CN110655396A - 一种高Bs低功耗锰锌铁氧体材料及其制备方法 - Google Patents
一种高Bs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 38
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 title claims abstract description 21
- 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 21
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 238000005245 sintering Methods 0.000 claims abstract description 59
- 238000000034 method Methods 0.000 claims abstract description 24
- 230000008569 process Effects 0.000 claims abstract description 18
- 229910000859 α-Fe Inorganic materials 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 11
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims abstract description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 19
- 239000001301 oxygen Substances 0.000 claims description 19
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 18
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 11
- 239000011812 mixed powder Substances 0.000 claims description 8
- 239000002270 dispersing agent Substances 0.000 claims description 6
- 239000008187 granular material Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 229920002689 polyvinyl acetate Polymers 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 6
- 239000011701 zinc Substances 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 5
- 229910001308 Zinc ferrite Inorganic materials 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000005469 granulation Methods 0.000 claims description 3
- 230000003179 granulation Effects 0.000 claims description 3
- 229920002401 polyacrylamide Polymers 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- LNRYQGINUXUWLV-UHFFFAOYSA-N [Mn].[Fe].[Zn] Chemical compound [Mn].[Fe].[Zn] LNRYQGINUXUWLV-UHFFFAOYSA-N 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052681 coesite Inorganic materials 0.000 abstract description 4
- 229910052906 cristobalite Inorganic materials 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000000377 silicon dioxide Substances 0.000 abstract description 4
- 229910052682 stishovite Inorganic materials 0.000 abstract description 4
- 229910052905 tridymite Inorganic materials 0.000 abstract description 4
- 239000000306 component Substances 0.000 description 16
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 7
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 7
- 239000011787 zinc oxide Substances 0.000 description 7
- 150000001768 cations Chemical class 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 230000004907 flux Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000011161 development Methods 0.000 description 4
- 238000009472 formulation Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000035699 permeability Effects 0.000 description 4
- 150000001450 anions Chemical class 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- 206010063385 Intellectualisation Diseases 0.000 description 1
- 229910017163 MnFe2O4 Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 229910052635 ferrosilite Inorganic materials 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- -1 oxygen ions Chemical class 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- AXWLFOKLQGDQFR-UHFFFAOYSA-N zinc iron(2+) manganese(2+) oxygen(2-) Chemical compound [O-2].[Fe+2].[Zn+2].[Mn+2].[O-2].[O-2] AXWLFOKLQGDQFR-UHFFFAOYSA-N 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Bs低功耗锰锌铁氧体材料及其制备方法。包括主要成分和辅助成分；主要成分以摩尔百分比计算，包括：54‑55mol％Fe2O3、40‑41mol％Mn3O4、4.5‑5.5mol％ZnO；辅助成分按照主要成分的重量百分比计算，包括：150‑200ppmSiO2、100‑150ppm P2O5、500‑800ppm CaO、300‑400ppm ZrO2、400‑500ppm Nb2O5。本发明在不添加NiO的基础上制备高Bs低功耗锰锌铁氧体材料，大大降低了生产成本，同时，采用独特的烧结工艺，并使用SiO2、P2O5作为烧结促进剂，有效提高了产品的烧结密度、磁导率、Bs，并大大降低了产品的功耗。
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Bs低功耗锰锌铁氧体材料及其制备方法。
背景技术
随着数字技术、汽车电子、网络通讯、能源、生物技术和国防技术等领域的飞速发展，对电子器件提出了更高的要求，而电子器件的小型化、智能化、高效率化、集成化等也使得变压器不断发展，这对作为变压器核心部件的磁性材料提出了更高的性能要求。而作为一种功能材料，软磁铁氧体对国民经济的发展起到了重要的推动作用，并在各个领域得到了广泛的应用。
开关电源变压器是在开关电源中使用的一种电子变压器，由于它工作在高功率、高Bs条件下，因而对应用在这类变压器中的磁心Bs、功耗特性要求较高。对于这类变压器来说，其工作输出功率较高，电流输出较大，可能会导致磁心饱和，从而使得导磁能力(电感量)下降。磁心的电感量会随着线圈中激磁电流的增加先增加到一个最大值，然后下降，此时磁心就饱和了。在大电流工作条件下，磁心Bs越高，其抗饱和能力便越强，传输功率就越高。同时，材料的功耗不宜过高，否则磁心本身发热增加，温度升高，一旦磁心温度高于功耗谷点温度，其功耗会更高，发热量会更大，影响整个器件的正常工作。
基于此，研发高Bs低功耗的锰锌铁氧体材料成为一种发展趋势。目前，市场上已经出现此类锰锌铁氧体材料，但其成分中含有NiO，导致其制造成本较高，限制了该类产品的推广应用。
发明内容
本发明的目的在于，提供一种高Bs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Bs低功耗锰锌铁氧体材料，其特征在于：包括主要成分和辅助成分；主要成分以摩尔百分比计算，包括：54-55mol％Fe2O3、40-41mol％Mn3O4、4.5-5.5mol％ZnO；辅助成分按照主要成分的重量百分比计算，包括：150-200ppmSiO2、100-150ppm P2O5、500-800ppmCaO、300-400ppm ZrO2、400-500ppm Nb2O5。
本发明所述高Bs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，将54-55mol％Fe2O3、40-41mol％Mn3O4、4.5-5.5mol％ZnO用混料机混合30分钟，制得混合粉料；
2、将步骤1制得的混合粉料预烧，制成预烧粉料；
3、按照主要成分的重量百分比计算，将150-200ppmSiO2、100-150ppm P2O5、500-800ppm CaO、300-400ppm ZrO2、400-500ppm Nb2O5与步骤2制得的预烧粉料充分混合后，加入适量的水和分散剂，进行砂磨，砂磨时间90分钟；砂磨结束前5分钟加入PVA胶水，制成料浆；
4、将料浆进行喷雾造粒，得到颗粒料；
5、将颗粒料压制成Φ25mm*15mm*10mm的毛坯，在气氛保护钟罩炉中，采用烧结工艺制得锰铁锌氧体材料。
优选的，步骤2中，将混合粉料置于回转窑中进行预烧，预烧温度950℃，预烧时间50分钟。
优选的，步骤3中，所述分散剂为1％的聚丙烯酰胺；所述PVA胶水为0.1％的PVA溶液。
优选的，步骤5中，所述的烧结工艺为：14-16分钟时，温度由200℃升至300℃；25-30分钟时，温度由300℃升至800℃；80-100分钟时，温度由800℃升至1100℃；120-140分钟时，温度由1100℃升至1300℃，于1300℃保温6h后，自然降温。
优选的，步骤5中，所述烧结工艺的烧结气氛处理如下：烧结过程中，温度低于900℃时，烧结气氛为空气气氛；温度为900-1100℃时，烧结气氛为氧含量5-10％；温度为1100-1250℃时，烧结气氛为氧含量2-4％；1300℃保温时，烧结气氛为氧含量保持在1-2％；自然降温过程中，1300-1150℃时，烧结气氛为氧含量0.5-0.6％；1150-900℃时，烧结气氛为氧含量低于100ppm。
有益效果：与现有技术相比，本发明在不添加NiO的基础上制备高Bs低功耗锰锌铁氧体材料，大大降低了生产成本，同时，采用独特的烧结工艺，并使用SiO2、P2O5作为烧结促进剂，有效提高了产品的烧结密度、磁导率、Bs，并大大降低了产品的功耗。
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Bs低功耗锰锌铁氧体材料，包括主要成分和辅助成分；主要成分以摩尔百分比计算，包括：54-55mol％Fe2O3、40-41mol％Mn3O4、4.5-5.5mol％ZnO；辅助成分按照主要成分的重量百分比计算，包括：150-200ppmSiO2、100-150ppm P2O5、500-800ppmCaO、300-400ppm ZrO2、400-500ppm Nb2O5。
本发明所述高Bs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，将54-55mol％Fe2O3、40-41mol％Mn3O4、4.5-5.5mol％ZnO用混料机混合30分钟，制得混合粉料；
2、将步骤1制得的混合粉料置于回转窑中进行预烧，制成预烧粉料；预烧温度950℃，预烧时间50分钟；
3、按照主要成分的重量百分比计算，将150-200ppmSiO2、100-150ppm P2O5、500-800ppm CaO、300-400ppm ZrO2、400-500ppm Nb2O5与步骤2制得的预烧粉料充分混合后，加入适量的水和分散剂，进行砂磨，砂磨时间90分钟；砂磨结束前5分钟加入PVA胶水，制成料浆；所述分散剂为1％的聚丙烯酰胺；所述PVA胶水为0.1％的PVA溶液；
4、将料浆进行喷雾造粒，得到颗粒料；
5、将颗粒料压制成Φ25mm*15mm*10mm的毛坯，在气氛保护钟罩炉中，采用烧结工艺制得锰铁锌氧体材料；
所述的烧结工艺为：14-16分钟时，温度由200℃升至300℃；25-30分钟时，温度由300℃升至800℃；80-100分钟时，温度由800℃升至1100℃；120-140分钟时，温度由1100℃升至1300℃，于1300℃保温6h后，自然降温。
所述烧结工艺的烧结气氛处理如下：烧结过程中，温度低于900℃时，烧结气氛为空气气氛；温度为900-1100℃时，烧结气氛为氧含量5-10％；温度为1100-1250℃时，烧结气氛为氧含量2-4％；1300℃保温时，烧结气氛为氧含量保持在1-2％；自然降温过程中，1300-1150℃时，烧结气氛为氧含量0.5-0.6％；1150-900℃时，烧结气氛为氧含量低于100ppm。
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540mT(25℃)和440mT(100℃)；100KHz，200mT测试功耗达到320KW/m3(100℃)。
本发明所述锰锌铁氧体材料制备方法的原理及试验过程如下：
一、技术问题
众所周知，某一温度T下，铁氧体材料饱和磁通密度Bs可以用以下公式表示：
Bs(T)＝Bs(O)×(ρ/ρt)×(1-T/Tc)×α
式中，Bs(O)：绝对温度OK下材料的饱和磁通密度；
ρ/ρt：烧结密度/理论密度比值；
Tc：居里温度；α：定值。
绝对温度OK下材料的饱和磁通密度Bs(O)、居里温度Tc和烧结密度p是实际影响饱和磁通密度的主要因素。Bs(O)主要由铁氧体材料配方所决定，锰锌铁氧体中，这个数值由MnFe2O4，ZnFe2O4和Fe3O4含量来决定。提高Bs(O)措施主要是研究如何提高铁氧体中Fe3O4成分含量。
高Bs、低功耗产品生产过程中，为了保证产品具有较高的饱和磁通密度Bs，需要用过Fe2O3配方。过Fe2O3配方带来的问题是功耗谷点温度降低到接近室温甚至更低的温度，远远偏离电压器工作温度80-100℃，从而造成磁心发热严重。为了改变这一缺点，常在过Fe2O3配方的基础上加入部分NiO。NiO能明显提高谷点温度，并且不会改变Bs大小，对功耗的影响也很小。通过加入适量的NiO，能将功耗谷点温度从低温提高到100℃左右，并且产品依然保持较低的功耗。这样，产品就具有较高的Bs和较低的功耗。
无NiO类高Bs低功耗产品的开发主要问题是如何在不加入NiO的基础上，使得产品具有较高的Bs，并保持很低的功耗。
二、技术方案
生产锰锌铁氧体材料用的主要配方原料是Fe2O3、Mn3O4、ZnO，为了保证产品具有较高的Bs，必须增加配方Fe2O3的加入量。为了消除Fe2O3加入量提高对功耗谷点温度降低的影响，需要调整主配方Mn3O4、ZnO加入量，将谷点温度提高到80-100℃。通过反复试验，确定产品最佳配方为：以摩尔百分比计算，Fe2O3∶Mn3O4∶ZnO＝54.3∶40.8∶4.9。该配方Fe2O3加入量较高，并且谷点温度在100℃左右。
用上述配方进行实验，虽然谷点温度达到要求，但是Bs和功耗并未达到预期要求。1300℃，保温5h烧结后，烧结密度仅有4.68g/cm3，磁导率1600，25℃Bs也只有510mT，并且功耗也较高。究其原因，还是该配方烧结反应进行不充分。过Fe2O3配方烧结过程中，过量Fe2O3引入更多的阳离子空位。对锰锌铁氧体来说，烧结过程中，阳离子空位Vc与阴离子空位Va乘积为一定值：
Vc*Va＝K
阳离子空位增多意味着阴离子空位Va减少，烧结过程中尖晶石内部氧离子扩散速度降低，固相反应较慢。这样烧结的产品晶粒小、气孔多，密度和磁导率较低，功耗很难降低。
为了使得产品能烧结充分，做了以下改进：
(1)加入适量P2O5、SiO2作为烧结助剂
P2O5熔点为360℃，能在较低的烧结温度下就成为液相，促进烧结反应进行；SiO2能与Fe2O3反应形成FeSiO3，其熔点1100℃左右，低于锰锌铁氧体的烧结温度，因而也能形成液相，促进烧结反应进行。需要注意的是，这两类添加剂容易导致产品结晶，应合理控制加入量。
通过进行正交试验，最终这两种添加剂的最佳加入量：P2O5：0.01％，SiO2：0.015％。
同样经过1300℃，保温5h烧结后，产品烧结密度提高到4.82g/cm3，磁导率提高到1880，25℃Bs提高至523mT。产品性能大幅改善。
(2)低氧气氛烧结
铁氧体烧结过程中发生的主要反应：
2Fe3++3/4Vc+O2-<＝>2Fe2++1/2O2
式中，Vc为阳离子空位数量。
降低烧结气氛氧含量，烧结反应向左进行，阳离子空位Vc减少，相应的，阴离子空位Va增多，固相反应加快。
将烧结保温气氛氧含量由8％降低到2％，经1300℃，保温5h烧结后，烧结密度提高到4.89g/cm3，磁导率提高到2090，25℃Bs提高到540mT，100℃Bs达到450mT。谷点温度在95℃，功耗310KW/m3。产品性能完全满足高Bs、低功耗MnZn铁氧体材料的使用要求。
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Bs低功耗锰锌铁氧体材料，其特征在于：包括主要成分和辅助成分；主要成分以摩尔百分比计算，包括：54-55mol％Fe2O3、40-41mol％Mn3O4、4.5-5.5mol％ZnO；辅助成分按照主要成分的重量百分比计算，包括：150-200ppmSiO2、100-150ppm P2O5、500-800ppmCaO、300-400ppm ZrO2、400-500ppm Nb2O5。
2.如权利要求1所述高Bs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)以摩百分比计算，将54-55mol％Fe2O3、40-41mol％Mn3O4、4.5-5.5mol％ZnO用混料机混合30分钟，制得混合粉料；
(2)将步骤(1)制得的混合粉料预烧，制成预烧粉料；
(3)按照主要成分的重量百分比计算，将150-200ppmSiO2、100-150ppm P2O5、500-800ppm CaO、300-400ppm ZrO2、400-500ppm Nb2O5与步骤(2)制得的预烧粉料充分混合后，加入适量的水和分散剂，进行砂磨，砂磨时间90分钟；砂磨结束前5分钟加入PVA胶水，制成料浆；
(4)将料浆进行喷雾造粒，得到颗粒料；
(5)将颗粒料压制成Φ25mm*15mm*10mm的毛坯，在气氛保护钟罩炉中，采用烧结工艺制得锰铁锌氧体材料。
3.根据权利要求2所述高Bs低功耗锰锌铁氧体材料的制备方法，其特征在于：步骤(2)中，将混合粉料置于回转窑中进行预烧，预烧温度950℃，预烧时间50分钟。
4.根据权利要求2所述高Bs低功耗锰锌铁氧体材料的制备方法，其特征在于：步骤(3)中，所述分散剂为1％的聚丙烯酰胺；所述PVA胶水为0.1％的PVA溶液。
5.根据权利要求2所述高Bs低功耗锰锌铁氧体材料的制备方法，其特征在于：步骤(5)中，所述的烧结工艺为：14-16分钟时，温度由200℃升至300℃；25-30分钟时，温度由300℃升至800℃；80-100分钟时，温度由800℃升至1100℃；120-140分钟时，温度由1100℃升至1300℃，于1300℃保温6h后，自然降温。
6.根据权利要求5所述高Bs低功耗锰锌铁氧体材料的制备方法，其特征在于：步骤(5)中，所述烧结工艺的烧结气氛处理如下：烧结过程中，温度低于900℃时，烧结气氛为空气气氛；温度为900-1100℃时，烧结气氛为氧含量5-10％；温度为1100-1250℃时，烧结气氛为氧含量2-4％；1300℃保温时，烧结气氛为氧含量保持在1-2％；自然降温过程中，1300-1150℃时，烧结气氛为氧含量0.5-0.6％；1150-900℃时，烧结气氛为氧含量低于100ppm。
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