CN108101527B - 一种高频细晶粒软磁铁氧体材料及其制备方法 - Google Patents
一种高频细晶粒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 62
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 30
- 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 32
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 28
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 23
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims abstract description 17
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 13
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 11
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 11
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 11
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 11
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 11
- 229910052925 anhydrite Inorganic materials 0.000 claims abstract description 9
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims description 21
- 238000005469 granulation Methods 0.000 claims description 20
- 230000003179 granulation Effects 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 20
- 238000005245 sintering Methods 0.000 claims description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000000465 moulding Methods 0.000 claims description 10
- 239000004576 sand Substances 0.000 claims description 10
- 239000007921 spray Substances 0.000 claims description 10
- 238000001694 spray drying Methods 0.000 claims description 10
- 239000008187 granular material Substances 0.000 claims description 6
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- 238000004537 pulping Methods 0.000 claims description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 230000001050 lubricating effect Effects 0.000 abstract description 3
- WJZHMLNIAZSFDO-UHFFFAOYSA-N manganese zinc Chemical compound [Mn].[Zn] WJZHMLNIAZSFDO-UHFFFAOYSA-N 0.000 abstract description 3
- 238000005461 lubrication Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000006641 stabilisation Effects 0.000 abstract description 2
- 238000011105 stabilization Methods 0.000 abstract description 2
- 239000000696 magnetic material Substances 0.000 description 9
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 8
- 239000000306 component Substances 0.000 description 8
- 230000004907 flux Effects 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 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 description 2
- 230000035699 permeability Effects 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- TWFZGCMQGLPBSX-UHFFFAOYSA-N carbendazim Chemical compound C1=CC=C2NC(NC(=O)OC)=NC2=C1 TWFZGCMQGLPBSX-UHFFFAOYSA-N 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- QELJHCBNGDEXLD-UHFFFAOYSA-N nickel zinc Chemical compound [Ni].[Zn] QELJHCBNGDEXLD-UHFFFAOYSA-N 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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Abstract
本发明公开一种高频细晶粒软磁铁氧体材料，其特征在于，包括如下组分：主料：Fe2O3：51~55mol%、MnO：32~36 mol%、ZnO：8~12 mol%，MgO：4~8 mol%、CaSO4：4~8 mol%。辅料：Bi2O3：100~400ppm、TiO2：50~150ppm、SiO2：10~50ppm、CaO：10~50ppm、SnO2：10~30ppm、BaCO3：10~30ppm、Nb2O5：10~30ppm、ZrO2：10~30ppm、Ta2O5：10~30ppm。本发明配方和方法合理，能够细化锰锌软磁铁氧体材料粉体，减小功率损耗和磁滞损耗。本发明在主料中加入MgO和CaSO4，能够起到润滑和稳定的作用，有利于降低粉磨时间，提高生产效率。本发明在辅料中加入Nb2O5、ZrO2、Ta2O5能够提高产品粉体的细度。
Description
技术领域
本发明属于软磁铁氧体材料领域，具体涉及一种高频细晶粒软磁铁氧体材料及其制备方法。
背景技术
软磁材料是指矫顽力小，容易磁化的磁性材料，其核心组分为三氧化二铁（Fe2O3），然而单一的Fe2O3不具备性能稳定、磁导率高、电阻率高的特点，因此研究人员加入锰、锌、镍的氧化物来提高其性能，因此软磁材料分为锰锌软磁铁氧体和镍锌软磁铁氧体。进一步地，为了适应电讯行业的快速发展，软磁材料提高多种辅料来提高其性能，使粉体细化，从而减少损失和提高工作频率。由此可见细化粉体对软磁材料的磁通量和频率的提高具有重要影响。
发明内容
为了解决现有技术领域存在的问题，提高锰锌铁氧体的功率，减少锰锌铁氧体材料的损耗，细化软磁材料粉体，本发明提出一种高频细晶粒软磁铁氧体材料，主要包括如下组分：
主料
Fe2O3：51~55mol%、MnO：32~36 mol%、ZnO：8~12 mol%，MgO：4~8 mol%、CaSO4：4~8mol%；
辅料
Bi2O3：100~400ppm、TiO2：50~150ppm、SiO2：10~50ppm、CaO：10~50ppm、SnO2：10~30ppm、BaCO3：10~30ppm、Nb2O5：10~30ppm、ZrO2：10~30ppm、Ta2O5：10~30ppm。
本发明还提供上述一种高频细晶粒软磁铁氧体材料的制备方法，包括如下步骤：
（1）配料，将主料中的各组分按照上述配比配料；
（2）混料与制浆，将配好的原料放入逆流混料机中混合，混料时间1~2h；
（3）预烧，在回转窑中进行预烧，预烧温度700~1000℃，预烧时间：3~5h；
（4）粗粉碎，将预烧后的混合料与按照权利要求1配比配好的辅料中的Bi2O3、TiO2、SiO2、CaO、SnO2、BaCO3一起进行粗粉碎，粗粉粹时间20~40min；
（5）细粉碎，将步骤（4）制得的混合料与按照权利要求1配比配好的辅料中的Nb2O5、ZrO2、Ta2O5一起进行细粉碎，采用循环式砂磨机进行砂磨，砂磨时间3~6h；
（6）一次喷雾造粒，采用喷雾干燥造粒，通入热空气的温度为250~280℃；
（7）细粉碎，将步骤（6）制得的颗粒采用循环式砂磨机进行砂磨，砂磨时间3~6h；
（8）二次喷雾造粒：采用喷雾干燥造粒，通入热空气的温度为300~350℃；
（9）成型，将步骤（7）获得的粒料压制成型；
（10）烧结，采用氮气单推板烧结炉进行气氛烧结，烧结温度为1300~1500℃。
进一步地，所述步骤（10）中在1100℃时保温1h。
优选地，所述Fe2O3为52 mol%。
优选地，所述MnO为34 mol%。
优选地，所述ZnO为10 mol%。
优选地，所述MgO为5 mol%。
优选地，所述CaSO4为4 mol%
本发明的主要原理是： 在主料中加入MgO和CaSO4，在组粉碎时能够起到良好的润滑作用，此外CaSO4具有的SO2离子对主料的预烧起到稳定的作用。辅料中的Nb2O5、ZrO2、Ta2O5，有利于细化粉体，因此在细粉碎时加入。SnO2能够提高主料的导电性。
本发明的有益效果是：
1、本发明配方和方法合理，能够细化锰锌软磁铁氧体材料粉体，减小功率损耗和磁滞损耗；
2、本发明在主料中加入MgO和CaSO4，能够起到润滑和稳定的作用，有利于降低粉磨时间，提高生产效率。
3、本发明在辅料中加入Nb2O5、ZrO2、Ta2O5能够提高产品粉体的细度。
具体实施方式
为了便于本领域技术人员理解，下面结合具体实施例对本发明作详细说明。
实施例1
一种高频细晶粒软磁铁氧体材料，主要包括如下组分：
主料
Fe2O3：51mol%、MnO：32 mol%、ZnO：8 mol%，MgO：6 mol%、CaSO4：6mol%；
辅料
Bi2O3：300ppm、TiO2：80ppm、SiO2：30ppm、CaO：30ppm、SnO2：10ppm、BaCO3：10ppm、Nb2O5：30ppm、ZrO2：30ppm、Ta2O5：30ppm。
本发明还提供上述一种高频细晶粒软磁铁氧体材料的制备方法，包括如下步骤：
（1）配料，将主料中的各组分按照上述配比配料；
（2）混料与制浆，将配好的原料放入逆流混料机中混合，混料时间1.5h；
（3）预烧，在回转窑中进行预烧，预烧温度700~1000℃，预烧时间：4h；
（4）粗粉碎，将预烧后的混合料与按照权利要求1配比配好的辅料中的Bi2O3、TiO2、SiO2、CaO、SnO2、BaCO3一起进行粗粉碎，粗粉粹时间40min；
（5）细粉碎，将步骤（4）制得的混合料与按照权利要求1配比配好的辅料中的Nb2O5、ZrO2、Ta2O5一起进行细粉碎，采用循环式砂磨机进行砂磨，砂磨时间5h；
（6）一次喷雾造粒，采用喷雾干燥造粒，通入热空气的温度为280℃；
（7）细粉碎，将步骤（6）制得的颗粒采用循环式砂磨机进行砂磨，砂磨时间5h；
（8）二次喷雾造粒：采用喷雾干燥造粒，通入热空气的温度为300~350℃；
（9）成型，将步骤（7）获得的粒料压制成型；
（10）烧结，采用氮气单推板烧结炉进行气氛烧结，烧结温度为1500℃。并在1100℃时保温1h。
实施例2
一种高频细晶粒软磁铁氧体材料，主要包括如下组分：
主料
Fe2O3：55mol%、MnO：36 mol%、ZnO：12 mol%，MgO：4 mol%、CaSO4：4 mol%；
辅料
Bi2O3：400ppm、TiO2：50ppm、SiO2：10ppm、CaO：10ppm、SnO2：30ppm、BaCO3：30ppm、Nb2O5：20ppm、ZrO2：20ppm、Ta2O5：20ppm。
本发明还提供上述一种高频细晶粒软磁铁氧体材料的制备方法，包括如下步骤：
（1）配料，将主料中的各组分按照上述配比配料；
（2）混料与制浆，将配好的原料放入逆流混料机中混合，混料时间2h；
（3）预烧，在回转窑中进行预烧，预烧温度700~1000℃，预烧时间：3h；
（4）粗粉碎，将预烧后的混合料与按照权利要求1配比配好的辅料中的Bi2O3、TiO2、SiO2、CaO、SnO2、BaCO3一起进行粗粉碎，粗粉粹时间20min；
（5）细粉碎，将步骤（4）制得的混合料与按照权利要求1配比配好的辅料中的Nb2O5、ZrO2、Ta2O5一起进行细粉碎，采用循环式砂磨机进行砂磨，砂磨时间6h；
（6）一次喷雾造粒，采用喷雾干燥造粒，通入热空气的温度为270℃；
（7）细粉碎，将步骤（6）制得的颗粒采用循环式砂磨机进行砂磨，砂磨时间4h；
（8）二次喷雾造粒：采用喷雾干燥造粒，通入热空气的温度为350℃；
（9）成型，将步骤（7）获得的粒料压制成型；
（10）烧结，采用氮气单推板烧结炉进行气氛烧结，烧结温度为1300℃。并在1100℃时保温1h。
实施例3
一种高频细晶粒软磁铁氧体材料，主要包括如下组分：
主料
Fe2O3：52mol%、MnO：34 mol%、ZnO：10mol%，MgO：5 mol%、CaSO4：4 mol%；
辅料
Bi2O3：200ppm、TiO2：100ppm、SiO2：40ppm、CaO：40ppm、SnO2：20ppm、BaCO3：20ppm、Nb2O5：10ppm、ZrO2：10ppm、Ta2O5：10ppm。
本发明还提供上述一种高频细晶粒软磁铁氧体材料的制备方法，包括如下步骤：
（1）配料，将主料中的各组分按照上述配比配料；
（2）混料与制浆，将配好的原料放入逆流混料机中混合，混料时间1h；
（3）预烧，在回转窑中进行预烧，预烧温度700~1000℃，预烧时间：4h；
（4）粗粉碎，将预烧后的混合料与按照权利要求1配比配好的辅料中的Bi2O3、TiO2、SiO2、CaO、SnO2、BaCO3一起进行粗粉碎，粗粉粹时间30min；
（5）细粉碎，将步骤（4）制得的混合料与按照权利要求1配比配好的辅料中的Nb2O5、ZrO2、Ta2O5一起进行细粉碎，采用循环式砂磨机进行砂磨，砂磨时间3h；
（6）一次喷雾造粒，采用喷雾干燥造粒，通入热空气的温度为250℃；
（7）细粉碎，将步骤（6）制得的颗粒采用循环式砂磨机进行砂磨，砂磨时间6h；
（8）二次喷雾造粒：采用喷雾干燥造粒，通入热空气的温度为300℃；
（9）成型，将步骤（7）获得的粒料压制成型；
（10）烧结，采用氮气单推板烧结炉进行气氛烧结，烧结温度为1400℃，并在1100℃时保温1h。
对上述实施例中制得的软磁铁氧体材料的性能进行测试，采用SY8232-BHAnalyzer测试仪测量饱和磁通密度（Bs）：用HP42484A LCR表测试起始磁导率（μi），用Protek digital Multimeter 测试仪测试功率损耗（Pc）。测试结果如下表所示：
由上表可以看出按照本发明所述的配方和方法制得的软磁铁氧体材料，从初始磁导率、功率损耗、饱和磁通密度三个软磁材料的核心性能指标来衡量均表现良好，其中实施例3的各项性能指标最佳。
Claims (8)
1.一种高频细晶粒软磁铁氧体材料，其特征在于，包括如下组分：
主料：Fe2O3：51~55mol%、MnO：32~36 mol%、ZnO：8~12 mol%，MgO：4~8 mol%、CaSO4：4~8mol%；
辅料：Bi2O3：100~400ppm、TiO2：50~150ppm、SiO2：10~50ppm、CaO：10~50ppm、SnO2：10~30ppm、BaCO3：10~30ppm、Nb2O5：10~30ppm、ZrO2：10~30ppm、Ta2O5：10~30ppm。
2.如权利要求1所述的一种高频细晶粒软磁铁氧体材料的制备方法，其特征在于， 包括如下步骤：
（1）配料，将主料中的各组分按照上述配比配料；
（2）混料与制浆，将配好的原料放入逆流混料机中混合，混料时间1~2h；
（3）预烧，在回转窑中进行预烧，预烧温度700~1000℃，预烧时间：3~5h；
（4）粗粉碎，将预烧后的混合料与按照权利要求1配比配好的辅料中的Bi2O3、TiO2、SiO2、CaO、SnO2、BaCO3一起进行粗粉碎，粗粉粹时间20~40min；
（5）细粉碎，将步骤（4）制得的混合料与按照权利要求1配比配好的辅料中的Nb2O5、ZrO2、Ta2O5一起进行细粉碎，采用循环式砂磨机进行砂磨，砂磨时间3~6h；
（6）一次喷雾造粒，采用喷雾干燥造粒，通入热空气的温度为250~280℃；
（7）细粉碎，将步骤（6）制得的颗粒采用循环式砂磨机进行砂磨，砂磨时间3~6h；
（8）二次喷雾造粒：采用喷雾干燥造粒，通入热空气的温度为300~350℃；
（9）成型，将步骤（8）获得的粒料压制成型；
（10）烧结，采用氮气单推板烧结炉进行气氛烧结，烧结温度为1300~1500℃。
3.如权利要求2中所述的一种高频细晶粒软磁铁氧体材料的制备方法，其特征在于，所述步骤（10）中在1100℃时保温1h。
4.如权利要求1所述的一种高频细晶粒软磁铁氧体材料，其特征在于，所述Fe2O3为52mol%。
5.如权利要求1所述的一种高频细晶粒软磁铁氧体材料，其特征在于，所述MnO为34mol%。
6.如权利要求1所述的一种高频细晶粒软磁铁氧体材料，其特征在于，所述ZnO为10mol%。
7.如权利要求1所述的一种高频细晶粒软磁铁氧体材料，其特征在于，所述MgO为5mol%。
8.如权利要求1所述的一种高频细晶粒软磁铁氧体材料，其特征在于，所述CaSO4为4mol%。
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Inventor after: Xu Jie Inventor after: Ge Changzhi Inventor after: Ma Yingying Inventor after: Zhang Jun Inventor after: Zhou Fulin Inventor after: Zhang Wenjun Inventor after: Zeng Xingru Inventor after: Wang Yuzhi Inventor after: Zhang Zongren Inventor after: Xu Erming Inventor after: Dong Wenlong Inventor after: Tao Tianliang Inventor before: Xu Jie Inventor before: Zhou Fulin Inventor before: Zhang Wenjun Inventor before: Zeng Xingru Inventor before: Wang Yuzhi Inventor before: Zhang Zongren Inventor before: Xu Erming Inventor before: Dong Wenlong Inventor before: Tao Tianliang |
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Effective date of registration: 20210923 Address after: Room 1402-2, 14 / F, Changxing world trade building, 1278 Mingzhu Road, Changxing County Economic Development Zone, Huzhou City, Zhejiang Province 313000 Applicant after: Zhejiang Boan Inspection Technology Co.,Ltd. Address before: 239300 east of Jingliu road and south of Weiyi Road, Tianchang Development Zone, Chuzhou City, Anhui Province Applicant before: TIANCHANG CITY ZHAOTIAN MAGNETOELECTRICITY TECHNOLOGY Co.,Ltd. |
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