CN111056829A - 一种高频低功耗锰锌铁氧体材料及其制备方法 - Google Patents
一种高频低功耗锰锌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 34
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 title claims abstract description 24
- 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 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000005245 sintering Methods 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000002994 raw material Substances 0.000 claims abstract description 18
- 239000000654 additive Substances 0.000 claims abstract description 8
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims abstract description 7
- 230000000996 additive effect Effects 0.000 claims abstract description 5
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 18
- 239000004576 sand Substances 0.000 claims description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 15
- 229910052760 oxygen Inorganic materials 0.000 claims description 15
- 239000001301 oxygen Substances 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 8
- 239000002002 slurry Substances 0.000 claims description 8
- 239000008187 granular material Substances 0.000 claims description 7
- 238000003801 milling Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 238000005469 granulation Methods 0.000 claims description 4
- 230000003179 granulation Effects 0.000 claims description 4
- 229920002689 polyvinyl acetate Polymers 0.000 claims description 4
- 239000007921 spray Substances 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 2
- 229910000859 α-Fe Inorganic materials 0.000 abstract description 2
- 239000011268 mixed slurry Substances 0.000 description 3
- 238000000498 ball milling Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
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Abstract
本发明涉及铁氧体材料制备技术领域，具体地说，涉及一种高频低功耗锰锌铁氧体材料及其制备方法。包括主要原料和添加剂；所述主要原料以摩尔百分比计算，包括：53.5‑56.5mol％Fe2O3、40.5‑42.5mol％Mn3O4、余量为ZnO；所述添加剂按照主要原料的重量百分比计算，包括：1000‑1500ppm CaO、100‑300ppm SiO2、1000‑3000ppm TiO2、2500‑4000ppmCo3O4、100‑500ppm ZrO2、200‑400ppm Nb2O5、1000‑2000ppm NiO。采用本发明所述配方和工艺制备的高频低功耗锰锌铁氧体材料，在1MHz，50mT测试条件下，100℃功耗仅有150KW/m3，同时，还具有较高的烧结Bs，达到500mT(25℃)和410mT(100℃)；而且，所采用的独特的烧结工艺保证了产品具有较低的高频功耗和较高的烧结密度。
Description
技术领域
本发明涉及铁氧体材料制备技术领域，具体地说，涉及一种高频低功耗锰锌铁氧体材料及其制备方法。
背景技术
开关电源被广泛应用于工业、民用及军事电子设备各个领域，是现代电子设备的重要组成部分。电子产品的小型化发展，要求开关电源体积小、重量轻、可靠性高。而其核心部件变压器的磁芯的体积和重量也就越小越好。根据变压器的工作原理，输出电压与频率成正比，即：
Vm＝KfBmAN
其中，K为波形因子，Bm为工作磁感应强度，f为开关频率，A为磁芯截面积，N为绕组匝数。
因此，要缩小变压器的体积和重量，就要提高开关电源的工作频率，这就要求开关电源用的锰锌铁氧体材料必须具有高频低功耗的特点。
发明内容
本发明的目的在于，提供一种高频低功耗锰锌铁氧体材料及其制备方法，以解决上述的技术问题。
为实现上述目的，本发明所采用的技术方案是：
一种高频低功耗锰锌铁氧体材料，其特征在于：包括主要原料和添加剂；所述主要原料以摩尔百分比计算，包括：53.5-56.5mol％Fe2O3、40.5-42.5mol％Mn3O4、余量为ZnO；所述添加剂按照主要原料的重量百分比计算，包括：1000-1500ppm CaO、100-300ppm SiO2、1000-3000ppm TiO2、2500-4000ppm Co3O4、100-500ppm ZrO2、200-400ppm Nb2O5、1000-2000ppm NiO。
本发明所述高频低功耗锰锌铁氧体材料的制备方法，包括以下步骤：
1、以摩尔百分比计算，以53.5-56.5mol％Fe2O3、40.5-42.5mol％Mn3O4、余量为ZnO的配比准备好主要原料后混合均匀，加入适量水，置入篮式砂磨机中砂磨60min，干燥；
2、将步骤1中干燥后的混合料置入回转窑进行预烧，制得预烧粉料；
3、按照主要原料的重量百分比计算，将1000-1500ppm CaO、100-300ppm SiO2、1000-3000ppm TiO2、2500-4000ppm Co3O4、100-500ppm ZrO2、200-400ppm Nb2O5、1000-2000ppm NiO与步骤2制得的预烧粉料充分混合，制得预烧料；
4、将步骤3制得的预烧料与水按照1∶1的重量比混合后，置入篮式砂磨机中进行二次砂磨，制得砂磨浆料；二次砂磨的粒度控制在D50＝1±0.2μm，砂磨时间2h；
5、步骤4制得的砂磨浆料中加入PVA胶水，混合均匀后，进行喷雾造粒，得到颗粒料；
6、将步骤5制得的颗粒料干压成型，制成毛坯；毛坯密度为2.8±0.2g/cm3；
7、将步骤6干压成型的毛坯在气氛保护钟罩炉中进行烧结，制得高频低功耗锰锌铁氧体材料。
优选的，步骤2中，将混合料置于回转窑中进行预烧，预烧温度980℃，预烧时间3h，预烧气氛为空气；
优选的，步骤5中，所述PVA胶水为0.8％的PVA溶液。
优选的，步骤7中，所述的烧结工艺为：先以1.2-1.4℃/min的升温速度升温到400℃；然后，以0.5-0.6℃/min的升温速度升温到700℃，再以2℃/min的升温速度升温到1150℃，保温时间3.5h后，开始降温，先以2℃/min的降温速度由1150℃降至1100℃，再以0.5℃/min的降温速度由1100℃降至1000℃，最后，由1000℃自然降温至室温。
优选的，步骤7中，所述烧结工艺的烧结气氛处理如下：烧结过程中，升温到400℃过程中，气氛为空气；烧结温度由700℃升至1000℃过程中，氧分压控制在10％-15％；烧结温度由1000℃升至1100℃过程中，氧分压控制在8％-10％；1150℃的保温阶段，氧分压控制在8％；降温过程中，由1150℃降至1100℃时，氧分压控制在1％-2％；由1100℃降至1000℃时，氧分压控制在100-300ppm。
有益效果：与现有技术相比，采用本发明所述配方和工艺制备的高频低功耗锰锌铁氧体材料，在1MHz，50mT测试条件下，100℃功耗仅有150KW/m3，同时，还具有较高的烧结Bs，达到500mT(25℃)和410mT(100℃)；而且，所采用的独特的烧结工艺保证了产品具有较低的高频功耗和较高的烧结密度。
具体实施方式
下面结合具体实施例对本发明做进一步的描述。
本发明所述的高频低功耗锰锌铁氧体材料，包括主要原料和添加剂；所述主要原料以摩尔百分比计算，包括：53.5-56.5mol％Fe2O3、40.5-42.5mol％Mn3O4、余量为ZnO；所述添加剂按照主要原料的重量百分比计算，包括：1000-1500ppm CaO、100-300ppm SiO2、1000-3000ppm TiO2、2500-4000ppm Co3O4、100-500ppm ZrO2、200-400ppm Nb2O5、1000-2000ppm NiO。
本发明所述高频低功耗锰锌铁氧体材料的制备方法，包括以下步骤：
1、以摩尔百分比计算，以53.5-56.5mol％Fe2O3、40.5-42.5mol％Mn3O4、余量为ZnO的配比准备好主要原料后混合均匀，加入适量水，置入篮式砂磨机中砂磨60min，制得混合料浆；将混合料浆置于干燥箱中干燥12h，干燥温度120℃；
2、将步骤1中干燥后的混合料浆置入回转窑进行预烧，制得预烧粉料；预烧温度980℃，预烧时间3h，预烧气氛为空气；
3、按照主要原料的重量百分比计算，将1000-1500ppm CaO、100-300ppm SiO2、1000-3000ppm TiO2、2500-4000ppm Co3O4、100-500ppm ZrO2、200-400ppm Nb2O5、1000-2000ppm NiO与步骤2制得的预烧粉料充分混合，制得预烧料；
4、将步骤3制得的预烧料与水按照1∶1的重量比混合后，置入篮式砂磨机中进行二次砂磨，砂磨时间60min，制得砂磨浆料；期间进行两次置换，将底部料浆倒出，再从篮式砂磨机顶部开口加入球磨罐中；二次砂磨的粒度控制在D50＝1±0.2μm，砂磨时间2h；
5、步骤4制得的砂磨浆料中加入0.8％的PVA溶液，经过搅拌，混合均匀并沉淀后，进行喷雾造粒，得到颗粒料；造粒塔进口温度350℃，出口温度120℃左右，喷雾造粒的颗粒料松比1.40-1.45，水分0.2-0.3％，安息角26.7-27.1°；
6、将步骤5制得的颗粒料干压成型，制成毛坯；毛坯密度为2.8±0.2g/cm3；
7、将步骤6干压成型的毛坯在气氛保护钟罩炉中进行烧结，制得高频低功耗锰锌铁氧体材料；
所述的烧结工艺为：先以1.2-1.4℃/min的升温速度升温到400℃；然后，以0.5-0.6℃/min的升温速度升温到700℃，再以2℃/min的升温速度升温到1150℃，保温时间3.5h后，开始降温，先以2℃/min的降温速度由1150℃降至1100℃，再以0.5℃/min的降温速度由1100℃降至1000℃，最后，由1000℃自然降温至室温；
所述烧结工艺的烧结气氛处理如下：烧结过程中，升温到400℃过程中，气氛为空气；烧结温度由700℃升至1000℃过程中，氧分压控制在10％-15％；烧结温度由1000℃升至1100℃过程中，氧分压控制在8％-10％；1150℃的保温阶段，氧分压控制在8％；降温过程中，由1150℃降至1100℃时，氧分压控制在1％-2％；由1100℃降至1000℃时，氧分压控制在100-300ppm。
采用本发明所述制备方法制备的锰锌铁氧体材料比常规PC40材料具有更高的Bs，并且功耗水平与之接近。经测试，在H＝1194A/m，10KHz测试条件下，本发明所述锰锌铁氧体材料的Bs达到500mT(25℃)和410mT(100℃)；1MHz，50mT，100℃测试功耗达到150KW/m3(100℃)。
以上对本发明的较佳实施方式进行了具体说明，但本发明并不限于所述实施例，熟悉本领域的技术人员在不违背本发明精神的前提下还可作出种种的等同变型或替换，这些等同的变型或替换均包含在本申请权利要求所限定的范围内。
Claims (6)
1.一种高频低功耗锰锌铁氧体材料，其特征在于：包括主要原料和添加剂；所述主要原料以摩尔百分比计算，包括：53.5-56.5mol％Fe2O3、40.5-42.5mol％Mn3O4、余量为ZnO；所述添加剂按照主要原料的重量百分比计算，包括：1000-1500ppm CaO、100-300ppm SiO2、1000-3000ppm TiO2、2500-4000ppm Co3O4、100-500ppm ZrO2、200-400ppm Nb2O5、1000-2000ppm NiO。
2.如权利要求1所述高频低功耗锰锌铁氧体材料的制备方法，其特征在于：包括以下步骤：
(1)以摩尔百分比计算，以53.5-56.5mol％Fe2O3、40.5-42.5mol％Mn3O4、余量为ZnO的配比准备好主要原料后混合均匀，加入适量水，置入篮式砂磨机中砂磨60min，干燥；
(2)将步骤(1)中干燥后的混合料置入回转窑进行预烧，制得预烧粉料；
(3)按照主要原料的重量百分比计算，将1000-1500ppm CaO、100-300ppm SiO2、1000-3000ppm TiO2、2500-4000ppm Co3O4、100-500ppm ZrO2、200-400ppm Nb2O5、1000-2000ppmNiO与步骤(2)制得的预烧粉料充分混合，制得预烧料；
(4)将步骤(3)制得的预烧料与水按照1∶1的重量比混合后，置入篮式砂磨机中进行二次砂磨，制得砂磨浆料；二次砂磨的粒度控制在D50＝1±0.2μm，砂磨时间2h；
(5)步骤(4)制得的砂磨浆料中加入PVA胶水，混合均匀后，进行喷雾造粒，得到颗粒料；
(6)将步骤(5)制得的颗粒料干压成型，制成毛坯；毛坯密度为2.8±0.2g/cm3；
(7)将步骤(6)干压成型的毛坯在气氛保护钟罩炉中进行烧结，制得高频低功耗锰锌铁氧体材料。
3.根据权利要求2所述高频低功耗锰锌铁氧体材料的制备方法，其特征在于：步骤(2)中，将混合料置于回转窑中进行预烧，预烧温度980℃，预烧时间3h，预烧气氛为空气。
4.根据权利要求2所述高频低功耗锰锌铁氧体材料的制备方法，其特征在于：步骤(5)中，所述PVA胶水为0.8％的PVA溶液。
5.根据权利要求2所述高频低功耗锰锌铁氧体材料的制备方法，其特征在于：步骤(7)中，所述的烧结工艺为：先以1.2-1.4℃/min的升温速度升温到400℃；然后，以0.5-0.6℃/min的升温速度升温到700℃，再以2℃/min的升温速度升温到1150℃，保温时间3.5h后，开始降温，先以2℃/min的降温速度由1150℃降至1100℃，再以0.5℃/min的降温速度由1100℃降至1000℃，最后，由1000℃自然降温至室温。
6.根据权利要求5所述高频低功耗锰锌铁氧体材料的制备方法，其特征在于：步骤(7)中，所述烧结工艺的烧结气氛处理如下：烧结过程中，升温到400℃过程中，气氛为空气；烧结温度由700℃升至1000℃过程中，氧分压控制在10％-15％；烧结温度由1000℃升至1100℃过程中，氧分压控制在8％-10％；1150℃的保温阶段，氧分压控制在8％；降温过程中，由1150℃降至1100℃时，氧分压控制在1％-2％；由1100℃降至1000℃时，氧分压控制在100-300ppm。
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