CN109485403A - 一种高Bs低损耗软磁铁氧体材料及其制备方法 - Google Patents
一种高Bs低损耗软磁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 43
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 24
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 17
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 16
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000004576 sand Substances 0.000 claims abstract description 16
- 239000004615 ingredient Substances 0.000 claims abstract description 15
- 238000003801 milling Methods 0.000 claims abstract description 11
- 239000002019 doping agent Substances 0.000 claims abstract description 9
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 8
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 5
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 5
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 5
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 5
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 4
- 238000005245 sintering Methods 0.000 claims description 15
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 238000000280 densification Methods 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 5
- 235000020985 whole grains Nutrition 0.000 claims description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 3
- 238000000748 compression moulding Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000011236 particulate material Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 239000002002 slurry Substances 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000011701 zinc Substances 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- 238000000465 moulding Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 13
- 230000004907 flux Effects 0.000 description 6
- 230000035699 permeability Effects 0.000 description 6
- 239000000047 product Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
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- 238000000227 grinding Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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Abstract
本发明提供了一种高Bs低损耗软磁铁氧体材料,所述软磁铁氧体材料各主料包括:Fe2O3:58.0~62.0mol%,ZnO:12.0~14.0mol%,NiO:1.0~4.0mol%,余量为MnO。按重量百分比,并以预烧后的主料为参考基准,以氧化物计算,掺杂剂包括SiO2:0.00~0.01wt%,CaCO3:0.01~0.12wt%,ZrO2:0.01~0.05wt%,Nb2O5:0.01~0.03wt%,Ta2O5:0.005~0.02wt%;然后依次通过配方、一次砂磨、预烧、掺杂、二次砂磨、成型和烧结,即得所述磁环样品。材料具有高Bs低损耗特性,能满足电源变压器小型化和高效率化的要求。
Description
技术领域
本发明属于软磁铁氧体材料技术领域,具体涉及一种高Bs低损耗软磁铁氧体材料及其制备方法。
背景技术
随着便携电子设备的广泛应用,电子产品朝着轻、薄、短、小方向发展已经成为必然的趋势,促使电源***向轻、薄、小和高效率方向发展,要求电源变压器承载更大的功率密度,即要求进一步提高磁心材料的饱和磁通密度、降低损耗。为对应电源变压器的要求,开发对应的高Bs低损耗软磁铁氧体材料非常必要。
在国内己有一些相关高Bs低损耗软磁铁氧体材料及其制备方法的专利,具体如下:
(1) 在中国公开的专利 CN1294099A 中,公开了一种高温高Bs功率铁氧体材料,其通过NiO 取代MnO提高材料的Bs,但是其100℃、1194A/m下的Bs仅为 440mT;
(2) 在中国公开的专利CN101429016A 中,公开了一种MnZn功率铁氧体材料,其居里温度为280℃,100℃、1194A/m下的 Bs为460mT,是现有材料中 Tc和Bs均较高的材料,具有较强的市场竞争力;
(3) 在中国公开的专利 CN1890197A 中,公开了一种高温超高Bs MnZn功率铁氧体材料,其主配方为:Fe2O3:63-80mol%,ZnO:3-15mol%,余为 MnO,辅助成分包括 CaO、Si02,在1175℃下保温 8小时。获得的铁氧体材料性能为:100 ℃下,Bs为520mT,但其损耗太高,在50kHz,150mT下的损耗高达1100kW/m3;
(4) 在中国公开的专利CN103214233A中,公开了一种高Tc、宽温超高Bs MnZn铁氧体材料及制备方法,属于铁氧体材料制备技术领域。本发明的铁氧体材料由主料和掺杂剂组成,特征在于,主料包括:58.0~62.0mol% Fe2O3,10.0~15.0mol%ZnO,4.0~6.0mol%NiO,余量为MnO;按重量百分比,并以预烧后的主料为参考基准,以氧化物计算,掺杂剂包括:Mo03:0.001~0.30wt%、Bi203:0.01~0.40wt%、Sn02:0.001~0.05wt%、Nb205:0.001~0.05wt%、Ta2O5:0.001~0.20wt%。本发明具有高居里温度(Tc≥320℃)、宽温高Bs (25℃,Bs≥600mT; 100℃,Bs≥490mT)及较低损耗(100℃、100kHz 200mT,PL≤800kW/m3)等特性。
发明内容
针对电源变压器小型化和高效率化的要求,本发明的目的是提供一种高Bs低损耗软磁铁氧体材料。
为了达到上述目的,本发明采取以下的技术方案:一种高Bs低损耗软磁铁氧体材料,所述软磁铁氧体材料各主料包括: Fe2O3:58.0~62.0mol%,ZnO: 12.0~14.0mol%,NiO:1.0~4.0mol%,余量为MnO。
按重量百分比,并以预烧后的主料为参考基准,以氧化物计算,掺杂剂包括SiO2:0.00~0.01wt%,CaCO3:0.01~0.12wt%,ZrO2:0.01~0.05wt%,Nb2O5:0.01~0.03wt%,Ta2O5:0.005~0.02wt%。
作为一种优选,所述成分优选Fe2O3:60.0mol%,ZnO:13.0mol%,NiO:3.0mol%,MnO:24.0 mol%。掺杂剂优选SiO2:0.005wt%,CaCO3:0.09wt%,ZrO2:0.04wt%,Nb2O5:0.02wt%,Ta2O5:0.01wt%。
上述配方的制备方法包括有以下步骤:配方、一次砂磨、预烧、掺杂、二次砂磨、成型和烧结,其中:
(1)配方:按如下主成分配比Fe2O3:58.0~62.0mol%,ZnO:12.0~14.0mol%,NiO:1.0~4.0mol%,余量为MnO;
(2)一次砂磨:使用去离子水作为溶剂进行湿法混合,用砂磨机使步骤(1)的各原材料充分混合均匀,砂磨时间10~30min;
(3)预烧:将步骤(2)所得砂磨料烘干,并在760~1000℃预烧1~3小时;
(4)掺杂:将步骤(3)制作的预烧料中按重量比添加以下副成分掺杂剂,SiO2:0.00~0.01wt%、CaCO3:0.01~0.12wt%、ZrO2:0.01~0.05wt%、Nb2O5:0.01~0.03wt%、Ta2O5:0.005~0.02wt%;
(5)二次砂磨:将步骤(4)所得粉料然后用砂磨机砂磨70~140分钟,控制粒径D50:0.50~1.60μm;
(6)成型:将步骤(5)所得的料浆进行喷雾或机械设备造粒,添加0.01~0.02wt%硬脂酸锌整粒,将颗粒料用压机压制成型为相应的产品坯件;
(7)烧结:将步骤(6)所得产品坯件放入气氛炉内烧结,在升温段,控制氧分压<1.0vol%进行N2气保护排胶致密化烧结,并在1345~1400℃下保温4~8小时,保温时的氧分压为0.2 ~ 5vol%,在降温段进行平衡气氛烧结。
优选的,所述一次砂磨时间15min,在930℃预烧3小时,二次砂磨时间为100分钟,控制粒径D50:1.30μm,添加0.015wt%硬脂酸锌整粒。在升温段,控制氧分压0.2vol%进行N2气保护排胶致密化烧结,并在1390℃下保温6小时,保温时的氧分压为2.6vol%,在降温段进行平衡气氛烧结。
通过以上工序制得所述磁环样品(T18×8×5)。
本发明采用合理的主配方,通过调整Fe2O3和NiO含量来提高材料的Bs;通过调整SiO2、CaCO3、ZrO2、Nb2O5、Ta2O5含量来来细化晶粒,减少气孔,改善材料的显微结构实现材料的低损耗;通过调整预烧温度、粉碎时间以及采用N2气保护排胶致密化烧结工艺来提高烧成密度db和提高材料的起始磁导率μi,获得致密的结晶状态。该材料具有较好的电磁性能,适应电源变压器的要求。
材料的性能指标如下:
起始磁导率μi:2000±25%;
功率损耗密度PV (25kHz,200mT):<350 kW/m3(100)℃;
饱和磁通密度Bs (1kHz,1194A/m):≥490 mT(100)℃;
密度db:>4.9×103kg/m3。
附图说明
图1中(a)为实施例1的微观结构图;(b)为对比例1的微观结构图。
具体实施方式
下面结合所有附图对本发明作进一步说明,参照附图1,以下按照具体实施例说明本发明,但本发明不限定于这些实施例。
本发明的高Bs低损耗软磁铁氧体材料采用氧化物法制造,具体步骤依次如下:
(1) 配方:按表1(实施例和对比例)成分进行配比;
(2) 一次砂磨:使用去离子水作为溶剂进行湿法混合,将以上配方的各原材料充分混合均匀,砂磨时间10~30min;
(3) 预烧:将步骤(2)所得砂磨料烘干,并在760~1000℃预烧1~3小时;
(4) 掺杂:将步骤(3)制作的预烧料中按重量比添加以下副成分掺杂剂,SiO2:0.00~0.01wt%、CaCO3:0.01~0.12wt%、ZrO2:0.01~0.05wt%、Nb2O5:0.01~0.03wt%、Ta2O5:0.005~0.02wt%;
(5) 二次砂磨:将步骤(4)所得粉料然后用砂磨机砂磨70~140分钟,控制粒径D50:0.50~1.60μm;
(6) 成型:将步骤(5)所得的料浆进行喷雾或机械设备造粒,添加0.01~0.02wt%硬脂酸锌整粒,将颗粒料用压机压制成型为相应的产品坯件;
(7) 烧结:将步骤(6)所得产品坯件放入气氛炉内烧结,在升温段,控制氧分压<1.0vol%进行N2气保护排胶致密化烧结,并在1345~1400℃下保温4~8小时,保温时的氧分压为0.2 ~ 5vol%,在降温段进行平衡气氛烧结。
在一种优选方案中,所述一次砂磨时间15min,在930℃预烧3小时,二次砂磨时间为100分钟,控制粒径D50:1.30μm,添加0.015wt%硬脂酸锌整粒。在升温段,控制氧分压0.2vol%进行N2气保护排胶致密化烧结,并在1390℃下保温6小时,保温时的氧分压为2.6vol%,在降温段进行平衡气氛烧结。
通过以上工序制得所述磁环样品(T18×8×5)。
将烧结后的磁环进行测试和评价。在匝数N=20Ts条件下,用HP4284A LCR测试仪测试磁环样品的起始磁导率μi;配合PHH-101高温试验箱,使用SY-8218型B-H分析仪测试样品的功率损耗密度PV和饱和磁通密度Bs;用排水法测试材料的密度db。
表1 实施例和对比例的成分配比
表2 实施例和对比例的磁性能
注意:超过规格上限的附加“※”,超过规格下限的附加“*”。
表1为实施例和对比例的成分配比,表2列出了实施例和对比例的性能及评价。实施例1~5主成分和副成分均在本发明限定范围之内,材料性能指标完全达标。对比例1中主要是由于主成分Fe2O3含量偏少引起超交换作用减弱,导致饱和磁通密度Bs偏低,起始磁导率超高。对比例2中主要是由于主成分Fe2O3含量偏多,导致Fe2+和Fe3+之间的电子跃迁几率增高,电阻率降低,功率损耗密度偏大。又由于过多的Fe2+离子对K1进行过补偿,使其增大导致起始磁导率偏低。对比例3中主要是由于主成分NiO含量偏少,由于Ni的原子量大于Mn的,可见主成分中过少的Ni取代Mn会使材料的密度降低整体性能恶化。对比例4中主要是由于主成分NiO含量偏多,由于NiO具有较大的负值磁晶各向异性常数,能抑制功耗谷点向低温方向移动,降低高温下的损耗。又由于镍铁氧体的居里温度比较高还可以提高材料的高温Bs,但是添加过多的NiO会使二峰往高温方向移动,导致起始磁导率偏低。对比例5中主要是由于主成分ZnO含量偏多,会使居里温度降低导致饱和磁通密度Bs偏低。
从表2中可以看出,本发明的实施例和对比例相比较,本发明有效地提高了材料的起始磁导率μi、饱和磁通密度Bs以及烧成密度db,同时也降低了功率损耗密度PV。如图1所示,实施例1的晶粒尺寸为10~30μm,气孔较少;对比例1的晶粒尺寸为40~60μm,气孔较多。晶粒尺寸细化和气孔的减少是材料性能提高的重要原因之一。本发明的材料应该能够满足电源变压器对软磁材料的要求。
本发明所描述的具体实施例仅仅是对本发明作举例说明,相关技术领域的专家或技术人员可以对所描述的具体实施例做不同程度的修改,补充或者用类似的方式替代,但并不会偏离本发明的精神或者超越所附权利要求书所定义的范围。
Claims (2)
1.一种高Bs低损耗软磁铁氧体材料,其特征在于:
所述软磁铁氧体材料各主料包括: Fe2O3:58.0~62.0mol%,ZnO:12.0~14.0mol%,NiO:1.0~4.0mol%,余量为MnO;
按重量百分比,并以预烧后的主料为参考基准,以氧化物计算,掺杂剂包括SiO2:0.00~0.01wt%,CaCO3:0.01~0.12wt%,ZrO2:0.01~0.05wt%,Nb2O5:0.01~0.03wt%,Ta2O5:0.005~0.02wt%。
2.一种制备如权利要求1所述的高Bs低损耗软磁铁氧体材料的方法,其特征在于,包括以下步骤:
(1)配方:按如下主成分配比 58.0~62.0mol%Fe2O3,12.0~14.0mol%ZnO, 1.0~4.0mol%的NiO,余量为MnO;
(2)一次砂磨:使用去离子水作为溶剂进行湿法混合,用砂磨机使步骤(1)的各原材料充分混合均匀,砂磨时间10~30min;
(3)预烧:将步骤(2)所得砂磨料烘干,并在760~1000℃预烧1~3小时;
(4)掺杂:将步骤(3)制作的预烧料中按重量比添加以下副成分掺杂剂,SiO2:0.00~0.01wt%、CaCO3:0.01~0.12wt%、ZrO2:0.01~0.05wt%、Nb2O5:0.01~0.03wt%、Ta2O5:0.005~0.02wt%;
(5)二次砂磨:将步骤(4)所得粉料然后用砂磨机砂磨70~140分钟,控制粒径D50:0.50~1.60μm;
(6)成型:将步骤(5)所得的料浆进行喷雾或机械设备造粒,添加0.01~0.02wt%硬脂酸锌整粒,将颗粒料用压机压制成型为相应的产品坯件;
(7)烧结:将步骤(6)所得产品坯件放入气氛炉内烧结,在升温段,控制氧分压<1.0vol%进行N2气保护排胶致密化烧结,并在1345~1400℃下保温4~8小时,保温时的氧分压为0.2 ~ 5vol%,在降温段进行平衡气氛烧结。
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