Figure PCTCN2021082877-appb-000017
研磨球比例是3:1，球磨速度50r/min，球磨4小时。 Put aluminum isopropoxide into deionized water, go through a 100 ℃ water bath and stir magnetically for 60 minutes, then dropwise into HNO3 and continue magnetic stirring for 6h, aluminum isopropoxide, deionized water and nitric acid in a molar ratio of 1:90:0.4; After the magnetic stirring, continue to stand in a water bath for 15 hours at 100 °C; the AlOOH sol obtained by filtration and the aerosolized FeSiAl (chemical composition: 87.8% iron, 6.8% silicon and 5.4% aluminum) magnetic powder with an average particle size of 35 μm Mix uniformly, and the weight of the sol is 3% of that of the aerosolized FeSiAl magnetic powder; then the mixture is kept in a drying oven at 120° C. for 180 min to obtain AlOOH gel-coated powder; the obtained powder is then ball-milled in a ball mill, using
Figure PCTCN2021082877-appb-000014
and
Figure PCTCN2021082877-appb-000015
Two grinding balls,
Figure PCTCN2021082877-appb-000016
and
Figure PCTCN2021082877-appb-000017
The grinding ball ratio was 3:1, the ball milling speed was 50 r/min, and the ball milling was performed for 4 hours.
将球磨后的粉末在N 2气氛中加热到800℃保温80min，即得到纳米α-Al 2O 3所包覆的磁性粉末；随后将热处理过的混合料中加入占总质量0.5％的硅烷偶联剂进行混合均匀，将占总质量1.2％硅树脂加入混合均匀；将混合好的物料放入烘干箱中150℃干燥2h，冷却后物料经解碎过100目筛；所得粉末加入0.7％含量的硬脂酸锌润滑剂混合均匀，随后经2300MPa压力压制成
Figure PCTCN2021082877-appb-000018
环。将得到的试样在纯N2气氛的烧结炉中720℃热处理，保温60min，最后在VR152测试仪上对样品进行磁性能测试。所得试样性能见表3、表4所示。 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-α-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
Figure PCTCN2021082877-appb-000018
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.
表3table 3
Figure PCTCN2021082877-appb-000019
Figure PCTCN2021082877-appb-000019
表4Table 4
Figure PCTCN2021082877-appb-000020
Figure PCTCN2021082877-appb-000020
从表3、表4中检测数据显示本发明FeSiAl磁粉芯与现有工艺FeSiAl磁粉芯相比，本发明制备的磁粉芯具有较好的磁导率频率特性，随着频率的提高，磁导率衰减很小；在高频下具有更小的磁损耗。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.
实施例3：Example 3:
将异丙醇铝放入去离子水中经98℃水浴并磁力搅拌70min，随后滴入HNO3并继续磁力搅拌8h，异丙醇铝、去离子水和硝酸按摩尔比1:80:0.3配比；磁力搅拌结束后继续在98℃下水浴静置陈化17h；将过滤得到的AlOOH溶胶与平均粒径为38μm的气雾化FeSiAl(化学组成为铁87.8％、硅6.8％和铝5.4％)磁粉混合均匀，溶胶重量为气雾化FeSiAl磁粉的0.5％；随后将混合料在干燥箱中150℃保温120min即得到AlOOH凝胶包覆的粉末；再将所得粉末在球磨机内进行球磨，采用
Figure PCTCN2021082877-appb-000021
和
Figure PCTCN2021082877-appb-000022
三种研磨球，
Figure PCTCN2021082877-appb-000023
研磨球比例是3:6:1，球磨速度35r/min，球磨8小时。 Put aluminum isopropoxide into deionized water, go through a water bath at 98°C and stir magnetically for 70 minutes, then drop in HNO3 and continue magnetic stirring for 8 hours. The molar ratio of aluminum isopropoxide, deionized water and nitric acid is 1:80:0.3; After the magnetic stirring, continue to stand in a water bath for 17 hours at 98 °C; filter the AlOOH sol and the aerosolized FeSiAl (chemical composition: 87.8% iron, 6.8% silicon and 5.4% aluminum) magnetic powder with an average particle size of 38 μm. Mix uniformly, and 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
Figure PCTCN2021082877-appb-000021
and
Figure PCTCN2021082877-appb-000022
Three grinding balls,
Figure PCTCN2021082877-appb-000023
The ratio of grinding balls is 3:6:1, the ball milling speed is 35r/min, and the ball milling is 8 hours.
将球磨后的粉末在H 2气氛中加热到700℃保温90min，即得到纳米α-Al 2O 3所包覆的磁性粉末；随后将热处理过的混合料中加入占总质量0.5％的硅烷偶联剂进行混合均匀，将 占总质量1.2％硅树脂加入混合均匀；将混合好的物料放入烘干箱中150℃干燥2h，冷却后物料经解碎过100目筛；所得粉末加入0.7％含量的硬脂酸锌润滑剂混合均匀，随后经1500MPa压力压制成
Figure PCTCN2021082877-appb-000024
环。将得到的试样在纯H2气氛的烧结炉中800℃热处理，保温60min，最后在VR152测试仪上对样品进行磁性能测试。所得试样性能见表5、表6所示。 The ball-milled powder was heated to 700°C for 90min in a H 2 atmosphere to obtain a magnetic powder coated with nano-α-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
Figure PCTCN2021082877-appb-000024
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.
表5table 5
Figure PCTCN2021082877-appb-000025
Figure PCTCN2021082877-appb-000025
表6Table 6
Figure PCTCN2021082877-appb-000026
Figure PCTCN2021082877-appb-000026
从表5、表6中检测数据显示本发明FeSiAl磁粉芯与现有工艺FeSiAl磁粉芯相比，本发明制备的磁体具有较好的磁导率频率特性，随着频率的提高，磁导率衰减很小；在高频下具有更小的磁损耗。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.
实施例4：Example 4:
将异丙醇铝放入去离子水中经98℃水浴并磁力搅拌90min，随后滴入HNO3并继续磁力搅拌7h，异丙醇铝、去离子水和硝酸按摩尔比1:80:0.4配比；磁力搅拌结束后继续在98℃下水浴静置陈化15h；将过滤得到的AlOOH溶胶与平均粒径为35μm的气雾化FeNi(化学组成为铁54.5％、镍45.5％)磁粉混合均匀，溶胶重量为气雾化FeNi磁粉的2％；随后将混合料在干燥箱中140℃保温150min即得到AlOOH凝胶包覆的粉末；再将所得粉末在球磨机内进行球磨，采用
Figure PCTCN2021082877-appb-000027
和
Figure PCTCN2021082877-appb-000028
三种研磨球，
Figure PCTCN2021082877-appb-000029
研磨球比例是3:6:1，球磨速度40r/min，球磨10小时。 Put aluminum isopropoxide into deionized water, go through a water bath at 98°C and stir magnetically for 90 minutes, then drop in HNO3 and continue magnetic stirring for 7 hours. The molar ratio of aluminum isopropoxide, deionized water and nitric acid is 1:80:0.4; After the magnetic stirring, continue to stand in a water bath for 15 hours at 98°C; the AlOOH sol obtained by filtration and the aerosolized FeNi (chemical composition: iron 54.5%, nickel 45.5%) magnetic powder with an average particle size of 35 μm are mixed uniformly, and the sol is evenly mixed. 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
Figure PCTCN2021082877-appb-000027
and
Figure PCTCN2021082877-appb-000028
Three grinding balls,
Figure PCTCN2021082877-appb-000029
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.
将球磨后的粉末在H 2气氛中加热到800℃保温60min，即得到纳米α-Al 2O 3所包覆的磁性粉末；随后将热处理过的混合料中加入占总质量1％的硅烷偶联剂进行混合均匀，将占总质量1.5％硅树脂加入混合均匀；将混合好的物料放入烘干箱中150℃干燥2h，冷却后物料经解碎过100目筛；所得粉末加入0.8％含量的硬脂酸锌润滑剂混合均匀，随后经1900MPa压力压制成
Figure PCTCN2021082877-appb-000030
环。将得到的试样在纯H2气氛的烧结炉中720℃热处理，保温60min，最后在VR152测试仪上对样品进行磁性能测试。所得试样性能见表4所示。 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-α-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
Figure PCTCN2021082877-appb-000030
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.
表7Table 7
Figure PCTCN2021082877-appb-000031
Figure PCTCN2021082877-appb-000031
表8Table 8
Figure PCTCN2021082877-appb-000032
Figure PCTCN2021082877-appb-000032
从表7、表8中检测数据显示本发明FeNi磁粉芯与现有工艺FeNi磁粉芯相比，本发明制备的磁体具有较好的磁导率频率特性，随着频率的提高，磁导率衰减很小；在高频下具有更小的磁损耗。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.
如图3、4所示，本发明通过控制球磨时间与球磨速度，可以得到不同性能要求的磁粉芯。As shown in Figures 3 and 4, the present invention can obtain magnetic powder cores with different performance requirements by controlling the ball milling time and ball milling speed.
尽管已经示出和描述了本发明的实施例，对于本领域的普通技术人员而言，可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型，本发明的范围由所附权利要求及其等同物限定。Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, and substitutions can be made in these embodiments without departing from the principle and spirit of the invention and modifications, the scope of the present invention is defined by the appended claims and their equivalents.

Claims (10)

  1. 一种球磨改性溶胶－凝胶包覆磁粉芯的方法，其特征在于包括以下步骤：A method for ball milling modified sol-gel coating magnetic powder core, which is characterized by comprising the following steps:
    S1、把异丙醇铝和去离子水放入烧杯中并置于95～100℃水浴搅拌溶解60～90min；S1. Put aluminum isopropoxide and deionized water into a beaker and place it in a water bath at 95 to 100°C and stir to dissolve for 60 to 90 minutes;
    S2、然后加入HNO 3,继续在95～100℃水浴中搅拌6～9.5h； S2, then add HNO 3 , and continue to stir in a water bath at 95 to 100° C. for 6 to 9.5 hours;
    S3、随后在85-95℃水浴中静置陈化15～19.5h,然后过滤得到AlOOH溶胶；S3, then stand for 15-19.5 h in a water bath at 85-95 °C, and then filter to obtain AlOOH sol;
    S4、将步骤S3得到的AlOOH溶胶与金属磁性粉末混合，溶胶重量为金属磁性粉末重量的0.5-3％；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;
    S5、接着在120-150℃干燥120～180min得到AlOOH凝胶包覆的粉末；S5, then drying at 120-150° C. for 120-180 min to obtain AlOOH gel-coated powder;
    S6、将步骤S5得到的粉末用球磨机球磨；S6, the powder obtained in step S5 is ball milled with a ball mill;
    S7、将球磨后的粉末在H 2或N 2气氛下高温热处理，即得到纳米α-Al 2O 3包覆后的金属磁性粉末； S7, heat-treating the ball-milled powder at a high temperature in an atmosphere of H 2 or N 2 to obtain a metal magnetic powder coated with nano-α-Al 2 O 3 ;
    S8、在步骤S7得到的金属磁性粉末上先包覆硅烷偶联剂，静置30～60min，再包覆硅树脂，并将混合好的物料于120-180℃保温干燥120～180min,即得到包覆粉末；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 ℃ for 120-180 min to obtain coated powder;
    S9、将干燥后的包覆粉末采用80～200目筛进行过筛；S9, sieve the dried coated powder with an 80-200 mesh sieve;
    S10、随后加入适量润滑剂后混合均匀；S10, then add an appropriate amount of lubricant and mix evenly;
    S11、将混合料压制成形；S11, press the mixture into forming;
    S12、最后将压坯进行退火热处理，即得到所需的球磨改性溶胶－凝胶包覆磁粉芯。S12. Finally, annealing and heat treatment is performed on the compact to obtain the desired ball-milled modified sol-gel coated magnetic powder core.
  2. 根据权利要求1所述的一种球磨改性溶胶－凝胶包覆磁粉芯的方法，其特征在于：所述步骤S6中的球磨机球磨时间设为4～12小时，研磨球直径为10～100mm，球磨速度为20～50r/min。The method for ball milling modified sol-gel coated magnetic powder core according to claim 1, wherein the ball milling time of the ball mill in the step S6 is set to 4-12 hours, and the diameter of the grinding ball is 10-100 mm , the ball milling speed is 20 ~ 50r/min.
  3. 根据权利要求2所述的一种球磨改性溶胶－凝胶包覆磁粉芯的方法，其特征在于：所述步骤S6中的研磨球直径粗细搭配：φ50～100mm占25％，φ10～20mm占比75％；或者φ50～100mm占30％，φ20～30mm占比60％，φ10～15mm占比10％。A method for ball-milling modified sol-gel coating magnetic powder core according to claim 2, characterized in that: the diameter of the grinding ball in the step S6 is matched: φ50～100mm accounts for 25%, φ10～20mm accounts for 25% The ratio is 75%; or φ50～100mm accounts for 30%, φ20～30mm accounts for 60%, and φ10～15mm accounts for 10%.
  4. 根据权利要求1所述的一种球磨改性溶胶－凝胶包覆磁粉芯的方法，其特征在于：所述步骤S7中的高温热处理的温度为600～800℃,保温时间30～180min。The method for coating a magnetic powder core by ball milling modified sol-gel according to claim 1, wherein the temperature of the high temperature heat treatment in the step S7 is 600-800°C, and the holding time is 30-180min.
  5. 根据权利要求1所述的一种球磨改性溶胶－凝胶包覆磁粉芯的方法，其特征在于：所述步骤S1、S2中的异丙醇铝、去离子水和HN0 3的加入量的摩尔比为1:80～100:0.3～0.5。 The method for ball-milling modified sol-gel coating magnetic powder core according to claim 1 , wherein the added amount of aluminum isopropoxide, deionized water and HNO in the steps S1 and S2 is equal to The molar ratio is 1:80 to 100:0.3 to 0.5.
  6. 根据权利要求1所述的一种球磨改性溶胶－凝胶包覆磁粉芯的方法，其特征在于：所述步骤S4中的金属磁性粉末是由纯Fe、FeSi、FeSiAl、FeSiNi、FeNi、FeNiMo或FeNiCr中的一种或多种组成，金属磁性粉末平均粒度为20-100μm。A method of ball milling modified sol-gel coating magnetic powder core according to claim 1, wherein the metal magnetic powder in step S4 is made of pure Fe, FeSi, FeSiAl, FeSiNi, FeNi, FeNiMo Or one or more compositions of FeNiCr, and the average particle size of the metal magnetic powder is 20-100 μm.
  7. 根据权利要求1所述的一种球磨改性溶胶－凝胶包覆磁粉芯的方法，其特征在于：步骤S8中的金属磁性粉末占总成分97.5～99wt％,硅烷偶联剂占总成分0.3～1.Owt％,硅树脂占总成分0.5～1.5wt％。The method for coating a magnetic powder core with ball-milled modified sol-gel according to claim 1, wherein the metal magnetic powder in step S8 accounts for 97.5-99 wt % of the total composition, and the silane coupling agent accounts for 0.3 wt % of the total composition. ～1.0wt%, silicone resin accounts for 0.5～1.5wt% of the total composition.
  8. 根据权利要求1所述的一种球磨改性溶胶－凝胶包覆磁粉芯的方法，其特征在于：所述步骤S10的润滑剂为KP-11、硬脂酸、硬脂酸锌或硬脂酸锂中的一种或几种混合,润滑剂含量为混合料重量的0.1～1.0％。The method for coating a magnetic powder core with ball-milled modified sol-gel according to claim 1, wherein the lubricant in step S10 is KP-11, stearic acid, zinc stearate or stearin One or more of the lithium oxides are mixed, and the lubricant content is 0.1-1.0% by weight of the mixed material.
  9. 根据权利要求1所述的一种球磨改性溶胶－凝胶包覆磁粉芯的方法，其特征在于：所述步骤S11的压制成形的工艺为在1000～2300MPa压力下压制成环形、E形或U形。The method for ball-milling modified sol-gel coating magnetic powder core according to claim 1, characterized in that: the press-forming process in step S11 is to press into a ring, E-shape or U shape.
  10. 根据权利要求1所述的一种球磨改性溶胶－凝胶包覆磁粉芯的方法，其特征在于：所述步骤S12的退火热处理的工艺参数为：温度500～800℃,保温时间30～120min,气氛为 N 2或H 2气氛。 The method for coating a magnetic powder core with ball-milled modified sol-gel according to claim 1, wherein the process parameters of the annealing heat treatment in step S12 are: temperature 500-800°C, holding time 30-120min , the atmosphere is N 2 or H 2 atmosphere.
PCT/CN2021/082877 2021-03-25 2021-03-25 Method for preparing ball milling-modified sol-gel coated magnetic powder core WO2022198539A1 (en)

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