CN107151135B - 一种绿色照明用纳米软磁铁氧体及其制备方法 - Google Patents

一种绿色照明用纳米软磁铁氧体及其制备方法 Download PDF

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CN107151135B
CN107151135B CN201710341814.5A CN201710341814A CN107151135B CN 107151135 B CN107151135 B CN 107151135B CN 201710341814 A CN201710341814 A CN 201710341814A CN 107151135 B CN107151135 B CN 107151135B
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CN107151135A (zh
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瞿德林
王久如
王晓祥
李丛俊
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Zhongde Electronics Co ltd
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Abstract

本发明公开了一种绿色照明用纳米软磁铁氧体及其制备方法，包括如下步骤：S1、将溶剂、助剂和表面活剂在微波条件下混合均匀得到混合液；S2、按配比将主料和蒸馏水混合均匀，加入混合液搅拌混合得到乳液1；S3、另取混合液依次加入氢氧化钠和氨水，搅拌得到乳液2；S4、将乳液1滴加至乳液2中，搅拌，静置陈化离心洗涤，干燥得到物料1；S5、将氧化钴、五氧化二钒、二氧化钛、碳酸钙和二氧化硅混合均匀后，球磨，加入物料1混合均匀，压制成型，烧结后冷却得到绿色照明用纳米软磁铁氧体。本发明添加了铜离子，采用多组分参杂，优化了乳化液组分，拓宽了铁氧体材料适用温域范围，提高了低温条件下的电磁性能，满足了绿色照明的使用要求。

Description

一种绿色照明用纳米软磁铁氧体及其制备方法
技术领域
本发明涉及纳米软磁铁氧体技术领域，尤其涉及一种绿色照明用纳米软磁铁氧体及其制备方法。
背景技术
绿色照明是指通过提高照明电器和系统的效率来节约能源，通过减少发电排放的大气污染物和温室气体来保护环境，从而达到改善生活质量、提高工作效率、营造现代光文化的目的。绿色照明不只是简单的节能和节约电费的经济效益问题，而是将认识提高到节约能源、保护环境的高度，更加着眼于资源的利用和环境保护。当前市场上最优质的光源当数高频无极灯和发光二极管(LED)，两者都离不开高性能的铁氧体磁芯，由于电阻率高、涡流损耗小、的特性，镍锌铁氧体材料成为绿照明领域常用的功能材料之一。虽然镍锌铁氧体具有高频，电阻率高的优点，但是其在低温无法保证较高的磁导率，且损耗较大，因此，对镍锌软磁铁氧体的性能改进是目前急需解决的问题。
近年来随着研究的不断深入，制备工艺的不断改进，铁氧体粉体特别是纳米粉体制备工艺取得快速发展，涌现出如高能球磨法、溶胶-凝胶-自蔓延燃烧法、湿法如水热法、化学共沉淀法等多种工艺路线。但是目前工艺制得绿色照明用软磁铁氧体的性能不是特别理想，损耗率及适用温度范围等无法很好的满足绿色照明领域对铁氧体材料的要求，工艺大多复杂，成本高。本发明基于微乳液法，对镍锌铁氧体制备工艺进行改进，旨在寻求一种简单、高效且制品满足实际使用要求的软磁铁氧体的制备工艺。
发明内容
本发明提出了一种绿色照明用纳米软磁铁氧体及其制备方法，拓宽了铁氧体材料适用温域范围，提高了低温条件下的电磁性能，降低了磁芯损耗，满足了绿色照明的使用要求。
本发明提出的一种绿色照明用纳米软磁铁氧体的制备方法，包括如下步骤：
S1、将溶剂、助剂和表面活剂在微波条件下混合均匀得到混合液；
S2、按配比将主料和蒸馏水混合均匀，加入混合液搅拌混合得到乳液1，主料按摩尔份数包括：40-50份硝酸铁、10-25份硝酸锌、5-15份硝酸镍、3-8份硝酸铜；
S3、另取混合液依次加入0.5-1mol/L氢氧化钠和浓度为20-30wt％氨水，搅拌得到乳液2；
S4、将乳液1滴加至乳液2中，搅拌，静置陈化12-16h，离心洗涤，干燥得到物料1；
S5、将氧化钴、五氧化二钒、二氧化钛、碳酸钙和二氧化硅混合均匀后，球磨至粒径为100-300nm，加入物料1混合均匀，压制成型，烧结后冷却得到绿色照明用纳米软磁铁氧体。
优选地，S1中，混合液中溶剂和助剂的体积比为10：1-3，溶剂与表面活性剂的体积重量比ml：g为100：1-3。
优选地，S1中，溶剂为甲苯或/或环己烷，助剂为正己醇，表面活性剂为十二烷基苯磺酸钠、十二烷基磺酸钠、十六烷基三甲基溴化铵、十二烷基硫酸钠、异辛基苯基聚氧乙烯醚中的一种或两种以上混合物。
优选地，S2中，主料与混合液摩尔体积比mol：ml为10-15：1，混合液与蒸馏水的体积比为2-4：1。
优选地，S3中，氢氧化钠、氨水、混合液的体积比为4-5：8-12：100。
优选地，S4中，乳液1与乳液2的体积比为1：1-1.3。
本发明中乳液1需缓慢滴加，控制滴加速度为3-5ml/min，滴加后进行强烈搅拌使乳液1和乳液2均匀混合并反应完全，反应完成后，将反应液用无水乙醇进行离心洗涤，以除去残留在产物表面活性剂和有机溶剂。
本发明中球磨可采用干法球磨或湿法球磨。
优选地，S5中，氧化钴、五氧化二钒、二氧化钛、碳酸钙和二氧化硅的重量比为3-5：1-3：0.5-1：0.3-0.5：0.3-0.5；优选地，碳酸钙和二氧化硅的重量比为1：1。
优选地，S5中，物料1与氧化钴的重量比为100：0.05-0.1。
优选地，烧结温度为850-930℃，烧结时间为6-8h。
优选地，在850-900℃下保温烧结4-6h，然后升温900-930℃保温烧结2-3h。
本发明提出的一种绿色照明用纳米软磁铁氧体，由绿色照明用纳米软磁铁氧体的制备方法制得。
本发明以微乳液法为基础，在镍锌铁氧体中添加了铜离子，同时采用多组分参杂，并控制各部工艺参数对镍锌铁氧体性能晶型改进；其中，铜离子的加入替换了部分铁离子，使得烧结温度降低、密度增大，磁矩增加，但是CuO添加量过大时，由于过烧使密度下降、气孔增多，导致磁导率下降，同时过多的CuO析出在晶粒边界上，引起晶粒畸变，致使磁导率降低，因此需严格控制铜离子添加量；氧化钴、五氧化二钒配合，利用钴离子和亚铁离子产生叵明伐效应，钴离子沿各磁畴自发磁化方向有序扩散，形成局域性感生单轴各向异性，同时五氧化二钒促使晶粒均匀、连续生长，可促进材料的晶粒生长、致密化并降低损耗，拓宽了镍锌铁氧体的温域，尤其是低温条件下的低损耗和电磁性能；碳酸钙在高温下与二氧化硅生成偏硅酸钙，具有很高的电阻率，提高了晶界电阻率，抑制了涡流损耗，二氧化钛和氧化钴抵消铁离子的各向异性，使铁氧体的各向异性值趋近于零，提高低温条件下的磁导率，矫顽力磁滞损耗也有所下降。
本发明工艺中优化了乳化液组分，以溶剂、助剂和表面活剂配合，将主料和碱液分别乳化，两者在纳米微球中进行反应，细化了铁氧体粉末颗粒，为后期研磨和烧结打好基础，使参杂料更好的渗入铁氧基体中，同时控制烧结工艺步骤，促进铁氧体的传质和烧结，加速晶粒生长，进一步提高产品的低温磁导率和温域范围，有效降低磁芯损耗。
具体实施方式
下面，通过具体实施例对本发明的技术方案进行详细说明。
实施例1
一种绿色照明用纳米软磁铁氧体，由如下步骤制得：
S1、将溶剂、助剂和表面活剂在微波条件下混合均匀得到混合液；
S2、按配比将主料和蒸馏水混合均匀，加入混合液搅拌混合得到乳液1，主料按摩尔份数包括：40份硝酸铁、25份硝酸锌、5份硝酸镍、8份硝酸铜；
S3、另取混合液依次加入0.5mol/L氢氧化钠和浓度为30wt％氨水，搅拌得到乳液2；
S4、将乳液1滴加至乳液2中，搅拌，静置陈化12h，离心洗涤，干燥得到物料1；
S5、将氧化钴、五氧化二钒、二氧化钛、碳酸钙和二氧化硅混合均匀后，球磨至粒径为100nm，加入物料1混合均匀，压制成型，烧结后冷却得到绿色照明用纳米软磁铁氧体。
实施例2
一种绿色照明用纳米软磁铁氧体，由如下步骤制得：
S1、将溶剂、助剂和表面活剂在微波条件下混合均匀得到混合液；其中，混合液中溶剂和助剂的体积比为10：1，溶剂与表面活性剂的体积重量比ml：g为100：3，溶剂为甲苯，助剂为正己醇，表面活性剂为十二烷基苯磺酸钠；
S2、按配比将主料和蒸馏水混合均匀，加入混合液搅拌混合得到乳液1，主料按摩尔份数包括：50份硝酸铁、10份硝酸锌、15份硝酸镍、3份硝酸铜；其中，主料与混合液摩尔体积比mol：ml为10：1，混合液与蒸馏水的体积比为2：1；
S3、另取混合液依次加入1mol/L氢氧化钠和浓度为20wt％氨水，搅拌得到乳液2；其中，氢氧化钠、氨水、混合液的体积比为4：8：100；
S4、将乳液1滴加至乳液2中，搅拌，静置陈化12h，离心洗涤，干燥得到物料1；其中，乳液1与乳液2的体积比为1：1；
S5、将氧化钴、五氧化二钒、二氧化钛、碳酸钙和二氧化硅混合均匀后，球磨至粒径为300nm，加入物料1混合均匀，压制成型，烧结后冷却得到绿色照明用纳米软磁铁氧体；其中，氧化钴、五氧化二钒、二氧化钛、碳酸钙和二氧化硅的重量比为3：1：0.5：0.3：0.5，物料1与氧化钴的重量比为100：0.05，烧结温度为850℃，烧结时间为8h。
实施例3
一种绿色照明用纳米软磁铁氧体，由如下步骤制得：
S1、将溶剂、助剂和表面活剂在微波条件下混合均匀得到混合液；其中，混合液中溶剂和助剂的体积比为10：3，溶剂与表面活性剂的体积重量比ml：g为100：1，溶剂为环己烷，助剂为正己醇，表面活性剂为十二烷基磺酸钠；
S2、按配比将主料和蒸馏水混合均匀，加入混合液搅拌混合得到乳液1，主料按摩尔份数包括：45份硝酸铁、20份硝酸锌、10份硝酸镍、5份硝酸铜；其中，主料与混合液摩尔体积比mol：ml为15：1，混合液与蒸馏水的体积比为4：1；
S3、另取混合液依次加入1mol/L氢氧化钠和浓度为20wt％氨水，搅拌得到乳液2；其中，氢氧化钠、氨水、混合液的体积比为5：12：100；
S4、将乳液1滴加至乳液2中，搅拌，静置陈化12h，离心洗涤，干燥得到物料1；其中，乳液1与乳液2的体积比为1：1.3；
S5、将氧化钴、五氧化二钒、二氧化钛、碳酸钙和二氧化硅混合均匀后，球磨至粒径为300nm，加入物料1混合均匀，压制成型，烧结后冷却得到绿色照明用纳米软磁铁氧体；其中，氧化钴、五氧化二钒、二氧化钛、碳酸钙和二氧化硅的重量比为5：3：1：0.5：0.3，物料1与氧化钴的重量比为100：0.1，烧结温度为930℃，烧结时间为6h。
实施例4
一种绿色照明用纳米软磁铁氧体，由如下步骤制得：
S1、将溶剂、助剂和表面活剂在微波条件下混合均匀得到混合液；其中，混合液中溶剂和助剂的体积比为10：2，溶剂与表面活性剂的体积重量比ml：g为100：2，溶剂为甲苯，助剂为正己醇，表面活性剂为十六烷基三甲基溴化铵；
S2、按配比将主料和蒸馏水混合均匀，加入混合液搅拌混合得到乳液1，主料按摩尔份数包括：45份硝酸铁、20份硝酸锌、10份硝酸镍、5份硝酸铜；其中，主料与混合液摩尔体积比mol：ml为12：1，混合液与蒸馏水的体积比为3：1；
S3、另取混合液依次加入1mol/L氢氧化钠和浓度为20wt％氨水，搅拌得到乳液2；其中，氢氧化钠、氨水、混合液的体积比为4.5：10：100；
S4、将乳液1滴加至乳液2中，搅拌，静置陈化12h，离心洗涤，干燥得到物料1；其中，乳液1与乳液2的体积比为1：1.2；
S5、将氧化钴、五氧化二钒、二氧化钛、碳酸钙和二氧化硅混合均匀后，球磨至粒径为300nm，加入物料1混合均匀，压制成型，烧结后冷却得到绿色照明用纳米软磁铁氧体；其中，氧化钴、五氧化二钒、二氧化钛、碳酸钙和二氧化硅的重量比为4：2：0.8：0.4：0.4，物料1与氧化钴的重量比为100：0.08，在880℃下保温烧结6h，然后升温930℃保温烧结2h。
实施例5
一种绿色照明用纳米软磁铁氧体，由如下步骤制得：
S1、将溶剂、助剂和表面活剂在微波条件下混合均匀得到混合液；其中，混合液中溶剂和助剂的体积比为10：2，溶剂与表面活性剂的体积重量比ml：g为100：2，溶剂为甲苯，助剂为正己醇，表面活性剂为十二烷基苯磺酸钠；
S2、按配比将主料和蒸馏水混合均匀，加入混合液搅拌混合得到乳液1，主料按摩尔份数包括：45份硝酸铁、20份硝酸锌、10份硝酸镍、5份硝酸铜；其中，主料与混合液摩尔体积比mol：ml为12：1，混合液与蒸馏水的体积比为3：1；
S3、另取混合液依次加入1mol/L氢氧化钠和浓度为20wt％氨水，搅拌得到乳液2；其中，氢氧化钠、氨水、混合液的体积比为4.5：10：100；
S4、将乳液1滴加至乳液2中，搅拌，静置陈化12h，离心洗涤，干燥得到物料1；其中，乳液1与乳液2的体积比为1：1.2；
S5、将氧化钴、五氧化二钒、二氧化钛、碳酸钙和二氧化硅混合均匀后，球磨至粒径为300nm，加入物料1混合均匀，压制成型，烧结后冷却得到绿色照明用纳米软磁铁氧体；其中，氧化钴、五氧化二钒、二氧化钛、碳酸钙和二氧化硅的重量比为4：2：0.8：0.4：0.4，物料1与氧化钴的重量比为100：0.08，在900℃下保温烧结4h，然后升温930℃保温烧结3h。
对照例
一种纳米软磁铁氧体，由如下步骤制得：
S1、按配比将主料和蒸馏水混合均匀，得到溶液1，主料按摩尔份数包括：45份硝酸铁、20份硝酸锌、10份硝酸镍、5份硝酸铜；其中，主料与蒸馏水摩尔体积比mol：ml为12：0.3，表面活性剂为十二烷基苯磺酸钠；
S2、将1mol/L氢氧化钠和浓度为20wt％氨水，搅拌得到溶液2；其中，氢氧化钠、氨水的体积比为4.5：10；
S3、将溶液1滴加至溶液2中，搅拌，静置陈化12h，离心洗涤，干燥得到物料1；其中，溶液1与溶液2的体积比为1：1.2；
S4、将氧化钴、五氧化二钒、二氧化钛、碳酸钙和二氧化硅混合均匀后，球磨至粒径为300nm，加入物料1混合均匀，压制成型，烧结后冷却得到绿色照明用纳米软磁铁氧体；其中，氧化钴、五氧化二钒、二氧化钛、碳酸钙和二氧化硅的重量比为4：2：0.8：0.4：0.4，物料1与氧化钴的重量比为100：0.08，在900℃下保温烧结4h，然后升温930℃保温烧结3h。
将实施4-5制得的绿色照明用纳米软磁铁氧体与对照例制得纳米软磁铁氧体进行性能测试，测试结果如下表所示：
Figure BDA0001295375350000081
Figure BDA0001295375350000091
从测试数据可以看出，本发明以微乳液法为基础，在镍锌铁氧体中添加了铜离子，同时采用多组分参杂，优化了乳化液组分，以溶剂、助剂和表面活剂配合，大大拓宽了铁氧体材料适用温域范围，提高了低温条件下的电磁性能，降低了磁芯损耗，促进铁氧体的传质和烧结，加速晶粒生长，致密化，提高了制品的密度，满足了绿色照明的使用要求。
以上所述，仅为本发明较佳的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，根据本发明的技术方案及其发明构思加以等同替换或改变，都应涵盖在本发明的保护范围之内。

Claims (4)

1.一种绿色照明用纳米软磁铁氧体的制备方法，其特征在于，包括如下步骤：
S1、将溶剂、助剂和表面活剂在微波条件下混合均匀得到混合液；
S2、按配比将主料和蒸馏水混合均匀，加入混合液搅拌混合得到乳液1，主料按摩尔份数包括：40-50份硝酸铁、10-25份硝酸锌、5-15份硝酸镍和3-8份硝酸铜；
S3、另取混合液依次加入0.5-1mol/L氢氧化钠和浓度为20-30wt％氨水，搅拌得到乳液2；
S4、将乳液1滴加至乳液2中，搅拌，静置陈化12-16h，离心洗涤，干燥得到物料1；
S5、将氧化钴、五氧化二钒、二氧化钛、碳酸钙和二氧化硅混合均匀后，球磨至粒径为100-300nm，加入物料1混合均匀，压制成型，烧结后冷却得到绿色照明用纳米软磁铁氧体；
S1中，混合液中溶剂和助剂的体积比为10：1-3，溶剂与表面活性剂的体积重量比ml：g为100：1-3；
S1中，溶剂为甲苯或环己烷，助剂为正己醇，表面活性剂为十二烷基苯磺酸钠、十二烷基磺酸钠、十六烷基三甲基溴化铵、十二烷基硫酸钠、异辛基苯基聚氧乙烯醚中的一种或两种以上混合物；
S2中，主料与混合液摩尔体积比mol：ml为10-15：1，混合液与蒸馏水的体积比为2-4：1；
S3中，氢氧化钠、氨水、混合液的体积比为4-5：8-12：100；
S4中，乳液1与乳液2的体积比为1：1-1.3；
S5中，氧化钴、五氧化二钒、二氧化钛、碳酸钙和二氧化硅的重量比为3-5：1-3：0.5-1：0.3-0.5：0.3-0.5；
S5中，物料1与氧化钴的重量比为100：0.05-0.1；
S5中，烧结温度为850-930℃，烧结时间为6-8h。
2.根据权利要求1所述的绿色照明用纳米软磁铁氧体的制备方法，其特征在于，S5中，碳酸钙和二氧化硅的重量比为1：1。
3.根据权利要求1或2所述的绿色照明用纳米软磁铁氧体的制备方法，其特征在于，S5中，在850-900℃下保温烧结4-6h，然后升温900-930℃保温烧结2-3h。
4.一种绿色照明用纳米软磁铁氧体，其特征在于，由1-3任一项所述的绿色照明用纳米软磁铁氧体的制备方法制得。
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