CN115116733B - 一种高频低损耗mpp软磁合金粉芯的制备方法 - Google Patents

一种高频低损耗mpp软磁合金粉芯的制备方法 Download PDF

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CN115116733B
CN115116733B CN202210842019.5A CN202210842019A CN115116733B CN 115116733 B CN115116733 B CN 115116733B CN 202210842019 A CN202210842019 A CN 202210842019A CN 115116733 B CN115116733 B CN 115116733B
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mpp
slurry
powder
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CN115116733A (zh
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侯海彬
刘志坚
杨陆
王雨
李奇
胡作启
刘卫忠
贺泓鑫
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Emicore Corp
Huazhong University of Science and Technology
CETC 9 Research Institute
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Huazhong University of Science and Technology
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    • H—ELECTRICITY
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    • 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
    • H01F41/0206—Manufacturing of magnetic cores by mechanical means
    • H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
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    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
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    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • 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
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling

Abstract

本发明提供一种高频低损耗MPP软磁合金粉芯的制备方法，包括以下步骤：S1.MPP粉体粒径大小配比，用行星球磨机混合；S2.按照质量份数配比浆料原料：硼酐15‑40份、二氧化硅20‑40份和氧化铝15‑35份，加入锆球和酒精，在行星球磨机中磨成浆料；S3.浆料中加入硅烷偶联剂处理，再添加树脂；S4.将S3的浆料混合物加入到高堆积密度的MPP磁粉中，再加入分散剂，均匀混合30‑180分钟，干燥；S5.利用热压成型技术成型得到磁芯胚，并把磁芯胚热处理。该方法制备的磁芯具有高的电阻率，低损耗，高的致密度和气孔少的优点。

Description

一种高频低损耗MPP软磁合金粉芯的制备方法
技术领域
本发明属于软磁磁粉芯技术领域，具体涉及一种高频低损耗MPP软磁合金粉芯的制备方法。
背景技术
MPP软磁合金材料，是由17％的铁，81％的镍和2％的钼组成。和其它种类的软磁合金材料相比，具有较高的电阻率，高的温度稳定性，具有最宽的磁导率可选范围。特别适合回扫变压器，高Q滤波器、射频滤波器等，在要求高精度和高灵敏性的国防军工、医疗和尖端科技领域，起到不可替代的作用，目前国内制做的MPP软磁合金材料的综合磁特性普遍较差，尤其是和美日韩相比有着较大的差距。
科技的进步对电子器件的高频、高精度、高灵敏度和小型化提出了更高的要求，需要通过提升材料制备技术来提高材料的应用频率和降低材料的功耗等磁特性。目前普遍的制备方法是将MPP磁粉和有机树脂等绝缘混合包覆，成型、热处理等工艺，提高磁粉的电阻率。由于有机绝缘剂耐温低，热处理过程中绝缘剂挥发或低温处理，这些都会导致损耗或高频特性变差；
其它采用加入无机绝缘剂制备的磁粉，由于无机粘接剂存在包覆不均匀和附着力差的问题，不得不加大无机包覆剂的用量来达到绝缘效果，这样做出的磁芯特性差或不稳定等。
发明内容
针对上述技术问题，本发明采取新的方法和工艺进行粉末绝缘和热处理来提高电阻率，使其能够适应高频条件的应用。
本发明可以实现磁导率μi＝60±5％，低损耗Pv≤750mW/cm3，(100KHz，0.1T，25℃)和1兆赫兹高频特性。
具体是技术方案：
本发明提供一种高频低损耗MPP软磁合金粉芯的制备方法，具体包括以下步骤：
S1.根据MPP粉体粒径大小配比，用行星球磨机混合待用；
S1中，MPP粉体，按照粒径200目：300目：400目为0.5-2:1-3:5-8质量比例，用行星球磨机混合40分钟待用。
S2.按照质量份数配比浆料原料：硼酐15-40份、二氧化硅20-40份和氧化铝15-35份，加入二倍浆料原料质量的锆球和一倍浆料原料质量的酒精，在行星球磨机中磨成D50为0.5到1.5μm粒径的浆料；
S2中温度设定在500-650℃。
S3.称取上述浆料，为MPP磁粉质量的0.1到10％；浆料中加入硅烷偶联剂处理，硅烷偶联剂的加入量为MPP磁粉质量的0.1到10％；再添加树脂，树脂加入量为MPP磁粉质量的0.1到10％；
S3获得的浆料固含量为5-95％；
S4.将S3的浆料混合物加入到高堆积密度的MPP磁粉中，再加入分散剂，分散剂加入量为MPP磁粉质量的0.01到5％，均匀混合30-180分钟，干燥；
S5.利用热压成型技术成型得到磁芯胚，并把磁芯胚热处理。
S5中，磁芯胚在500到650℃温度及氮氢混合保护气氛下热处理0.5-10小时。
该方法制备的磁芯具有高的电阻率，低损耗，高的致密度和气孔少的优点。
本发明具有的有益效果：
1.在二氧化硅和氧化铝中加入硼酐，降低了混合物的熔点，为500-650℃，高温烧结使固体浆料熔化为液体，熔化的液体包覆在粉体表面，形成一层致密的陶瓷绝缘薄膜层，这样包覆膜层更薄，包覆更均匀。
2.膜层与大部分酸、碱不起化学反应，具有较强的抗腐蚀能力，具有更稳定的优点。
3.采用粉体颗粒度配比，可以使堆积密度更高，有利于低成型压力下就可以实现高的磁芯密度，气孔率更低，更容易做出高性能的磁芯。
4.相比加入的环氧树脂和其它的无机包覆剂，该专利解决了包覆均匀和老化问题，提高了器件的可靠性。
具体实施方式
结合实施例说明本发明的具体技术方案。
步骤一，MPP磁粉粒度配比：
按照比例分别称量MPP磁粉：200目200g、300目300g，400目500g，共1kg。无水乙醇1kg，称量锆球3kg，锆球直径为2.8mm，称好的锆球先水磨30分钟，再用洁净水洗干净并干燥后，装入气氛保护球磨罐中，充入N2，混合30分钟，取出分离锆球晾干待用；
步骤二，绝缘包覆浆料制备：
绝缘包覆浆料制备，分别称量硼酐6g、超细二氧化硅8g、氧化铝若干6g，，硅烷偶联剂10ml，分散剂5ml，加入酒精20g球磨，粒径D50控制到0.8μm；
步骤三，把制备好的绝缘包覆浆料加入混好的MPP磁粉中放入多角度变距混合机中均匀混合60分钟，晾干。
步骤四，把晾干的材料成型，并把磁芯在N2/H2混合保护气氛中烧结，烧结温度600℃，烧结时间3小时，自由降到室温测试。
步骤五，性能测试，把烧好的磁芯进行磁特性对比测试并记录数据如表1：
表1测试数据
项目 1 2 3 4 5
磁导率(1MHz) 60 60 58 62 57
功耗(mW/cm<sup>3</sup>)100K/100mT(25℃) 660 656 683 672 662
从测试结果看，本实施列磁芯磁导率和功耗达到了设计要求。
本发明的技术原理主要在于：
a、把绝缘性好的二氧化硅，氧化铝和硼酐配成一定的比例，放入到行星球磨机球磨，粒径磨到0.5到1.5μm，超细的粉体具有高的比表面积和熔点500-650℃。
b、在浆料中加入硅烷偶联剂，作用使浆料和各类树脂具有良好的相容性，吸附性能好，有利于后续粉体均匀包覆。
c、把配好的浆料按照需要比例加入到粉体中，经压制成型，然后在保护气氛中500-650℃烧结，浆料中的无机混合物熔化为液体，均匀包覆在粉体表面，形成一层均匀、致密，高绝缘的薄膜，提高了材料的电阻率，应用中降低了涡流损耗，提高了磁芯的应用频率；
a，b，c，配合作用，使无机粉体经过高温烧结熔化为液体，不仅解决了无机粉体不易均匀分散的问题，用较少的使用量就达到了有机树脂溶液对MPP粉末均匀包覆的效果；又解决了有机树脂耐温低，导致磁芯在应用过程中老化失效的问题。
MPP粉体粒度进行配比，提高了堆积密度，压制成型后磁芯的气孔率降低了5-15％，增加了磁性的理论密度,有利于提高磁性能。

Claims (5)

1.一种高频低损耗MPP软磁合金粉芯的制备方法，其特征在于，包括以下步骤：
S1.根据MPP粉体粒径大小配比，用行星球磨机混合待用；
S2.按照质量份数配比浆料原料：硼酐15-40份、二氧化硅20-40份和氧化铝15-35份，加入二倍浆料原料质量的锆球和一倍浆料原料质量的酒精，在行星球磨机中磨成D50为0.5到1.5μm粒径的浆料；
S3.称取上述浆料，为MPP磁粉质量的0.1到10％；浆料中加入硅烷偶联剂处理，硅烷偶联剂的加入量为MPP磁粉质量的0.1到10％；再添加树脂，树脂加入量为MPP磁粉质量的0.1到10％；
S4.将S3的浆料混合物加入到高堆积密度的MPP磁粉中，再加入分散剂，分散剂加入量为MPP磁粉质量的0.01到5％，均匀混合30-180分钟，干燥；
S5.利用热压成型技术成型得到磁芯胚，并把磁芯胚热处理。
2.根据权利要求1所述的一种高频低损耗MPP软磁合金粉芯的制备方法，其特征在于，S1中，MPP粉体，按照粒径200目：300目：400目为0.5-2:1-3:5-8质量比例，用行星球磨机混合40分钟待用。
3.根据权利要求1所述的一种高频低损耗MPP软磁合金粉芯的制备方法，其特征在于，S2中温度设定在500-650℃。
4.根据权利要求1所述的一种高频低损耗MPP软磁合金粉芯的制备方法，其特征在于，S3获得的浆料固含量为5-95％。
5.根据权利要求1所述的一种高频低损耗MPP软磁合金粉芯的制备方法，其特征在于，S5中，磁芯胚在500到650℃温度及氮氢混合保护气氛下热处理0.5-10小时。
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