CN112079633B - 一种宽温低比温度系数的镍锌高磁导率材料及其制备方法 - Google Patents
一种宽温低比温度系数的镍锌高磁导率材料及其制备方法 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 32
- QELJHCBNGDEXLD-UHFFFAOYSA-N nickel zinc Chemical compound [Ni].[Zn] QELJHCBNGDEXLD-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 230000005291 magnetic effect Effects 0.000 claims abstract description 45
- 230000035699 permeability Effects 0.000 claims description 38
- 238000005245 sintering Methods 0.000 claims description 15
- 239000007921 spray Substances 0.000 claims description 12
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 7
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims description 6
- 238000005469 granulation Methods 0.000 claims description 6
- 230000003179 granulation Effects 0.000 claims description 6
- 239000004576 sand Substances 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 4
- 239000002002 slurry Substances 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 3
- 238000009826 distribution Methods 0.000 claims description 2
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 claims 2
- 238000003801 milling Methods 0.000 claims 1
- 229910000859 α-Fe Inorganic materials 0.000 abstract description 8
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 abstract description 2
- 239000011324 bead Substances 0.000 abstract description 2
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 abstract 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 30
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 18
- 239000011787 zinc oxide Substances 0.000 description 15
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 239000000654 additive Substances 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- 229910001035 Soft ferrite Inorganic materials 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000008187 granular material Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229910003321 CoFe Inorganic materials 0.000 description 2
- 239000005751 Copper oxide Substances 0.000 description 2
- 229910003962 NiZn Inorganic materials 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 229910000431 copper oxide Inorganic materials 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- WJZHMLNIAZSFDO-UHFFFAOYSA-N manganese zinc Chemical compound [Mn].[Zn] WJZHMLNIAZSFDO-UHFFFAOYSA-N 0.000 description 2
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229910020599 Co 3 O 4 Inorganic materials 0.000 description 1
- 229910001053 Nickel-zinc ferrite Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- 230000005350 ferromagnetic resonance Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- -1 iron ion Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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Abstract
本发明属于软磁铁氧体技术领域，公开了一种宽温低比温度系数的镍锌高磁导率材料及其制备方法。本发明的宽温低比温度系数的镍锌高磁导率材料包含主成分和辅助成分，其中，所述主成分按Fe2O3、ZnO、NiO、CuO总量计算的含有47～49.8mol％的Fe2O3、11.6～15.6mol％的NiO和30～34.5mol％的ZnO，余量为CuO；辅助成分的含量以主成分的总重量计，包含0.01～0.3wt％的Co2O3、0.05～0.25wt％的SnO2和0.03～0.4wt％的Bi2O3。该材料具有磁导率高、Bs高、居里温度高等优点，可应用于电子电路宽带变压器、滤波电感、叠层磁珠等中，能够在很大程度上解决软磁铁氧体材料在极端条件下的应用限制。
Description
技术领域
本发明涉及软磁铁氧体技术领域，具体是涉及一种宽温低比温度系数的镍锌高磁导率材料及其制备方法。
背景技术
近年来，随着铁氧体在通信、IT产业、汽车产业、航空航天领域、舰船及国防武器装备系统等各行业的广泛应用，现代通信设备的户外设施、卫星等设备，不论在炎热的热带还是寒冷的寒带地区，不仅要求耐高温，还要承受严寒。这就要求所使用的元器件具有宽温、高稳定、长寿命的优良特性。
目前采用的NiZn软磁铁氧体材料磁导率最高只有500～700、居里温度只有90度、Bs 260mT以下，所以导致使用NiZn材料制作的产品在使用过程中会出现电感量低、能量转化效率低及使用温度低等缺点。
公开号为CN104529423A的中国专利公开了一种低温度系数抗应力镍锌软磁铁氧体材料，其主成分为氧化铁、氧化锌、氧化亚镍和氧化铜，副成分为纳米SiO2、纳米Bi2O3、Co3O4、TiO2、滑石粉0.10～0.45w，该发明提供了一种具有较高磁导率的比温度系数的镍锌铁氧体制备方法，但该发明专利的铁氧体磁导率μi较小，不到600，达不到高磁导率的要求。
公开号为CN109369168A的中国专利公开了一种铁氧体组合物，其主成分是以Fe2O3换算为40.0～49.8摩尔％的氧化铁、以CuO换算为5.0～14.0摩尔％的氧化铜、以ZnO换算为0～32.0摩尔％的氧化锌、余量为氧化镍所构成，相对于所述主成分100重量％，含有以SnO2换算为0.5～4.0重量％的氧化锡、以Bi2O3换算为0.10～1.00重量％的氧化铋、以Co3O4换算为0.21～3.00重量％的氧化钴作为副成分，但其发明的材料磁导率只有500左右，达不到高磁导率的要求。
公开号为CN109485399A的中国专利公开了一种用于NFC和无线充电的NiCuZn铁氧体磁片，公开了由48～49mol％Fe2O3、8～12mol％CuO、15～18mol％NiO、余量ZnO，掺杂0.1～1wt％Bi2O3、0.01～0.1wt％Co2O3、0.05～0.3％SnO2的铁氧体磁片，所述铁氧体磁片具有高饱和磁感应强度、高剩余磁感应强度、高剩磁比、低矫顽力、低介电损耗和低铁磁共振线宽等优异特性，但其主要用于NFC和无线充电，且低温度条件下磁导率偏低，达不到极端条件下的应用要求。
发明内容
本发明的目的是为了克服上述背景技术的不足，提供一种宽温低比温度系数的镍锌高磁导率材料及其制备方法，该材料具有磁导率高、Bs高、居里温度高等优点，可应用于电子电路宽带变压器、滤波电感、叠层磁珠等中，能够在很大程度上解决软磁铁氧体材料在极端条件下的应用限制。
为达到本发明的目的，本发明的宽温低比温度系数的镍锌高磁导率材料包含主成分和辅助成分，其中，所述主成分按Fe2O3、ZnO、NiO、CuO总量计算的含有47～49.8mol％的Fe2O3、11.6～15.6mol％的NiO和30～34.5mol％的ZnO，余量为CuO；辅助成分的含量以主成分的总重量计，包含0.01～0.3wt％的Co2O3、0.05～0.25wt％的SnO2和0.03～0.4wt％的Bi2O3。
优选地，在本发明的一些实施例中，所述主成分按Fe2O3、ZnO、NiO、CuO总量计算的含有48～49.5mol％的Fe2O3、12～15mol％的NiO、30～33mol％的ZnO和5.6～7.0mol％的CuO。
优选地，在本发明的一些实施例中，辅助成分的含量以主成分的总重量计，包含0.25wt％的Co2O3、0.10wt％的SnO2和0.15wt％的Bi2O3。
进一步地，本发明还提供了一种前述宽温低比温度系数的镍锌高磁导率材料的制备方法，所述制备方法包括配料、球磨、预烧、二次砂磨、喷雾造粒、成型和辊道炉烧结。
优选地，所述球磨中采用球磨机，使得料浆的粒度分布D50：0.9～1.2μm，D99：1.5～3.6μm。
优选地，所述辊道炉烧结中采用辊道窑低温快速空气气氛烧结方式，可以大规模量产磁芯样品，实现低成本的生产方式。
本发明的宽温低比温度系数的镍锌高磁导率材料具有如下性能：
μi[-55℃]：600～700；μi[25℃]：700～900；μi[125℃]：650～1000(@128KHz，0.25mT)；
Bs[25℃]：300～400mT(@50Hz，1194A/m)；
Tc：120～150℃；
ρ：≥108Ω·m；
比磁导率温度系数αμr[-55℃～125℃]：<2×10-6/℃(测试条件f＝128kHz B＝0.25mT)。
因为本发明的宽温低比温度系数的镍锌高磁导率材料具有上述优良的性能，解决了材料在-55℃到125℃，频率128kHz电感变化大的问题，从而提高了电感器在极端低温/高温条件下的输出稳点性，在产品的实际应用上可以使器件在非常宽的温度条件下及更高的频率下使用。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合实施例，对本发明进行进一步详细说明。本发明的附加方面和优点将在下面的描述中部分给出，部分将从下面的描述中变得明显，或通过本发明的实践了解到。应当理解，以下描述仅仅用以解释本发明，并不用于限定本发明。
本文中所用的术语“包含”、“包括”、“具有”、“含有”或其任何其它变形，意在覆盖非排它性的包括。例如，包含所列要素的组合物、步骤、方法或制品不必仅限于那些要素，而是可以包括未明确列出的其它要素或此种组合物、步骤、方法或制品所固有的要素。
由于本发明的宽温低比温度系数的镍锌高磁导率材料可以使用传统工艺进行批量生产，故以下实施例和对比例均采用统一的生产工艺进行生产，具体工艺如下：
1.配料
按照设计配比，分别以Fe2O3、NiO、ZnO、CuO形式计算比例，称取Fe2O3、NiO、ZnO、CuO四种原料，然后在球磨机中加入去离子水进行混合和破碎，时间30-90分钟，循环混合10-40分钟后进行喷雾造粒；
2.预烧
将喷雾造粒料放入预烧炉中，在700～950℃下进行预烧，时间2～6个小时；
3.砂磨
将预烧后所得粉料放入砂磨机中加入添加剂、粘合剂、分散剂，砂磨时间2～3小时；
4.喷雾造粒和成型
在砂磨料中加入0.10-0.14wt％的PVA，以及0.0015-0.0025wt％的消泡剂，然后在喷雾塔中喷雾造粒成50～200μm的颗粒；
将不同实施例与对比例的颗粒成型成密度为3.00～3.15g/cm3的H25*15*8mm标准样环毛坯；
5.烧结
烧结曲线：常温到空气最高温度900-1200℃，升温速率0.3～2℃/min，保温3-8h；降温到500℃，降温速率为0.5-2.5℃/min；再降温到常温，降温速率为1-3℃/min。
6.测试
将烧结好的样环用惠普的HP4284A LCR测试仪进行电感测试，测试条件分别为：-55℃、25℃、125℃，在f＝128kHz，u＝0.1v的条件下测试电感并换算成磁导率；将烧结好的外径25、内径15的磁环用Agilent E4990A测试磁导率μi，用CH3302和烘箱测试居里温度Tc，用日本岩崎公司的SY8218仪器进行磁通密度Bs的测试。
实施例1
具体制备工艺如下：
(1)配料
按照设计配比，分别以称取49mol％Fe2O3、12.5mol％NiO、32.5mol％ZnO和6mol％CuO四种原料，然后在球磨机中加入去离子水进行混合和破碎，其中料水比为1:1，循环球磨40分钟，出浆料后进行喷雾造粒；
(2)预烧
将喷雾造粒料放入预烧炉中，预烧炉升温速率为2℃/min，在850℃下进行预烧，保温时间3个小时；
(3)砂磨
将预烧后所得粉料放入砂磨机中，再加入适量的添加剂、粘合剂、分散剂和纯水，其中预烧料：水：粘合剂：分散剂量之比为100:100:10:1；加料时，先采用低转速研磨(约10min)，再高速砂磨时间2小时；研磨后，把浆料转移到搅拌罐；
(4)喷雾造粒和成型
在搅拌罐中加入0.10-0.14wt％的PVA，以及0.0015-0.0025wt％的消泡剂，然后在喷雾塔中喷雾造粒成50～200μm的颗粒；
将不同实施例与对比例的颗粒成型成密度为3.00～3.15g/cm3的H25*15*8mm标准样环毛坯；
(5)烧结
烧结曲线：在空气环境中烧结，常温到最高温度1090℃，升温速率1.5℃/min，保温6h；降温到500℃，降温速率为2.2℃/min；再降温到常温，降温速率为2.8℃/min。
(6)测试
将烧结好的样环用惠普的HP4284A LCR测试仪进行电感测试，测试条件分别为：-55℃、25℃、125℃，在f＝128kHz，u＝0.1v的条件下测试电感并换算成磁导率；将烧结好的外径25mm、内径15mm的磁环用Agilent E4990A测试磁导率μi，用CH3302和烘箱测试居里温度Tc，用日本岩崎公司的SY8218仪器进行磁通密度Bs的测试。
以下表1和表2的实施例和对比例是为了更好的说明本发明而列举的实施例和对比例，但是本发明并不限于这些实施例。
表1实施例1-8和对比例1-9主成分和添加剂配方及性能测试结果
表2中，对比例10-17的主成分与实施例1相同。
表2实施例1和对比例10-17的性能测试表
由上述测试结果可知，本发明的宽温低比温度系数的锰锌高磁导率材料为了得到较高的磁导率值和Bs值，是通过增加Fe2O3的含量以及减少ZnO的含量来实现，由于需要保持-55℃的磁导率，Fe2O3、ZnO和NiO的含量需要搭配调整来实现。并且，本发明为了得到在-55℃到125℃温度下均有较高的磁导率值和Bs值的锰锌高磁导率材料，不仅需要控制主成分Fe2O3、ZnO和NiO的含量，还需要控制添加剂的种类和含量，需要主成分和添加剂搭配调整来实现，如对比例16，其引入过量的Co2O3和SnO2，降低了室温下的烧结磁导率，这主要因为过多的Co3+、Sn4+将会取代B位铁离子，使其Ms降低，进而导致其磁导率和Bs偏低。又如对比例17，其引入SiO2、氧化钛和滑石粉，所得铁氧体材料虽然有宽温低比温度系数的性能，但其磁导率只有572，远远低于840，Bs也低于340mT，这会导致材料的叠加性能不佳。
具体的：
1.当Fe2O3、NiO和ZnO的含量在本发明范围内时，可以同时满足磁导率和宽温的要求，当Fe2O3含量低于本发明范围时，-55℃的磁导率将低于600；当Fe2O3的含量高于本发明范围时，125℃的磁导率将高于1050，也就是高于室温下磁导率的25％，从而不可兼顾-55℃和125℃的磁导率变化；
2.副成分Co2O3的主要作用是：通过添加Co2O3可以生成K1正值很大的CoFe2O4，由于Co3+的K1值很大，所以组成中CoFe2O4含量的多少在很大程度上决定了材料的Ⅱ峰位置，从而可以兼顾-55℃和125℃的磁导率变化；
3.由于Co3+不仅对K1有影响，而且会使K2增加，如果Fe2+或Co3+过量的话，会导致高温下K1值远大于零，而且随着温度的升高，K1值增大，对应的μi～T曲线在高温区明显下降，出现较大的负温度系数，综合利用Fe2+和Co3+对K1的补偿作用，若Fe2+和Co3+的比例适当，K1值可能有多个补偿点，对应的μi～T曲线在较宽的温度范围较平坦，由此可获得宽温低比温度系数材料，另外磁滞系数与磁导率有一定的对应关系，磁导率高的材料磁滞系数亦小，相反磁导率低的材料磁滞系数大，而磁导率与K1的倒数呈正比，显然，磁滞系数与K1有着内在的联系，调节Fe2+与Co3+的含量，使K1值趋近于零，可减小磁滞系数，提高磁导率。
本领域的技术人员容易理解，以上所述仅为本发明的实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。
Claims (2)
1.一种宽温低比温度系数的镍锌高磁导率材料，其特征在于，所述宽温低比温度系数的镍锌高磁导率材料包含主成分和辅助成分，其中，所述主成分按Fe2O3、ZnO、NiO、CuO总量计算的含有48～49.5mol％的Fe2O3、12～15mol％的NiO、30～33mol％的ZnO和5.6～7.0mol％的CuO；辅助成分的含量以主成分的总重量计，包含0.04～0.25wt％的Co2O3、0.05～0.2wt％的SnO2和0.1～0.2wt％的Bi2O3；
上述宽温低比温度系数的镍锌高磁导率材料的制备方法包括配料、球磨、预烧、二次砂磨、喷雾造粒、成型和辊道炉烧结；
所述球磨中采用球磨机，使得料浆的粒度分布D50：0.9～1.2μm，D99：1.5～3.6μm。
2.根据权利要求1所述的宽温低比温度系数的镍锌高磁导率材料，所述辅助成分的含量以主成分的总重量计，包含0.25wt％的Co2O3、0.10wt％的SnO2和0.15wt％的Bi2O3。
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