CN112592169A - 一种led用宽温高频低损耗、高磁导率锰锌铁氧体及其制备方法 - Google Patents
一种led用宽温高频低损耗、高磁导率锰锌铁氧体及其制备方法 Download PDFInfo
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- 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 description 8
- 239000000463 material Substances 0.000 claims abstract description 37
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 28
- 239000000654 additive Substances 0.000 claims abstract description 24
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 15
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 15
- 239000007921 spray Substances 0.000 claims description 41
- 238000005245 sintering Methods 0.000 claims description 25
- 230000000996 additive effect Effects 0.000 claims description 18
- 238000000227 grinding Methods 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 15
- 239000001301 oxygen Substances 0.000 claims description 15
- 229910052760 oxygen Inorganic materials 0.000 claims description 15
- 238000001694 spray drying Methods 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 239000008187 granular material Substances 0.000 claims description 14
- 239000002002 slurry Substances 0.000 claims description 14
- 238000001238 wet grinding Methods 0.000 claims description 10
- UPWOEMHINGJHOB-UHFFFAOYSA-N cobalt(III) oxide Inorganic materials O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000000280 densification Methods 0.000 claims description 7
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- 239000011701 zinc Substances 0.000 claims description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 4
- 229910052681 coesite Inorganic materials 0.000 claims description 4
- 229910052906 cristobalite Inorganic materials 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 229910052682 stishovite Inorganic materials 0.000 claims description 4
- 229910052905 tridymite Inorganic materials 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000007580 dry-mixing Methods 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 230000035699 permeability Effects 0.000 claims 7
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000004907 flux Effects 0.000 abstract description 3
- 238000012797 qualification Methods 0.000 abstract description 2
- 239000011230 binding agent Substances 0.000 abstract 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 28
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 28
- 239000011787 zinc oxide Substances 0.000 description 13
- 230000009286 beneficial effect Effects 0.000 description 8
- 239000013078 crystal Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000011161 development Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 150000005837 radical ions Chemical class 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种LED用宽温高频低损耗、高磁导率锰锌铁氧体，包括：Fe2O3、MnO、ZnO、聚乙烯醇、辅料、粘结剂和添加剂；本发明铁氧体在性能方面与其他同行先进指标相比，本发明铁氧体在25‑140℃宽温、高频低功耗基础上，‑40℃～25℃功耗进一步降低，同时饱和磁通密度Bs进一步提高，25℃Bs比常规的PC95类材料提高10mT，100℃Bs比常规类PC95材料提高20mT，居里温度达到230℃以上，因而具有良好的直流叠加特性。本发明铁氧体具有更低的使用损耗，且生产合格率高。
Description
技术领域
本发明涉及磁性材料生产制造领域，具体的说涉及一种LED用宽温高频低损耗、高磁导率锰锌铁氧体及其制备方法。
背景技术
目前我国能源日益紧缺，节约能源是全球共同的目标。通过国家有关部门预测，2020年我国用电量将达7.8万亿度，照明用电量将超过9000亿度。如果在这个领域上节省50％，那将是4500亿度。所以如何降低照明用电能耗成为了当前迫在眉睫的问题。LED无疑在这个领域有着非常大的应用地位和前景以及无穷的商机。
LED取代型灯具及其他新型LED照明的发展十分迅速，从大批量DC/DC 电源的低电流、高亮度LED(用于手机、标识及笔记本电脑)，到AC/DC电源的更高电流LED(一般是照明应用)的离线型LED照明电源的发展将是主流，因此对大功率低损耗铁氧体的要求也越来越高。愈来愈多的业内人士认识到，要充分发挥LED的潜能，照明驱动电源是关键的支撑因素之一。对于LED照明驱动电源，当前的主要诉求集中在高可靠性、高效节能等方面。要具有高的可靠性，需要与LED光源相匹配的长寿命，宽的工作温度适应性(-40℃-65℃，甚至-55℃-85℃)，宽的电网适应及自保护性能等。这要求电源要有良好的 EMC，较高的功率因数(PFC)，基于以上LED电源对电源高效率及高可靠性的要求。
因此提供一种LED用宽温高频低损耗、高磁导率锰锌铁氧体及其制备方法是本领域技术人员亟需解决的技术问题。
发明内容
有鉴于此，本发明提供了一种宽温高频低损耗、高磁导率锰锌铁氧体，其性能在25-140℃宽温、高频低功耗基础上，-40℃～25℃功耗进一步降低，同时饱和磁通密度Bs进一步提高，25℃Bs比常规的PC95类材料提高10mT， 100℃Bs比常规类PC95材料提高20mT，居里温度达到230℃以上。
为了实现上述目的，本发明采用如下技术方案：
一种LED用宽温高频低损耗、高磁导率锰锌铁氧体，包括以下物质的量分数原料：Fe2O365.6-75.3％、MnO 18.5-25.5％、ZnO 4.9-9.5％、7-9‰聚乙烯醇、余量为添加剂。
进一步，所述辅助添加剂为CaO、SiO2、V2O5、ZrO2、Nb2O5、TiO2、SnO2 和Co2O3中的一种或多种混合。
采用上述进一步的有益效果在于：掺杂改性是对粉体性能快速提升的重要手段，本发明添加物对Mn-Zn铁氧体微观结构的影响非常明显。宽温低功耗材料的宽温特性改善主要依靠掺杂工艺优化。CaO、SiO2课在晶界形成高电阻率的绝缘层，提高电阻率，降低涡流损耗；V2O5为低熔点杂质可以降低烧结温度150℃-200℃，且能提高烧结密度和电阻率，细化晶粒，从而获得高密度细晶粒结构，进而提升Bs和叠加特性。ZrO2和Nb2O5能细化晶粒，使得晶粒大小均匀，内应力小，进一步降低涡流损耗。TiO2、SnO2、Co2O3类的添加剂能改善宽温特性，降低宽温功耗，同时降低-40-25℃的功耗。
本发明还提供了上述LED用宽温高频低损耗、高磁导率锰锌铁氧体的制备方法，包括以下步骤：
(1)按上述物质的量分数称取各原料，并将：Fe2O3、MnO和ZnO用干法混合均匀后，将混料溶于水中，得到浆料；
(2)将浆料送入至喷雾塔中进行喷雾干燥；
(3)将喷雾干燥后的材料放入电阻炉中并在保护气体条件下进行预烧；
(4)将预烧后的材料进行湿法粉碎，并混合加入添加剂，然后将粉碎后的材料溶于水中；
(5)将聚乙烯醇加入至步骤(4)所得溶液中，然后在喷雾塔中进行喷雾干燥得到颗粒料；
(6)将颗粒料送至烧结窑中进行进行烧结，得到软磁铁氧体；
(7)将软磁铁氧体磁心通过四轴780磨床磨面-磨底-磨面进行磨加工，即得高频低损耗、高磁导率锰锌铁氧体。
进一步，上述步骤(1)中干法混合时间为60-70min；
所述水为去离子水。
采用上述进一步的有益效果在于：能够防止杂质粒子进入。
进一步，上述步骤(2)中喷雾塔进风温度为210-230℃，喷雾塔出风温度为90-110℃。
采用上述进一步的有益效果在于：本发明上述操作可以保证造粒均匀性。
进一步，上述步骤(3)中保护气体为氮气，且整个预烧结气氛中含有1-2％质量分数的氧气；
所述预烧温度为810-850℃，所述预烧时间为120-180min。
采用上述进一步的有益效果在于：进行预烧结能够有效去除杂质酸根离子。
进一步，上述步骤(4)中湿法粉碎时间为60-80min；粉碎粒度为1.0-1.3 μm。
采用上述进一步的有益效果在于：湿法粉碎能有效保证喷雾造粒和粉料性能的稳定性。
进一步，上述步骤(5)中喷雾塔进风温度为210-230℃，喷雾塔出风温度为90-110℃。
步骤(6)中所述烧结温度为1360℃，进风量80m3/h，窑压为1.6KPa，保温氧含量为6％，在1000℃-1250℃下致密化致O2含量在1％以下。
采用上述进一步的有益效果在于：本发明的烧结方法能保证产品晶粒均匀及性能优良生成。
进一步，上述步骤(7)中磨加工操作方法为通过四轴780磨床磨面-磨底-磨面进行磨加工。
采用上述进一步的有益效果在于：本发明采用的磨加工操作方法能完成产品加工正常操作。
本发明的有益效果在于：本发明铁氧体在性能方面与其他同行先进指标相比，本发明铁氧体在25-140℃宽温、高频低功耗基础上，-40℃～25℃功耗进一步降低，同时饱和磁通密度Bs进一步提高，25℃Bs比常规的PC95类材料提高10mT，100℃Bs比常规类PC95材料提高20mT，居里温度达到230℃以上，因而具有良好的直流叠加特性。本发明铁氧体具有更低的使用损耗，且生产合格率高。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
本发明实施例中所有氧气含量百分比均为烧结气氛质量分数。
实施例1
一种LED用宽温高频低损耗、高磁导率锰锌铁氧体
(1)按百分比称取Fe2O375.3％、MnO 18.5％、ZnO 4.9％、聚乙烯醇7‰以及余量添加剂，辅助添加剂为V2O5和ZrO2；
并将：Fe2O3、MnO和ZnO用干法混合60min后，将混料溶于去离子水中，得到浆料；
(2)将浆料送入至喷雾塔中进行喷雾干燥，喷雾塔进风温度为230℃，喷雾塔出风温度为110℃；
(3)将喷雾干燥后的材料放入电阻炉中并在氮气下810℃条件下预烧 120min，整个预烧结气氛中含有2％质量分数的氧气；
(4)将预烧后的材料进行湿法粉碎60min至粒度为1.3μm，并混合加入添加剂，然后将粉碎后的材料溶于水中；
(5)将聚乙烯醇加入至步骤(4)所得溶液中，然后在喷雾塔中进行喷雾干燥得到颗粒料，喷雾塔进风温度为230℃，喷雾塔出风温度为110℃；
(6)将颗粒料送至1200℃的烧结窑中然后升温至1360℃烧结，控制进风量为80m3/h，窑压为1.6KPa，保温氧含量为6％，在1250℃下致密化致O2含量在1％以下，得到软磁铁氧体；
(7)将软磁铁氧体通过四轴780磨床磨面-磨底-磨面进行磨加工，即得高频低损耗、高磁导率锰锌铁氧体。
实施例2
一种LED用宽温高频低损耗、高磁导率锰锌铁氧体
(1)按百分比称取Fe2O365.6％、MnO 25.5％、ZnO 9.5％、聚乙烯醇7‰以及余量添加剂，辅助添加剂为CaO和SiO2；
并将：Fe2O3、MnO和ZnO用干法混合70min后，将混料溶于去离子水中，得到浆料；
(2)将浆料送入至喷雾塔中进行喷雾干燥，喷雾塔进风温度为210℃，喷雾塔出风温度为90℃；
(3)将喷雾干燥后的材料放入电阻炉中并在氮气下850℃条件下预烧 120min，整个预烧结气氛中含有1％质量分数的氧气；
(4)将预烧后的材料进行湿法粉碎80min至粒度为1.0μm，并混合加入添加剂，然后将粉碎后的材料溶于水中；
(5)将聚乙烯醇加入至步骤(4)所得溶液中，然后在喷雾塔中进行喷雾干燥得到颗粒料，喷雾塔进风温度为210℃，喷雾塔出风温度为90℃；
(6)将颗粒料送至500℃的烧结窑中然后升温至1360℃烧结，控制进风量为80m3/h，窑压为1.6KPa，保温氧含量为6％，在1000℃℃下致密化致O2含量在1％以下，得到软磁铁氧体；
(7)将软磁铁氧体通过四轴780磨床磨面-磨底-磨面进行磨加工，即得高频低损耗、高磁导率锰锌铁氧体。
实施例3
一种LED用宽温高频低损耗、高磁导率锰锌铁氧体
(1)按百分比称取Fe2O368.8％、MnO 21.2％、ZnO 8.4％、聚乙烯醇7-9‰以及余量添加剂，辅助添加剂为Nb2O5、TiO2和Co2O3；
并将：Fe2O3、MnO和ZnO用干法混合65min后，将混料溶于去离子水中，得到浆料；
(2)将浆料送入至喷雾塔中进行喷雾干燥，喷雾塔进风温度为220℃，喷雾塔出风温度为110℃；
(3)将喷雾干燥后的材料放入电阻炉中并在氮气下830℃条件下预烧 150min，整个预烧结气氛中含有1.5％质量分数的氧气；
(4)将预烧后的材料进行湿法粉碎70min至粒度为1.2μm，并混合加入添加剂，然后将粉碎后的材料溶于水中；
(5)将聚乙烯醇加入至步骤(4)所得溶液中，然后在喷雾塔中进行喷雾干燥得到颗粒料，喷雾塔进风温度为220℃，喷雾塔出风温度为100℃；
(6)将颗粒料送至1000℃的烧结窑中然后升温至1360℃烧结，控制进风量为80m3/h，窑压为1.6KPa，保温氧含量为6％，在1150℃下致密化致O2含量在1％以下，得到软磁铁氧体；
(7)将软磁铁氧体通过四轴780磨床磨面-磨底-磨面进行磨加工，即得高频低损耗、高磁导率锰锌铁氧体。
实施例4
一种LED用宽温高频低损耗、高磁导率锰锌铁氧体
(1)按百分比称取Fe2O369.2％、MnO 23.3％、ZnO 6.8％、聚乙烯醇8‰以及余量添加剂，辅助添加剂为Co2O3；
并将：Fe2O3、MnO和ZnO用干法混合70min后，将混料溶于去离子水中，得到浆料；
(2)将浆料送入至喷雾塔中进行喷雾干燥，喷雾塔进风温度为220℃，喷雾塔出风温度为100℃；
(3)将喷雾干燥后的材料放入电阻炉中并在氮气下840℃条件下预烧 170min，整个预烧结气氛中含有1.4％质量分数的氧气；
(4)将预烧后的材料进行湿法粉碎75min至粒度为1.1μm，并混合加入添加剂，然后将粉碎后的材料溶于水中；
(5)将聚乙烯醇加入至步骤(4)所得溶液中，然后在喷雾塔中进行喷雾干燥得到颗粒料，喷雾塔进风温度为215℃，喷雾塔出风温度为100℃；
(6)将颗粒料送至800℃的烧结窑中然后升温至1360℃烧结，控制进风量为80m3/h，窑压为1.6KPa，保温氧含量为6％，在1100℃下致密化致O2含量在1％以下，得到软磁铁氧体；
(7)将软磁铁氧体通过四轴780磨床磨面-磨底-磨面进行磨加工，即得高频低损耗、高磁导率锰锌铁氧体。
实施例5
一种LED用宽温高频低损耗、高磁导率锰锌铁氧体
(1)按百分比称取Fe2O371.2％、MnO 21.3％、ZnO 5.6％、聚乙烯醇7‰以及余量添加剂，辅助添加剂为V2O5和Co2O3；
并将：Fe2O3、MnO和ZnO用干法混合65min后，将混料溶于去离子水中，得到浆料；
(2)将浆料送入至喷雾塔中进行喷雾干燥，喷雾塔进风温度为230℃，喷雾塔出风温度为100℃；
(3)将喷雾干燥后的材料放入电阻炉中并在氮气下820℃条件下预烧 140min，整个预烧结气氛中含有2％质量分数的氧气；
(4)将预烧后的材料进行湿法粉碎65min至粒度为1.3μm，并混合加入添加剂，然后将粉碎后的材料溶于水中；
(5)将聚乙烯醇加入至步骤(4)所得溶液中，然后在喷雾塔中进行喷雾干燥得到颗粒料，喷雾塔进风温度为230℃，喷雾塔出风温度为90℃；
((6)将颗粒料送至1100℃的烧结窑中然后升温至1360℃烧结，控制进风量为80m3/h，窑压为1.6KPa，保温氧含量为6％，在1200℃下致密化致 O2含量在1％以下，得到软磁铁氧体；
(7)将软磁铁氧体通过四轴780磨床磨面-磨底-磨面进行磨加工，即得高频低损耗、高磁导率锰锌铁氧体。
试验例
将本发明实施例1-5制得的产品与常规95材料进行性能对比，结果如表 1所示。
表1
尽管上面已经示出和描述了本发明的实施例，可以理解的是，上述实施例是示例性的，不能理解为对本发明的限制，本领域的普通技术人员在本发明的范围内可以对上述实施例进行变化、修改、替换和变型。
Claims (10)
1.一种LED用宽温高频低损耗、高磁导率锰锌铁氧体，其特征在于，包括以下物质的量分数原料：Fe2O3 65.6-75.3％、MnO 18.5-25.5％、ZnO 4.9-9.5％、聚乙烯醇7-9‰、余量为添加剂。
2.根据权利要求1所述一种LED用宽温高频低损耗、高磁导率锰锌铁氧体，其特征在于，所述辅助添加剂为CaO、SiO2、V2O5、ZrO2、Nb2O5、TiO2、SnO2和Co2O3中的一种或多种混合。
3.一种LED用宽温高频低损耗、高磁导率锰锌铁氧体的制备方法，其特征在于，包括以下步骤：
(1)按权利要求1或2所述物质的量分数称取各原料，并将：Fe2O3、MnO和ZnO用干法混合均匀后，将混料溶于水中，得到浆料；
(2)将浆料送入至喷雾塔中进行喷雾干燥；
(3)将喷雾干燥后的材料放入电阻炉中并在保护气体条件下进行预烧；
(4)将预烧后的材料进行湿法粉碎，并混合加入添加剂，然后将粉碎后的材料溶于水中；
(5)将聚乙烯醇加入至步骤(4)所得溶液中，然后在喷雾塔中进行喷雾干燥得到颗粒料；
(6)将颗粒料送至烧结窑中进行烧结，得到软磁铁氧体；
(7)将软磁铁氧体磁心磨加工，即得高频低损耗、高磁导率锰锌铁氧体。
4.根据权利要求3所述一种LED用宽温高频低损耗、高磁导率锰锌铁氧体的制备方法，其特征在于，步骤(1)中所述干法混合时间为60-70min；
所述水为去离子水。
5.根据权利要求3所述一种LED用宽温高频低损耗、高磁导率锰锌铁氧体的制备方法，其特征在于，步骤(2)中所述喷雾塔进风温度为210-230℃，喷雾塔出风温度为90-110℃。
6.根据权利要求3所述一种LED用宽温高频低损耗、高磁导率锰锌铁氧体的制备方法，其特征在于，步骤(3)中所述保护气体为氮气，且整个预烧结气氛中含有1-2％质量分数的氧气；
所述预烧温度为810-850℃，所述预烧时间为120-180min。
7.根据权利要求3所述一种LED用宽温高频低损耗、高磁导率锰锌铁氧体的制备方法，其特征在于，步骤(4)中所述湿法粉碎时间为60-80min；粉碎粒度为1.0-1.3μm。
8.根据权利要求3所述一种LED用宽温高频低损耗、高磁导率锰锌铁氧体的制备方法，其特征在于，步骤(5)中所述喷雾塔进风温度为210-230℃，喷雾塔出风温度为90-110℃。
9.根据权利要求3所述一种LED用宽温高频低损耗、高磁导率锰锌铁氧体的制备方法，其特征在于，步骤(6)中所述烧结温度为1360℃，进风量80m3/h，窑压为1.6KPa，保温氧含量为6％，在1000℃-1250℃下致密化致O2含量在1％以下。
10.根据权利要求3所述一种LED用宽温高频低损耗、高磁导率锰锌铁氧体的制备方法，其特征在于，步骤(7)中所述磨加工操作方法为通过四轴780磨床磨面-磨底-磨面进行磨加工。
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