CN114133233B - 一种高频高Bs复合铁氧体材料及其制备方法 - Google Patents
一种高频高Bs复合铁氧体材料及其制备方法 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 45
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 36
- 239000002131 composite material Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 239000006247 magnetic powder Substances 0.000 claims abstract description 55
- 238000005245 sintering Methods 0.000 claims abstract description 53
- JIYIUPFAJUGHNL-UHFFFAOYSA-N [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] JIYIUPFAJUGHNL-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 claims abstract description 29
- 229910001053 Nickel-zinc ferrite Inorganic materials 0.000 claims abstract description 26
- WJZHMLNIAZSFDO-UHFFFAOYSA-N manganese zinc Chemical compound [Mn].[Zn] WJZHMLNIAZSFDO-UHFFFAOYSA-N 0.000 claims abstract description 25
- QELJHCBNGDEXLD-UHFFFAOYSA-N nickel zinc Chemical compound [Ni].[Zn] QELJHCBNGDEXLD-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000004576 sand Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000003825 pressing Methods 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- 238000000713 high-energy ball milling Methods 0.000 claims abstract description 7
- 230000004907 flux Effects 0.000 claims abstract description 6
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 claims description 22
- 239000002245 particle Substances 0.000 claims description 18
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical group O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 17
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 15
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 12
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 10
- 239000012467 final product Substances 0.000 claims description 8
- 239000012535 impurity Substances 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 238000003801 milling Methods 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 6
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Inorganic materials O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 6
- 229910018605 Ni—Zn Inorganic materials 0.000 claims description 4
- 238000007670 refining Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims 2
- 239000013078 crystal Substances 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 2
- 239000002105 nanoparticle Substances 0.000 abstract 1
- 229910019714 Nb2O3 Inorganic materials 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000011162 core material Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
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- 239000011258 core-shell material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
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- 238000013508 migration Methods 0.000 description 1
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- 238000000465 moulding Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000013139 quantization Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
本发明提供了一种高频高Bs复合铁氧体材料，其制备方法为1）分别制备锰锌铁氧体和镍锌铁氧体的预烧料，2）分别砂磨并加入辅助成分；3）分别进行二次预烧；4）分别通过砂磨和高能球磨制备成锰锌微米级磁粉和镍锌纳米级磁粉；5）在砂磨机中混合均匀后压制成型；6）在气氛炉中烧结。本发明通过主成分、辅助成分、助熔剂及其他掺杂成分的配方设计，并结合二次预烧、砂磨和高能球磨、混合等工艺设计，最终形成了内层是MnZnFeO4外层是NiZnFeO4的晶粒壳层结构，外层的NiZnFeO4结构增大了晶界电阻率，内层的MnZnFeO4结构又增大了晶粒的饱和磁通密度，最终制备了一种高频高Bs的复合铁氧体材料。
Description
技术领域
本发明涉及磁性材料技术领域，具体涉及一种复合铁氧体材料及其制备工艺。
背景技术
随着电子设备的小型化，软磁材料的应用也在向着高频高Bs和低损耗方向发展。一方面，随着市场对更小、更轻和更薄电子设备的需求，为减小磁路的体积（重量），要求磁芯在高频率（1~10MHz）和高磁通密度下进行处理大信号或功率传输时，产生较低的能量损耗，即需要更高频率（1~10MHz）下具有更高磁导率和更低功率损耗的软磁铁氧体材料；另一方面，在许多电路中，除交流（AC）成份外，又不得不兼容大的直流（DC）成份，这就要求磁芯材料必须有高的饱和磁通密度来提升抗直流叠加的能力。
锰锌功率铁氧体兼具高Bs和低损耗的特性，但因电阻率相对较低，在高频下容易产生涡流损耗，因此其应用频段和截止频率相比镍锌铁氧体来说较低；而镍锌铁氧体兼具高频（1~100MHz）和低损耗的特性，但是其饱和磁通密度和居里温度相比锰锌铁氧体来说较低。公开号为CN110467450A的专利公开了一种锰镍锌铁的四元配方体系，这种四元配方是通过改变元素的AB占位，增强AB位超交换作用，提升锰锌铁氧体的居里温度，从而达到提升Bs的目的，采用这种方法虽然有助于提升饱和磁通密度，但由于加氧化镍会使二峰右移，因此会使得常温磁导率有所下降。而若将锰锌和镍锌铁氧体两相复合，或可得到一种结合两者优点的高频高Bs低损耗铁氧体材料。公开号为CN107352991A的专利公开了一种核壳结构锰锌/镍锌复合铁氧体，是用化学共沉淀法制备了一种锰锌铁氧体核及镍锌铁氧体壳的复合铁氧体，从而制备了一种高频下低功率损耗，高截止频率的铁氧体，但此方法与本发明中的氧化物法完全不一样，生产成本高，不易量化控制。
发明内容
本发明提供一种高频高Bs复合铁氧体材料及其制备方法，本发明主要步骤如下：
1）通过配料、混合、预烧，分别制备锰锌铁氧体和镍锌铁氧体的预烧料，预烧温度为750~950℃，其中，锰锌铁氧体的成分为Fe2O3、ZnO和MnO，镍锌铁氧体的成分为Fe2O3、ZnO和NiO；
2）将锰锌铁氧体预烧料掺入助熔剂后砂磨至平均粒径0.5~3μm，助熔剂为Bi2O3、CuO、MoO3中的一种或多种，将镍锌铁氧体预烧料掺入细化晶粒的纳米杂质及辅助成分，砂磨至平均粒径0.5~3μm，细化晶粒的纳米杂质包括Nb2O5、CaCO3中的一种或两种，辅助成分包括Co2O3、TiO2、ZrO2中的一种或多种；
3）将步骤2中获得的锰锌磁粉和镍锌磁粉二次预烧，预烧温度为800~1000℃；
4）将二次预烧后的锰锌磁粉砂磨至平均粒径0.5-3μm，将二次预烧后的镍锌磁粉高能球磨至平均粒径100-500nm；
5）将步骤4制备的两种磁粉在砂磨机中混合均匀后造粒压制成T25*15*7.5生坯，砂磨时间为10~15min；
6）将压制好的生坯在氮气窑炉中烧结得到最终产品，烧结温度为1000~1300℃。
本发明解决其技术问题的技术方案进一步还包括：
所述步骤1中锰锌铁氧体的成分配比为：Fe2O3 65~75wt%、ZnO 1~10 wt%、余量为MnO，镍锌铁氧体的成分配比为Fe2O3 62~70wt%、ZnO 10~25 wt%、余量为NiO；
所述步骤1中，锰锌铁氧体的预烧温度为750-900℃，镍锌铁氧体的预烧温度为800-950℃；
所述步骤2中助熔剂为Bi2O3、CuO、MoO3中的一种或多种，成分含量为：Bi2O3 200-500ppm、CuO 500~5000ppm、MoO3 200-500ppm，细化晶粒的纳米杂质包括Nb2O5、CaCO3中的一种或两种，成分含量为：Nb2O5 100~400ppm、CaCO3 100-800ppm，辅助成分包括Co2O3、TiO2、ZrO2中的一种或多种，成分含量为：Co2O3 1000~4000ppm、TiO2 1000~4000ppm、ZrO2100 ~600ppm；
所述步骤3中锰锌磁粉预烧温度为800-950℃，镍锌磁粉预烧温度为850-1000℃；
所述步骤5中锰锌磁粉和镍锌磁粉混合的质量比范围为3:7~7:3；
所述步骤6中优选的烧结温度是1100-1250℃，保温时间2-4h，保温阶段平衡氧含量为1~5%。
本发明通过将添加辅助成分之后的锰锌铁氧体和镍锌铁氧体二次预烧，目的是将助熔剂和细化晶粒的纳米杂质分别固溶于锰锌铁氧体和镍锌铁氧体内，然后将锰锌铁氧体微米级磁粉和镍锌铁氧体纳米级磁粉均匀混合后进行造粒压制成型，形成镍锌纳米磁粉包覆锰锌磁粉的生坯，最后将其进行烧结，通过掺杂在锰锌磁粉中的助熔剂产生液相加速离子扩散，由于晶界总是朝着它们自身的曲率中心迁移，促使锰锌铁氧体在晶粒边界扩散迁移过程中吸收镍锌纳米磁粉而长大，同时，通过掺杂在镍锌磁粉中的纳米杂质抑制晶粒进一步扩大。因锰锌铁氧体和镍锌铁氧体同为尖晶石相，所以最终形成了同一晶粒中内层是MnZnFeO4而外层是NiZnFeO4的晶粒壳层结构，外层的NiZnFeO4提供了高的晶界电阻率，降低了整个晶粒的涡流损耗，而内层的MnZnFeO4提供了高的饱和磁通密度，这种晶粒壳层结构实现了锰锌铁氧体和镍锌铁氧体材料的优点共享和缺点互补，以便获得高频高Bs复合铁氧体材料。
本发明的有益效果是：
⑴ 本发明提供了一种锰锌铁氧体和镍锌铁氧体两相复合的方法，通过调节两种磁粉的质量比，调整铁氧体的Bs和截止频率，实现性能的可调控，衔接了锰锌铁氧体和镍锌铁氧体应用频段之间的空缺，尤其是5-10MHz区间；
⑵ 本发明通过制备尖晶石相的晶粒壳层结构，初始磁导率达到1201的同时，常温Bs达到473且截止频率达到7.3MHz，提供了一种高频高Bs复合铁氧体材料及其制备方法。
具体实施方式
本实施例为本发明优选实施方式，基于本发明的实施例，其他技术人员在没有做出创造性劳动前提下所获得的其他所有实施例都属于本发明的保护范围。
实施例1
本实施例按照如下方法制备高频高Bs复合铁氧体材料：
1）按照Fe2O3 72wt%、ZnO 4wt%、MnO 24wt%和Fe2O3 66wt%、ZnO 22wt%、NiO 12wt%的比例分别配料、混合，然后分别在800℃和850℃预烧，制备锰锌铁氧体和镍锌铁氧体的预烧料；
2）将锰锌铁氧体预烧料掺入CuO 1000ppm、Bi2O3 300ppm并砂磨至平均粒径0.5~3μm；将镍锌铁氧体预烧料掺入纳米Nb2O3 250ppm、CaO 500ppm、Co2O3 1000ppm并砂磨至平均粒径0.5~3μm；
3）将步骤2中获得的的锰锌磁粉和镍锌磁粉再次预烧，预烧温度分别为850℃、900℃；
4）将二次预烧的磁粉分别通过砂磨和高能球磨制备成0.5~3μm的锰锌磁粉和100~500nm的镍锌磁粉；
5）将锰锌和镍锌两种磁粉按照质量比5:5在砂磨机中混合均匀后造粒压制成T25*15*7.5生坯，砂磨时间为15min；
6）在1180℃、保温2h、保温段氧分压4%的条件下烧结生坯得到最终产品。
实施例2
本实施例按照如下方法制备高频高Bs复合铁氧体材料：
1）按照Fe2O3 72wt%、ZnO 4wt%、MnO 24wt%和Fe2O3 66wt%、ZnO 22wt%、NiO 12wt%的比例分别配料、混合，然后分别在800℃和850℃预烧，制备锰锌铁氧体和镍锌铁氧体的预烧料；
2）将锰锌铁氧体预烧料掺入CuO 1000ppm、Bi2O3 300ppm并砂磨至平均粒径0.5~3μm；将镍锌铁氧体预烧料掺入纳米Nb2O3250ppm、CaO 500ppm、Co2O3 1000ppm并砂磨至平均粒径0.5~3μm；
3）将步骤2中获得的的锰锌磁粉和镍锌磁粉再次预烧，预烧温度分别为850℃、900℃；
4）将二次预烧的磁粉分别通过砂磨和高能球磨制备成0.5~3μm的锰锌磁粉和100~500nm的镍锌磁粉；
5）将锰锌和镍锌两种磁粉按照质量比3:7在砂磨机中混合均匀后造粒压制成T25*15*7.5生坯，砂磨时间为15min；
6）在1180℃、保温2h、保温段氧分压4%的条件下烧结生坯得到最终产品。
实施例3
本实施例按照如下方法制备高频高Bs复合铁氧体材料：
1）按照Fe2O3 72wt%、ZnO 4wt%、MnO 24wt%和Fe2O3 66wt%、ZnO 22wt%、NiO 12wt%的比例分别配料、混合，然后分别在800℃和850℃预烧，制备锰锌铁氧体和镍锌铁氧体的预烧料；
2）将锰锌铁氧体预烧料掺入CuO 1000ppm、Bi2O3 300ppm并砂磨至平均粒径0.5~3μm；将镍锌铁氧体预烧料掺入纳米Nb2O3250ppm、CaO 500ppm、Co2O3 1000ppm并砂磨至平均粒径0.5~3μm；
3）将步骤2中获得的的锰锌磁粉和镍锌磁粉再次预烧，预烧温度分别为850℃、900℃；
4）将二次预烧的磁粉分别通过砂磨和高能球磨制备成0.5~3μm的锰锌磁粉和100~500nm的镍锌磁粉；
5）将锰锌和镍锌两种磁粉按照质量比7:3在砂磨机中混合均匀后造粒压制成T25*15*7.5生坯，砂磨时间为15min；
6）在1180℃、保温2h、保温段氧分压4%的条件下烧结生坯得到最终产品。
对比例1
本实施例按照如下方法制备高频高Bs复合铁氧体材料：
1）按照Fe2O3 72wt%、ZnO 4wt%、MnO 24wt%和Fe2O3 66wt%、ZnO 22wt%、NiO 12wt%的比例分别配料、混合，然后分别在850℃和900℃预烧，制备锰锌铁氧体和镍锌铁氧体的预烧料；
2）将锰锌和镍锌两种磁粉按照质量比5:5均匀混合，并掺入辅助成分CuO1000ppm、Bi2O3 300ppm、Nb2O3250ppm、CaO 500ppm、Co2O3 1000ppm后，在砂磨机中砂磨至平均粒径0.5~3μm；
3）将磁粉造粒压制成T25*15*7.5生坯；
4）在1180℃、保温2h、保温段氧分压4%的条件下烧结生坯得到最终产品。
对比例2
本实施例按照如下方法制备高频高Bs复合铁氧体材料：
1）按照Fe2O3 72wt%、ZnO 4wt%、MnO 24wt%的比例配料、混合，然后在850℃下预烧，制备锰锌铁氧体预烧料；
2）将锰锌铁氧体预烧料掺入CuO 1000ppm、Bi2O3 300ppm、Nb2O3250ppm、CaO500ppm、Co2O3 1000ppm并砂磨至平均粒径0.5~3μm；
3）将磁粉造粒压制成T25*15*7.5生坯；
4）在1180℃、保温2h、保温段氧分压4%的条件下烧结生坯得到最终产品。
对比例3
本实施例按照如下方法制备高频高Bs复合铁氧体材料：
1）按照Fe2O3 66wt%、ZnO 22wt%、NiO 12wt%的比例配料、混合，然后在900℃下预烧，制备镍锌铁氧体预烧料；
2）将镍锌铁氧体预烧料掺入CuO 1000ppm、Bi2O3 300ppm、Nb2O3250ppm、CaO500ppm、Co2O3 1000ppm并砂磨至平均粒径0.5~3μm；
3）将磁粉造粒压制成T25*15*7.5生坯；
4）在1180℃、保温2h、保温段氧分压4%的条件下烧结生坯得到最终产品。
下表中μi、Bs和fr均为常温下测试结果，m为锰锌磁粉与镍锌磁粉混合的质量比。
Claims (9)
1.一种高频高Bs复合铁氧体材料的制备方法，其特征在于，制备方法包括以下步骤：
1）通过配料、混合、预烧，分别制备锰锌铁氧体和镍锌铁氧体的预烧料，预烧温度为750~950℃，其中，锰锌铁氧体的成分为Fe2O3、ZnO和MnO，镍锌铁氧体的成分为Fe2O3、ZnO和NiO；
2）将锰锌铁氧体预烧料掺入助熔剂后砂磨至平均粒径0.5~3μm，助熔剂为Bi2O3、CuO、MoO3中的一种或多种，将镍锌铁氧体预烧料掺入细化晶粒的纳米杂质及辅助成分砂磨至平均粒径0.5~3μm，细化晶粒的纳米杂质包括Nb2O5、CaCO3中的一种或两种，辅助成分包括Co2O3、TiO2、ZrO2中的一种或多种；
3）将步骤2） 中获得的锰锌磁粉和镍锌磁粉二次预烧，预烧温度为800~1000℃；
4）将二次预烧后的锰锌磁粉砂磨至平均粒径0.5-3μm，将二次预烧后的镍锌磁粉高能球磨至平均粒径100-500nm；
5）将步骤4） 制备的两种磁粉在砂磨机中混合均匀后造粒压制成生坯；
6）将压制好的生坯在气氛炉中烧结得到最终产品，烧结温度为1000~1300℃。
2.根据权利要求1所述的高频高Bs复合铁氧体材料的制备方法，其特征在于，所述步骤1） 中，锰锌铁氧体的成分配比为Fe2O3 65~75wt%、ZnO 1~10 wt%、余量为MnO，镍锌铁氧体的成分配比为Fe2O3 62~70wt%、ZnO 10~25 wt%、余量为NiO。
3.根据权利要求1所述的高频高Bs复合铁氧体材料的制备方法，其特征在于，所述步骤1） 中，锰锌铁氧体的预烧温度为750-900℃，镍锌铁氧体的预烧温度为800-950℃。
4.根据权利要求1所述的高频高Bs复合铁氧体材料的制备方法，其特征在于，所述步骤2） 中助熔剂为Bi2O3、CuO、MoO3中的一种或多种，成分含量为Bi2O3 200-500ppm、CuO 500~5000ppm、MoO3 200-500ppm；细化晶粒的纳米杂质包括Nb2O5、CaCO3中的一种或两种，成分含量为Nb2O5 100~400ppm、CaCO3 100-800ppm；辅助成分包括Co2O3、TiO2、ZrO2中的一种或多种，成分含量为Co2O3 1000~4000ppm、TiO2 1000~4000ppm、ZrO2100 ~600ppm。
5.根据权利要求1所述的高频高Bs复合铁氧体材料的制备方法，其特征在于，所述步骤3） 中锰锌磁粉预烧温度为800-950℃，镍锌磁粉预烧温度为850-1000℃。
6.根据权利要求1所述的高频高Bs复合铁氧体材料的制备方法，其特征在于，所述步骤5） 中锰锌磁粉和镍锌磁粉混合的质量比范围为3:7~7:3。
7.根据权利要求1所述的高频高Bs复合铁氧体材料的制备方法，其特征在于，所述步骤5） 中，砂磨时间为10~15min。
8.根据权利要求1所述的高频高Bs复合铁氧体材料的制备方法，其特征在于，所述步骤6） 中烧结温度是1100-1250℃，保温时间2-4h，保温阶段平衡氧含量为1~5%。
9.根据权利要求1所述的制备方法制造的高频高Bs复合铁氧体材料，其特征在于，材料具有一种内层为MnZnFeO4、外层为NiZnFeO4的晶粒壳层结构。
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