CN108383514A - 一种纳米锰锌铁氧体粉末的制备方法 - Google Patents
一种纳米锰锌铁氧体粉末的制备方法 Download PDFInfo
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Abstract
本发明公开一种纳米锰锌铁氧体粉末的制备方法，属于磁性纳米软磁材料的制备技术领域。本发明所述方法为称取一定比例的六水合氯化铁、六水合硝酸锌和一水硫酸锰溶于乙二醇中；并依次加入适量的聚乙二醇和乙酸铵；在磁力搅拌机上以搅拌30分钟后成棕褐色溶液；放入微波消解罐中在微波下进行反应，经离心洗涤,超声振散,最后真空干燥得到纳米锰锌铁氧体粉末；所得产物为尖晶石结构，结晶度良好。本发明工艺流程简单，制备的锰锌铁氧体纳米颗粒团聚少，晶粒度小且可控，对环境友好。
Description
技术领域
本发明公开一种纳米锰锌铁氧体粉末的制备方法，属于磁性纳米软磁材料的制备技术领域。
背景技术
铁氧体为尖晶石结构的磁性氧化物，离子分布式可写为,同金属软磁一并组成软磁材料，其中锰锌铁氧体在铁氧体的产量中占据60%以上，其具备高磁导率、低矫顽力、高频低损等特点，另外制备出的纳米粉体由于其微观效应如：表面效应、小尺寸效应和宏观量子隧道效应等，使其具备更独特的磁学性能，如超顺磁。纳米锰锌铁氧体可用于高密度磁记录、吸波材料、磁感应热疗、药物靶向载体、传感器等方面，应用十分广泛。
锰锌铁氧体的制备方法众多，一般分为干法（氧化物法）和湿法制备。目前为止，干法制备锰锌铁氧体适宜大规模生产是最常用的制备方法，但在制备过程中易引入杂质以及高温离子扩散的不均匀引起成分偏析是其存在的最大问题。相比干法，湿法制备适宜实验室小规模制备，原料为各类金属盐，产物的纯度相比干法更高。常用的湿法制备方法有：化学共沉淀法、溶胶凝胶法、水热法以及喷雾焙烧法等。这些方法制备可较快的制备出锰锌铁氧体粉末，其颗粒可到达纳米级，可被直接使用。由于纳米粉体为减少表面能而发生大量团聚现象，在制备过程中往往会加入表面活性剂包覆粉体表面产生的空间位阻和提高zate电位来降低团聚状况。
不同的制备方法即有其优点也有其缺陷，如化学共沉淀法虽操作简单，但颗粒易团聚，重现性较差，一般需要高温煅烧；溶胶凝胶法在制备过程中易产生非晶体凝胶对后续煅烧生成的粉体成分造成影响；喷雾焙烧法工艺简单但一些金属盐类分解将释放有毒气体不易于生产；水热法中PH对反应结果影响较大，制备时间较长。
发明内容
本发明的目的在于提供一种纳米锰锌铁氧体粉末的制备方法，具体包括以下步骤：
（1）将六水合氯化铁、六水合硝酸锌、一水硫酸锰加入乙二醇中，磁力搅拌至完全溶解得到棕褐色混合溶液，六水合氯化铁、六水合硝酸锌、一水硫酸锰的摩尔比为4：x：2-x，其中（x>0），乙二醇与六水合氯化铁的摩尔比为1:0.003~0.009；
（2）边搅拌边在步骤（1）得到的混合溶液中依次加入聚乙二醇、乙酸铵，然后在室温下搅拌40min；其中，六水合氯化铁与乙酸铵摩尔比例为1:30～40，聚乙二醇的加入量为24~48g/L；
（3）步骤（2）得到的混合溶液通过以聚四氟乙烯材质的微波消解罐进行密封，然后放入实验微波炉中在180℃～200℃加热1～2小时；
（4）反应结束后待反应液自然冷却后，通过离心机以无水乙醇和丙酮离心洗涤4~5次，每次洗涤之后经过一次超声振散后再进行下一次洗涤，将所得沉淀在真空下干燥得到纳米锰锌铁氧体粉末。
优选的，本发明步骤（1）中磁力搅拌转速为500～800r/min。
优选的，本发明步骤（3）中微波炉内加热过程中进行搅拌，搅拌速度为100～180r/min。
优选的，本发明步骤（4）中离心机转速为5000r/min，每次洗涤时间10min。真空干燥温度为60℃，干燥时间为6h。
本发明的原理：通过微波使极性分子快速升温提供反应环境，以溶解-结晶机制，形核后通过小粒径向大粒径晶粒的物料运输和小晶粒聚集进行配向生长进行晶粒的长大。
本发明的有益效果：
本发明采用溶剂热法，以微波作为热源，和现有技术相比，本发明无需高温煅烧或高温环境，工艺简单，易于控制，重现性好，可快速生成纳米锰锌铁氧体。
本发明所述方法操作方便，反应温度较低，通过微波辅助加快反应进度，缩短反应时间，节约能源；制备出的反应物纯度高，具晶粒度小，少团聚且粒径可控，结晶度高；无需沉淀剂或凝胶剂的调试加快进程，反应内压相比较低，对反应釜抗压要求下降。
附图说明
图1为微波辅助溶剂热示意图；
图2为实施例3制备的纳米锰锌铁氧体XRD衍射图。
具体实施方式
下面结合具体实施例对本发明做进一步详细说明，但本发明的保护范围并不限于所述内容。
实施例1
（1）取3mmol六水合氯化铁、0.75mmol六水合硝酸锌、0.75mmol一水硫酸锰加入50mL的乙二醇中，磁力搅拌（500r/min）直至混合液变为棕褐色且完全溶解得到混合溶液；
（2）边搅拌边在步骤（1）得到的混合溶液中依次加入1.2g入聚乙二醇（PEG-6000）、0.18mol乙酸铵，然后在室温下搅拌40min；
（3）步骤（2）得到的混合溶液通过聚四氟乙烯材质的微波消解罐进行密封，然后放入实验室微波炉中在180℃加热1小时，加热过程中进行搅拌，搅拌速度为100r/min。
（4）反应结束后待反应液自然冷却后，通过离心机以无水乙醇和丙酮离心洗涤4次（离心机转速为5000r/min，每次洗涤时间10min），每洗涤完一次后经过超声振散后再进行下一次洗涤，将所得沉淀在真空下干燥（干燥温度为60℃，干燥时间为6h）得到纳米锰锌铁氧体粉末。
本实施例制备得到的纳米锰锌铁氧体粉末,相比现有技术制备速度更快，可直接制备出纳米锰锌铁氧体但结晶度较低。
实施例2
（1）取8mmol六水合氯化铁、2.0mmol六水合硝酸锌、2.0mmol一水硫酸锰加入50mL的乙二醇中，磁力搅拌（800r/min）直至混合液变为棕褐色且完全溶解得到混合溶液；
（2）边搅拌边在步骤（1）得到的混合溶液中依次加入2.4g聚乙二醇（PEG-6000）、0.24mol乙酸铵，然后在室温下搅拌40min；
（3）步骤（2）得到的混合溶液通过聚四氟乙烯材质的微波消解罐进行密封，然后放入实验室微波炉中在200℃加热2小时，加热过程中进行搅拌，搅拌速度为150r/min。
（4）反应结束后待反应液自然冷却后，通过离心机以无水乙醇和丙酮离心洗涤4次（离心机转速为5000r/min，每次洗涤时间10min），每洗涤完一次后经过超声振散后再进行下一次洗涤，将所得沉淀在真空下干燥（干燥温度为60℃，干燥时间为6h）得到纳米锰锌铁氧体粉末。
本实施例制备得到的纳米锰锌铁氧体粉末，相比现有技术制备速度较快。
实施例3
（1）取6mmol六水合氯化铁、1.5mmol六水合硝酸锌、1.5mmol一水硫酸锰加入50mL的乙二醇中，磁力搅拌（700r/min）直至混合液变为棕褐色且完全溶解得到混合溶液；
（2）边搅拌边在步骤（1）得到的混合溶液中依次加入1.8g聚乙二醇（PEG-6000）、0.21mol乙酸铵，然后在室温下搅拌40min；
（3）步骤（2）得到的混合溶液通过聚四氟乙烯材质的微波消解罐进行密封，然后放入实验室微波炉中在190℃加热1.5小时，加热过程中进行搅拌，搅拌速度为180r/min。
（4）反应结束后待反应液自然冷却后，通过离心机以无水乙醇和丙酮离心洗涤4次（离心机转速为5000r/min，每次洗涤时间10min），每洗涤完一次后经过超声振散后再进行下一次洗涤，将所得沉淀在真空下干燥（干燥温度为60℃，干燥时间为6h）得到纳米锰锌铁氧体粉末。
本实施例制备得到的纳米锰锌铁氧体粉末，相比现有技术制备速度快，通过XRD衍射图分析，样品为尖晶石结构，无杂相，结晶度高，晶粒在10nm左右。
Claims (4)
1.一种纳米锰锌铁氧体粉末的制备方法，其特征在于，具体包括以下步骤：
（1）将六水合氯化铁、六水合硝酸锌、一水硫酸锰加入乙二醇中，磁力搅拌至完全溶解得到棕褐色混合溶液，六水合氯化铁、六水合硝酸锌、一水硫酸锰的摩尔比为4：x：2-x，其中（x>0），乙二醇与六水合氯化铁的摩尔比为1:0.003~0.009；
（2）边搅拌边在步骤（1）得到的混合溶液中依次加入聚乙二醇、乙酸铵，然后在室温下搅拌40min；其中，六水合氯化铁与乙酸铵摩尔比例为1:30～40，聚乙二醇的加入量为24~48g/L；
（3）步骤（2）得到的混合溶液通过以聚四氟乙烯材质的微波消解罐进行密封，然后放入实验微波炉中在180℃～200℃下加热1～2小时；
（4）反应结束后待反应液自然冷却后，通过离心机以无水乙醇和丙酮离心洗涤4~5次，每次洗涤之后经过一次超声振散后再进行下一次洗涤，将所得沉淀在真空下干燥得到纳米锰锌铁氧体粉末。
2.根据权利要求1所述纳米锰锌铁氧体粉末的制备方法，其特征在于：步骤（1）中磁力搅拌转速为500～800r/min。
3.根据权利要求1所述纳米锰锌铁氧体粉末的制备方法，其特征在于：步骤（3）中微波炉内加热过程中进行搅拌，搅拌速度为100～180r/min。
4.根据权利要求1所述纳米锰锌铁氧体粉末的制备方法，其特征在于：步骤（4）中离心机转速为5000r/min，每次洗涤时间10min；真空干燥温度为60℃，干燥时间为6h。
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