CN112079394B - 一种花状纳米磁性Fe3O4材料的制备方法和应用 - Google Patents
一种花状纳米磁性Fe3O4材料的制备方法和应用 Download PDFInfo
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Abstract
本发明公开了一种花状纳米磁性Fe3O4材料的制备方法和应用，所述花状纳米磁性Fe3O4材料的原料以重量份计，包括三价铁盐30份，乙二醇100～500份，聚乙烯吡络烷酮1～30份。本发明利用微波辐射加热法，在特定条件下制得了有规则花状形貌的的Fe3O4材料，其具有很高的电磁屏蔽效能和电磁波吸收能力。本发明的整个反应体系简单可控，工艺重复性高，产物的产率高，工艺过程操作简便，能耗较低，设备便宜，可以大规模生产，推进纳米磁性Fe3O4材料在催化材料、杀菌材料、生物材料、光学材料、信息材料等领域的应用。
Description
技术领域
本发明涉及磁性纳米材料技术领域，更具体地，涉及一种花状纳米磁性Fe3O4材料的制备方法和应用。
背景技术
Fe3O4是一种非常重要的磁性材料，其结构为立方相反尖晶石结构。在Fe3O4晶体中，Fe阳离分别处于氧四而体间隙位置(A位)和氧八而体的间隙位置((B位)。由于A位间隙比B位小，A位全是半径较小的Fe3+，而B位由Fe3+和另一些Fe3+占据。位于B位的Fe2+和Fe3+之间的电子传递使得Fe3O4具有独特的电学和磁学性能，因而被广泛用作磁流体、磁记录材料等。
纳米尺度的Fe3O4具有与生物组织的相容性以及与尺寸和形貌有关的电学和磁学性能，在磁性墨水、电子与生物敏感材料、高密度磁记录介质和生物医药等领域具有广泛的应用。
Fe3O4纳米微粒具有单磁畴结构并且矫顽力很高，用做磁记录材料可以提高信噪比，改善图象质量，且廉价易得，可降低生产成木；同时Fe3O4纳米粒子还具有较高的饱和磁化强度，故常被用来制备磁流体，既有固体的强磁性又有液体的流变性，并且流动性和分布可由外加磁场实施定向和定位控制，因此在航空技术、快速印刷等领域得到广泛应用。
近年来制备纳米Fe3O4中包括沉淀法(共沉淀法、氧化沉淀法、还原沉淀法、交流电沉淀法和络合物分解法)、水热法、水解法、微乳液法、固相法、球磨法、超声波法、热解法、水溶液吸附分散法等，这些方法制备的绝大多数为圆颗粒状或者棒状的纳米Fe3O4，容易团聚，比表面积小，表面光滑的形貌结构限制对电磁波的吸收能力，影响了纳米Fe3O4的电磁屏蔽效应。并且，这些方法普遍存在着一些问题，比如操作复杂，反应分多步进行，且很难可控合；制备工艺重复性差，产率低等等，影响纳米Fe3O4在磁性墨水、电子与生物敏感材料、高密度磁记录介质和生物医药等领域的广泛应用。
发明内容
本发明要解决的技术问题是针对现有技术制备的圆形颗粒纳米Fe3O4易团聚，比表面积小以及形貌结构导致的对电磁波吸收能力有限，以及的操作复杂、重复性差、不宜大规模生产不足，提供一种花状纳米磁性Fe3O4材料的制备方法。
本发明的目的通过以下技术方案予以实现：
一种花状纳米磁性Fe3O4材料的制备方法，制备步骤包括：
S1.将三价铁盐和聚乙烯吡络烷酮与部分乙二醇配置成一定浓度的溶液；
S2.将另一部分的乙二醇溶液在搅拌条件下利用微波加热至120～160℃；
S3.将S1配置的溶液加入S2中加热的乙二醇溶液中，保持温度并以恒定的速率搅拌，反应后得到黑色固体；
S4.将S3所得的黑色固体清洗干净，干燥得到花状纳米磁性Fe3O4材料。
进一步地，所述花状纳米磁性Fe3O4材料的原料以重量份计，包括三价铁盐30份，乙二醇100～500份，聚乙烯吡络烷酮1～30份。
本发明以三价铁盐为原料，乙二醇作为溶剂和还原剂，聚乙烯吡络烷酮(PVP)作为分散剂快速制取花状结构的纳米Fe3O4材料。其中，乙二醇溶剂可以将三价铁盐还原为Fe3O4，同时，乙二醇会发生部分聚合，生成聚乙二醇会逐渐增大反应体系的粘稠度，并限制Fe3O4微粒的生长，对于生成纳米级别的Fe3O4有利。
进一步地，所述三价铁盐包括氯化铁、硫酸铁、硝酸铁的一种或多种。
进一步地，所述聚乙烯吡络烷酮的平均分子量为8000～40000。
进一步地，步骤S1所述溶液的浓度为15～25mg/mL。
进一步地，步骤S2所述微波加热的功率为400～800W。普通的加热方式，像油浴加热，烘箱加热等方法都是通过介质的导热要实现温度的上升和保持。这些方式加热时间比较长，加热是从外到里依次传导，所以对于整个体系来说，加热是不均匀的，也不够高效。而微波加热的方式是直接作用于溶剂分子，加热迅速且均匀，可以在很短的时间内实现反应，极大地加速了反应进程，并能够通过微波对其形貌进行控制调节。
进一步地，所述搅拌的速率为900～1200r/min。
进一步地，步骤S3所述反应时间为10～20min。
进一步地，步骤S4所述黑色固体清洗所用试剂为有机试剂；所述有机试剂包括无水乙醇、丙酮、丙二醇的一种或多种。
进一步地，步骤S4所述干燥的温度为60～70℃，时间为12～18h。
根据上述制备得到花状纳米磁性Fe3O4材料在催化材料、杀菌材料、生物材料、光学材料、信息材料的领域中的应用。
与现有技术相比，有益效果是：
本发明以三价铁盐为原料，乙二醇作为溶剂和还原剂，聚乙烯吡络烷酮(PVP)作为分散剂，通过微波辐射方法快速制取了花状结构的纳米Fe3O4材料。本发明制备的花状结构的纳米磁性Fe3O4材料，呈现出有序的花状结构外观，其具有极大地电磁波吸收能力，所得的花状结构的纳米磁性Fe3O4材料的电磁波吸收值是商用150目Fe3O4磁粉的3倍以上。
本发明所述制备方法极大地缩短了反应时间，由原来传统加热方式所需要的数十小时，缩短到了现在的10～20min。同时，本发明的整个反应体系简单可控，工艺重复性高，产物的产率高，工艺过程操作简便，能耗较低，设备便宜，可以大规模生产，推进纳米磁性Fe3O4材料在催化材料、杀菌材料、生物材料、光学材料、信息材料等领域的应用。
附图说明
图1是本发明制备的纳米磁性Fe3O4电镜扫描图；
图2是本发明制备的纳米磁性Fe3O4电镜扫描图；
图3是本发明制备的纳米磁性Fe3O4电镜扫描图；
图4是本发明制备的纳米磁性Fe3O4电镜扫描图；
图5是本发明制备的纳米磁性Fe3O4电镜扫描图；
图6是本发明制备的纳米磁性Fe3O4电镜扫描图；
图7是本发明制备的纳米磁性Fe3O4电镜扫描图；
图8是本发明制备的纳米磁性Fe3O4电镜扫描图；
图9是本发明制备的纳米磁性Fe3O4与商用商用150目磁粉电磁波吸收对比图。
具体实施方式
下面结合实施例进一步解释和阐明，但具体实施例并不对本发明有任何形式的限定。若未特别指明，实施例中所用的方法和设备为本领常规方法和设备，所用原料均为常规市售原料。
实施例1
本实施例提供一种纳米磁性Fe3O4材料的制备方法，步骤包括：
S1.将三价铁盐和聚乙烯吡络烷酮与部分乙二醇配置成15～25mg/mL的溶液；
S2.将另一部分的乙二醇溶液使用400～800W的微波加热至120～160℃，不断以900～1200r/min的速度进行搅拌；
S3.将S1配置的溶液倒入S2中搅拌加热的乙二醇溶液中，保持120～160℃温度并以恒定的速率搅拌，反应10～20min离心过滤得到黑色固体；
S4.将S3所得的黑色固体用无水乙醇、丙酮、丙二醇洗涤干净，在60～70℃干燥12～18h得到花状纳米磁性Fe3O4材料。
所述三价铁盐包括氯化铁、硫酸铁、硝酸铁的一种或多种。
所述聚乙烯吡络烷酮(PVP)的平均分子量为8000～40000。
所述乙二醇的纯度为分析纯级别。
实施例2～16
本实施例根据实施例1所述方法，按照表1所示原料及参数制备纳米磁性Fe3O4材料。
表1
实验例
1.电镜扫描
将实施例制备的纳米磁性Fe3O4材料进行电镜扫描，如图1～8，本发明制备的纳米磁性Fe3O4材料呈现出有序的花状结构的形貌，可以清晰的看到其花瓣的厚度在20nm以下。
2.电磁波吸收试验
将实施例9制备的花状纳米磁性Fe3O4材料与市面购买的商用150目磁粉进行电磁波吸收试验，如图9所示，本发明制备的花状纳米Fe3O4材料对于电磁波具有极强的吸收作用，具有很高的电磁屏蔽效能和电磁波吸收能力。
显然，本发明的上述实施例仅仅是为清楚地说明本发明所作的举例，而并非是对本发明的实施方式的限定。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明权利要求的保护范围之内。
Claims (4)
1.一种花状纳米磁性Fe3O4材料的制备方法，其特征在于，所述花状纳米磁性 Fe3O4材料的原料以重量份计，包括三价铁盐 30 份，乙二醇100~500 份，聚乙烯吡咯烷酮1~30 份，所述聚乙烯吡咯烷酮的平均分子量为8000~40000；所制备的纳米磁性Fe3O4材料呈现有序的花状结构的形貌，其花瓣的厚度在20nm以下；
制备步骤包括：
S1.将三价铁盐和聚乙烯吡咯烷酮与部分乙二醇配制成浓度为15~25 mg/mL 的溶液；
S2.将另一部分的乙二醇溶液在900~1200r/min搅拌速率下利用功率为 400~800W的微波加热至120~160℃；
S3.将S1配制的溶液加入S2中加热的乙二醇溶液中，保持温度并以恒定的速率搅拌，反应10~20min后得到黑色固体；
S4.将S3所得的黑色固体清洗干净，干燥得到花状纳米磁性Fe3O4材料。
2.根据权利要求1所述花状纳米磁性Fe3O4材料的制备方法，其特征在于，所述三价铁盐包括氯化铁、硫酸铁、硝酸铁的一种或多种。
3.根据权利要求1所述花状纳米磁性Fe3O4材料的制备方法，其特征在于，步骤S4所述黑色固体清洗所用试剂为有机试剂；所述有机试剂包括无水乙醇、丙酮、丙二醇的一种或多种。
4.根据权利要求1所述花状纳米磁性Fe3O4材料的制备方法，其特征在于，步骤S4所述干燥的温度为60~70℃，时间为12~18h。
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