CN112094115A - 超高磁导率锰锌铁氧体材料及其制备方法 - Google Patents
超高磁导率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 37
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 title claims abstract description 29
- 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 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 230000035699 permeability Effects 0.000 claims abstract description 17
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 11
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000007921 spray Substances 0.000 claims description 35
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 23
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 15
- 239000001301 oxygen Substances 0.000 claims description 15
- 229910052760 oxygen Inorganic materials 0.000 claims description 15
- 238000005245 sintering Methods 0.000 claims description 15
- 239000012298 atmosphere Substances 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000001238 wet grinding Methods 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 9
- 238000001694 spray drying Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000007599 discharging Methods 0.000 claims description 5
- 239000008187 granular material Substances 0.000 claims description 5
- 238000005469 granulation Methods 0.000 claims description 5
- 230000003179 granulation Effects 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 4
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- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 3
- 238000000748 compression moulding Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 7
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 239000000696 magnetic material Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
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- 239000004372 Polyvinyl alcohol Substances 0.000 description 6
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- 229920002451 polyvinyl alcohol Polymers 0.000 description 6
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Abstract
本发明公开了一种超高磁导率锰锌铁氧体材料及其制备方法,涉及磁性材料领域。用以解决现有技术中对高导磁率材料需求的问题,其包含功能性组分和辅助性组分,其中功能性组分及用量为:50.15‑55.3mol%Fe2O3、23.25‑27.75mol%MnO、19.93‑24.05mol%ZnO,辅助组分及其用量按照重量百分比来计算为0.005‑0.01%SiO2,0.01‑0.03%CaO,0.05‑0.1%Bi2O3。本发明所制得得锰锌铁氧体磁性得初始磁导率可以达到22000,距离温度达到120℃以上,有良好的材料频率特性、损耗特性,有利于器件和系统的小型化、轻量化,具有巨大的环保和经济效意。
Description
技术领域
本发明涉及磁性材料领域,具体地说,涉及一种超高导磁率锰锌铁氧体材料及其制备方法。
背景技术
进入20世纪80年代以后,软磁铁氧体材料总产量有了很大的增长,除了功率铁氧体有了很大的发展以外,还与高ui材料的应用领域得到开拓有关,高ui材料的产品已占到软磁铁氧体的30%左右,现已成为广大铁氧体工作者研究开发的重点方向之一。高导磁率的锰锌铁氧体由于材料的磁导率高时,较少的线圈匝数就可以获得需求的电感量,进而有效地降低线圈的直流电阻及由其引起的损耗,能明显减小变压器的体积,有利于器件和系统的小型化、轻量化,适用于宽频多频段高磁导率产品。
发明内容
为解决上述问题,本发明提供一种超高磁导率锰锌铁氧体材料及其制备方法,其具有较高的初始导磁率,生产成本低、顺应现代电子产品的发展趋势。
本发明所述的超高磁导率锰锌铁氧体材料,包含功能性组分和辅助性组分,其中功能性组分及用量为:50.15-55.3mol%Fe2O3、23.25-27.75mol%MnO、19.93-24.05mol%ZnO,辅助组分及其用量为0.005-0.01%SiO2,0.01-0.03%CaO,0.05-0.1%Bi2O3,辅助性组分的用量为其占功能性组分质量的百分比。
本发明的另一个目的是提供一种超高导磁率锰锌铁氧体材料的制备方法,包括以下步骤:(1)湿法混合,(2)喷雾干燥,(3)预烧,(4)湿法粉碎,(5)喷雾造粒,(6)压制成型,(7)烧结;其中,烧结具体操作条件为:①从室温以0.5-2℃/min升温至500℃;②从500℃以1.5-2.0℃/min升温至1000℃;③从1000℃以2.0-5℃/min升温速度升至终烧温度1430-1450℃;④保温5-8h。保温5-8h后,关闭炉门,充氮气,调解平衡炉体气氛:自然降温至1400±10℃充氮气,控制氧含量在1.3%-2%;自然降温降至1200-1000℃,控制氧含量低于1.0%,自然冷却到低于200℃以下出炉。
进一步的,步骤(1)中,湿法混合使用去离子水作为溶剂,混合时间为60-70分钟。
进一步的,步骤(2)中,在喷雾塔中进行干燥,喷雾塔进风温度为220±10℃,喷雾塔出风温度为100±10℃。
进一步的,步骤(3)中,将喷雾干燥后的材料在保护气氛电阻炉中进行预烧,预烧温度为830±20℃,预烧时间为120-180分钟,预烧气氛为氮气保护,氧含量为1%-2%。
进一步的,步骤(4)中,预烧得到的预烧料进行湿法粉碎,使用去离子水作为溶剂,粉碎时间为60-80分钟,粉碎后料浆粒径控制在1.0-1.3μm。
进一步的,步骤(5)中,预烧后的原料中加入相当于原料重量的10-13%的PVA,在喷雾塔中进行干燥得到颗粒料,喷雾塔进风温度为220±10℃,喷雾塔出风温度为100±10℃。
进一步的,步骤(6)中,成型坯件为外径18mm,内径8mm,高度5mm的圆环状,密度为2.90-2.95g/cm3。
与现有技术相比,本发明的有益效果是:(1)本发明所制得得锰锌铁氧体磁性得初始磁导率可以达到22000,距离温度达到120℃以上;(2)本发明所述得制备方法,保证烧结磁心具有较高的磁导率,有良好的材料频率特性、损耗特性,有利于器件和系统的小型化、轻量化,具有巨大的环保和经济效意。
具体实施方式
下面结合实施例对本发明做进一步解释。
实施例1
一种超高磁导率锰锌铁氧体材料,包含功能性组分和辅助性组分,其中功能行组分及用量为:50.15mol%Fe2O3、23.25mol%MnO、19.93mol%ZnO,其他为辅助性组份,辅助组分及其各组分占功能性组分总量的质量百分比为0.005%SiO2,0.01%CaO,0.05%Bi2O3。具体制备方法为:
(1)湿法混合:湿法混合使用去离子水作为溶剂,混合时间为60分钟。
(2)喷雾干燥:在喷雾塔中进行喷雾干燥,喷雾塔进风温度为220±10℃,喷雾塔出风温度为100±10℃。
(3)预烧:将喷雾干燥后的材料在保护气氛电阻炉中进行预烧,预烧温度为830℃,预烧时间为120分钟,预烧气氛为氮气保护,氧含量为1%。
(4)湿法粉碎:预烧得到的预烧料进行湿法粉碎,使用去离子水作为溶剂,粉碎时间为60分钟,粉碎后料浆粒径控制在1.0μm。
(5)喷雾造粒:预烧后的原料中加入相当于原料重量的10%的PVA,在喷雾塔中进行干燥得到颗粒料,喷雾塔进风温度为220±10℃,喷雾塔出风温度为100±10℃。
(6)压制成型:成型坯件密度为2.90g/cm3,成型坯件为外径18mm,内径8mm,高度5mm的圆环状。
(7)烧结;其中,烧结具体操作条件为:①从室温以0.5℃/min升温至500℃;②从500℃以1.5℃/min升温至1000℃;③从1000℃以3.0℃/min升温速度升至终烧温度1450℃;④保温5h。保温5h后,关闭炉门,充氮气,调解平衡炉体气氛:自然降温至1410℃充氮气,控制氧含量在1.5%左右;自然降温降至1200℃,控制氧含量为0.7%,自然冷却到180℃出炉。
该实施例所制得的锰锌铁氧体材料的初始导磁率为22000,居里温度120℃,25℃饱和磁通密度Bs达到380mT,100℃饱和磁通密度Bs达到220mT。
实施例2
本发明所述的超高磁导率锰锌铁氧体材料,包含功能性组分和辅助性组分,其中功能行组分及用量为:55.3mol%Fe2O3、27.75mol%MnO、24.05mol%ZnO,其他为辅助性组份,辅助组分及其用量按照重量百分比来计算为0.01%SiO2,0.03%CaO,0.1%Bi2O3。
本发明的另一个目的是提供上述超高磁导率锰锌铁氧体材料的制备方法,包括以下步骤:
(1)湿法混合:湿法混合使用去离子水作为溶剂,混合时间为70分钟。
(2)喷雾干燥:在喷雾塔中进行喷雾干燥,喷雾塔进风温度为220±10℃,喷雾塔出风温度为100±10℃。
(3)预烧:将喷雾干燥后的材料在保护气氛电阻炉中进行预烧,预烧温度为850℃,预烧时间为180分钟,预烧气氛为氮气保护,氧含量为2%。
(4)湿法粉碎:预烧得到的预烧料进行湿法粉碎,使用去离子水作为溶剂,粉碎时间为60分钟,粉碎后料浆粒径控制在1.3μm。
(5)喷雾造粒:预烧后的原料中加入相当于原料重量的13%的PVA,在喷雾塔中进行干燥得到颗粒料,喷雾塔进风温度为220±10℃,喷雾塔出风温度为100±10℃。
(6)压制成型:成型坯件密度为2.95g/cm3,成型坯件为外径18mm,内径8mm,高度5mm的圆环状。
(7)烧结;其中,烧结具体操作条件为:①从室温以1.5℃/min升温至500℃;②从500℃以2.0℃/min升温至1000℃;③从1000℃以4℃/min升温速度升至终烧温度1430℃;④保温8h。保温8h后,关闭炉门,充氮气,调解平衡炉体气氛:自然降温至1400℃充氮气,控制氧含量在1.5%左右;自然降温降至1100℃,控制氧含量为0.6%,自然冷却到190℃出炉。
该实施例所制得的锰锌铁氧体材料的初始导磁率为22100,居里温度126℃,25℃饱和磁通密度Bs达到400mT,100℃饱和磁通密度Bs达到210mT。
实施例3
本发明所述的超高磁导率锰锌铁氧体材料,包含功能性组分和辅助性组分,其中功能行组分及用量为:504.1mol%Fe2O3、25.5mol%MnO、20.8mol%ZnO,其他为辅助性组份,辅助组分及其用量按照重量百分比来计算为0.008%SiO2,0.02%CaO,0.09%Bi2O3。
本发明的另一个目的是提供上述超高磁导率锰锌铁氧体材料的制备方法,包括以下步骤:
(1)湿法混合:湿法混合使用去离子水作为溶剂,混合时间为65分钟。
(2)喷雾干燥:在喷雾塔中进行喷雾干燥,喷雾塔进风温度为220±10℃,喷雾塔出风温度为100±10℃。
(3)预烧:将喷雾干燥后的材料在保护气氛电阻炉中进行预烧,预烧温度为840℃,预烧时间为150分钟,预烧气氛为氮气保护,氧含量为2%。
(4)湿法粉碎:预烧得到的预烧料进行湿法粉碎,使用去离子水作为溶剂,粉碎时间为70分钟,粉碎后料浆粒径控制在1.2μm。
(5)喷雾造粒:预烧后的原料中加入相当于原料重量的11%的PVA,在喷雾塔中进行干燥得到颗粒料,喷雾塔进风温度为220±10℃,喷雾塔出风温度为100±10℃。
(6)压制成型:成型坯件密度为2.93g/cm3,成型坯件为外径18mm,内径8mm,高度5mm的圆环状。
(7)烧结;其中,烧结具体操作条件为:①从室温以1℃/min升温至500℃;②从500℃以1.7℃/min升温至1000℃;③从1000℃以3.5/min升温速度升至终烧温度1445℃;④保温6h。保温6h后,关闭炉门,充氮气,调解平衡炉体气氛:自然降温至1405℃充氮气,控制氧含量在1.5%左右;自然降温降至1000℃,控制氧含量为0.8%,自然冷却到195℃出炉。
该实施例所制得的锰锌铁氧体材料的初始导磁率为21900,居里温度121℃,25℃饱和磁通密度Bs达到388mT,100℃饱和磁通密度Bs达到230mT。
Claims (9)
1.一种超高磁导率锰锌铁氧体材料,其特征在于,包含功能性组分和辅助性组分,其中功能性组分及用量为:50.15-55.3mol%Fe2O3、23.25-27.75mol%MnO、19.93-24.05mol%ZnO,辅助组分及其用量按照重量百分比来计算为0.005-0.01%SiO2,0.01-0.03%CaO,0.05-0.1%Bi2O3。
2.根据权利要求1所述的超高导磁率锰锌铁氧体材料的制备方法,其特征在于,包括以下步骤:(1)湿法混合,(2)喷雾干燥,(3)预烧,(4)湿法粉碎,(5)喷雾造粒,(6)压制成型,(7)烧结;其中,烧结具体操作条件为:①从室温以0.5-2℃/min升温至500℃;②从500℃以1.5-2.0℃/min升温至1000℃;③从1000℃以2.0-5℃/min升温速度升至终烧温度1430-1450℃;④保温5-8h。
3.根据权利要求2所述的超高导磁率锰锌铁氧体的制备方法,其特征在于,保温5-8h后,关闭炉门,充氮气,调解平衡炉体气氛:自然降温至1400±10℃充氮气,控制氧含量在1.3%-2%;自然降温降至1200-1000℃,控制氧含量低于1.0%,自然冷却到低于200℃以下出炉。
4.根据权利要求2所述的超高导磁率锰锌铁氧体的制备方法,其特征在于,步骤(1)中,湿法混合使用去离子水作为溶剂,混合时间为60-70分钟。
5.根据权利要求2所述的超高导磁率锰锌铁氧体的制备方法,其特征在于,步骤(2)中,在喷雾塔中进行干燥,喷雾塔进风温度为220±10℃,喷雾塔出风温度为100±10℃。
6.根据权利要求2所述的超高导磁率锰锌铁氧体的制备方法,其特征在于,步骤(3)中,将喷雾干燥后的材料在保护气氛电阻炉中进行预烧,预烧温度为830±20℃,预烧时间为120-180分钟,预烧气氛为氮气保护,氧含量为1%-2%。
7.根据权利要求2所述的超高导磁率锰锌铁氧体的制备方法,其特征在于,步骤(4)中,预烧得到的预烧料进行湿法粉碎,使用去离子水作为溶剂,粉碎时间为60-80分钟,粉碎后料浆粒径控制在1.0-1.3μm。
8.根据权利要求2所述的超高导磁率锰锌铁氧体的制备方法,其特征在于,步骤(5)中,预烧后的原料中加入相当于原料重量的10-13%的PVA,在喷雾塔中进行干燥得到颗粒料,喷雾塔进风温度为220±10℃,喷雾塔出风温度为100±10℃。
9.根据权利要求2所述的超高导磁率锰锌铁氧体的制备方法,其特征在于,步骤(6)中,成型坯件为外径18mm,内径8mm,高度5mm的圆环状,密度为2.90-2.95g/cm3。
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