CN112897595A - 一种水相中制备中空棒状纳米Fe3O4的方法 - Google Patents
一种水相中制备中空棒状纳米Fe3O4的方法 Download PDFInfo
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Abstract
本发明公开了一种水相中制备中空棒状纳米Fe3O4的方法，按以下过程进行：准备纳米棒状核壳结构的FeOOH@SiO2复合物，将所述FeOOH@SiO2复合物均匀分散于水合联胺的水溶液中，进行水热还原反应以除去SiO2壳层同时还原FeOOH得到Fe3O4中空纳米棒。本发明的有益效果：本发明制备Fe3O4的方法步骤简单，工艺条件相对温和，制得的Fe3O4中空纳米棒形貌均匀、结构完整性好，饱和磁化强度高达82.0emu·g‑1，高于现有技术报道的采用其他方法制备的同类产物，具有大规模、批量化生产前景。
Description
技术领域
本发明属于磁性纳米材料技术领域，具体涉及一种水相中制备中空棒状纳米Fe3O4的方法。
背景技术
Fe3O4是一种被广泛研究的功能材料，纳米Fe3O4粒子不仅具有磁性，且比表面积大、生物相容性好，因而在催化、环境污染物处理以及生物医药领域具有重要应用价值。特别是具有中空结构的Fe3O4颗粒，由于其内部具有较大空腔，在显影、载药、蛋白质检测、污染物吸附处理等领域有很大的应用价值。相比常见的球形颗粒，具有棒状结构的Fe3O4在磁场中能够产生较大的力矩以及更大的比表面积，因此更有应用前景。
制备中空结构纳米棒状Fe3O4具有相当大的难度，尤其是大范围合成尤其困难。目前最简单的方法是在还原气体下低温热处理，将棒状FeOOH直接还原为棒状Fe3O4，但是由于热处理过程中，FeOOH脱水生成Fe3O4，所以无法得到完整的Fe3O4纳米棒，而且极易团聚、破碎。Piao等(Piao Y,Kim J,HYON BIN N A,et al.Wrap-bake-peel process fornanostructural transformation from beta-FeOOH nanorods to biocompatible ironoxide nanocapsules.Nature Materials,2008.)在FeOOH上包裹十数纳米的SiO2，经还原热处理和碱溶液清洗的方法得到Fe3O4中空纳米棒，但由于还原生成的Fe3O4与SiO2结合紧密，一旦清洗SiO2将导致Fe3O4破裂，实际操作中SiO2极难清除干净，导致饱和磁化强度不高。Mohapatra等(Mohapatra J,Mitra A,Tyagi H,et al.Iron oxide nanorods as high-performance magnetic resonance imaging contrast agents.Nanoscale，2015.)使用油胺在200℃以上的高温下还原FeOOH纳米棒，同非极性有机溶媒正己烷和丙酮去除部分油胺后加入亲水性表面活性剂，例如PEI，进行亲水性的表面改性，得到棒状Fe3O4，但是亲油性的油胺一旦吸附在Fe3O4上极难去除，即便经过清洗和亲水性表面改性，仍残余大量的有机物，另外油胺的还原温度需要精细控制，一旦温度过高还原速度过快将导致Fe3O4破碎，而还原温度过低FeOOH还原程度不足导致饱和磁化强度低，实验测得的最高饱和磁化强度为60emug-1。Xu等(Xu W,Wang M,Li Z,et al.Chemical Transformation of ColloidalNanostructures with Morphological Preservation by Surface-Protection withCapping Ligands.Nano Letters,2017.)先在棒状FeOOH表面包覆PCC、PVP等软模版，再在弱还原剂二乙二醇溶液中将FeOOH还原为棒状中空Fe3O4，但是该方法只能在弱还原剂氛围下得到Fe3O4，其饱和磁化强度最高为40emu·g-1，而且制得的Fe3O4纳米棒很难从二乙二醇中分离。
所以，目前仍缺少一种简单、易操作，而且能够大批量稳定合成高饱和磁化强度的中空棒状Fe3O4的技术手段。
发明内容
有鉴于此，本发明提供一种水相中制备中空棒状纳米Fe3O4的方法。
其技术方案如下：
一种水相中制备中空棒状纳米Fe3O4的方法，其关键在于按以下过程进行，准备纳米棒状核壳结构的FeOOH@SiO2复合物，将所述FeOOH@SiO2复合物分散在水合联胺的水溶液中进行水热还原反应，除去SiO2壳层同时还原FeOOH，得到Fe3O4中空纳米棒。
在一种实施方式中，上述FeOOH@SiO2复合物与水合联胺的用量比为50mg：1-2mL。
在一种实施方式中，上述FeOOH@SiO2复合物的SiO2壳层厚度为2-5nm。
在一种实施方式中，上述还原反应温度为180-220℃。
在一种实施方式中，上述还原反应的温度为200℃。
在一种实施方式中，上述还原反应的时间为3-8h。
在一种实施方式中，上述FeOOH@SiO2复合物与水合联胺的水溶液混合后，采用超声分散10min。
在一种实施方式中，上述FeOOH@SiO2复合物的制备方法为，取干燥的FeOOH纳米棒，分散于乙醇和水的混合溶液中，随后加入氨水和正硅酸四乙酯(TEOS)，室温下搅拌反应，反应完成后清洗，高速离心得到所述FeOOH@SiO2复合物。
在一种实施方式中，上述FeOOH纳米棒与TEOS用量比为100mg:10-20μL。
附图说明
图1为实施例1、实施例5制得的FeOOH@SiO2复合物与Fe3O4中空纳米棒的XRD图谱，其中实施例1还原反应时间为8h，实施例5还原反应时间为6h；
图2为FeOOH@SiO2复合物的TEM图和EDS表征的图片；
图3为产物的SEM图片，其中(a)为实施例1的产物，(b)为对照例1的产物；
图4为实施例1的产物的TEM图片，其中：(a)低倍TEM图片；(b)高倍TEM图片；(c)高分辨图像；
图5为实施例1的产物的磁滞回线。
具体实施方式
以下结合实施例和附图对本发明作进一步说明。
一种水相中制备中空棒状纳米Fe3O4的方法，按以下过程进行：
首先准备FeOOH@SiO2复合物。原料FeOOH@SiO2复合物可以外购，也可以实验室合成。一种制备FeOOH@SiO2复合物的过程为，取100mg干燥的FeOOH纳米棒，加入15mL水，再加入150mL乙醇，随后加入10mL的27wt.％的氨水，投入10-20μL的TEOS，室温下搅拌反应4h，反应完成后，离心分离，先后用水和酒精清洗，真空干燥得到所述FeOOH@SiO2复合物，所述FeOOH@SiO2复合物的长径为300nm，SiO2层厚度约为5nm。通过调整反应物FeOOH纳米棒和TEOS的用量，可以调节壳层SiO2的厚度，本实施例中，FeOOH纳米棒与TEOS的用量比为100mg:10-20μL较为合适，得到的SiO2壳层厚度2～5nm。
接着，取纳米棒状核壳结构的FeOOH@SiO2复合物，将所述FeOOH@SiO2复合物与水合联胺(碱性)、水混合，并超声10min使之均匀分散，在180-220℃条件下还原反应3-8h以除去SiO2壳层，并还原FeOOH得到Fe3O4中空纳米棒，采用磁分离方法分离并清洗干燥。所述FeOOH@SiO2复合物与水合联胺的用量比为50mg：1-2mL。
原料FeOOH纳米棒可外购或通过氯化铁直接水解得到。一种实验室制备方法为：取0.1M三价氯化铁溶液，加热于100℃条件下反应4-12h，可以用水热反应釜也可以用回流装置，水解得到长度约300nm的棒状FeOOH，离心分离，水和酒精清洗，真空干燥。
表1列出了采用不同反应条件制备Fe3O4中空纳米棒的实施例。
表1采用不同反应条件的实施例
上述反应条件下均能成功制得中空棒状纳米Fe3O4。反应完成后，经磁吸附分离、水和乙醇清洗，干燥得到样品。以实施例1和5为例，对得到的FeOOH@SiO2复合物以及Fe3O4中空纳米棒，采用X射线衍射分析(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)进行结构和形貌表征，采用能谱分析仪(EDS)对元素分布进行表征，采用振动样品磁强计(VSM)检测其磁性能。
为研究SiO2对产物形貌的影响，对照例1以未包覆SiO2的FeOOH为原料进行还原反应，其余反应条件与实施例1相同。反应过程为：取50mg干燥的FeOOH纳米棒，与水合联胺、水混合，并超声10min使之均匀分散，在200℃条件下还原反应8h，分离得到产物。
如图1，对比FeOOH@SiO2复合物以及实施例1和5的产物的XRD图谱，可知还原反应后得到了纯相的Fe3O4。
图2是FeOOH@SiO2复合物的TEM图和EDS表征的图片。图中可以看到，厚度约5nm的SiO2均匀包覆在FeOOH外层。
图3(a)为实施例1的产物的大尺度SEM图片，可以看到产物为形貌均匀的棒状Fe3O4。图3(b)是对照例1的反应制备得到的产物SEM图片，该产物由未包覆SiO2的棒状FeOOH直接在水合肼溶液中还原得到，该产物为多边形Fe3O4颗粒。
采用TEM对实施例1的产物进行表征，结果如图4(a、b)，比较纳米棒不同部位的衬度可知，得到的纳米棒存在孔洞，内部有中空结构。如图4(c)，高分辨图像观察到其晶面间距0.297nm，与Fe3O4的(104)晶面间距一致，进一步证实其为Fe3O4。分析上述现象出现的原因在于，该反应利用水合肼溶液的碱性和还原性，在去除SiO2纳米包覆层的同时实现FeOOH向Fe3O4的转换，同时在FeOOH脱水后生成的Fe3O4将在棒状物表面再结晶，从而生成中空结构。
如图5，实施例1的产物磁滞回线显示，其具有优异的磁性能，饱和磁化强度为Ms＝82.0emu·g-1，矫顽力为Hc＝129.5Oe。
与现有技术相比，本发明的有益效果：本发明制备Fe3O4的方法步骤简单，工艺条件相对温和，制备过程中未加入难去除的亲油性或难分离的高密度有机还原剂和分散剂，无需对SiO2进行二次清洗，制得的Fe3O4中空纳米棒形貌均匀、结构完整性好，饱和磁化强度高达82.0emu·g-1，高于现有技术报道的采用其他方法制备的同类产物，具有大规模、批量化生产前景。
最后需要说明的是，上述描述仅仅为本发明的优选实施例，本领域的普通技术人员在本发明的启示下，在不违背本发明宗旨及权利要求的前提下，可以做出多种类似的表示，这样的变换均落入本发明的保护范围之内。
Claims (9)
1.一种水相中制备中空棒状纳米Fe3O4的方法，其特征在于按以下过程进行：准备纳米棒状核壳结构的FeOOH@SiO2复合物，将所述FeOOH@SiO2复合物分散在水合联胺的水溶液中进行水热还原反应，除去SiO2壳层同时还原FeOOH，得到Fe3O4中空纳米棒。
2.根据权利要求1所述的一种水相中制备中空棒状纳米Fe3O4的方法，其特征在于：所述FeOOH@SiO2复合物与水合联胺的用量比为50mg：1-2mL。
3.根据权利要求1所述的一种水相中制备中空棒状纳米Fe3O4的方法，其特征在于：所述FeOOH@SiO2复合物的SiO2壳层厚度为2-5nm。
4.根据权利要求1所述的一种水相中制备中空棒状纳米Fe3O4的方法，其特征在于：所述还原反应温度为180-220℃。
5.根据权利要求4所述的一种水相中制备中空棒状纳米Fe3O4的方法，其特征在于：所述还原反应的温度为200℃。
6.根据权利要求1所述的一种水相中制备中空棒状纳米Fe3O4的方法，其特征在于：所述还原反应的时间为3-8h。
7.根据权利要求1所述的一种水相中制备中空棒状纳米Fe3O4的方法，其特征在于：所述FeOOH@SiO2复合物与水合联胺的水溶液混合后，采用超声分散10min。
8.根据权利要求1所述的一种水相中制备中空棒状纳米Fe3O4的方法，其特征在于：所述FeOOH@SiO2复合物的制备方法为，取干燥的FeOOH纳米棒，分散于乙醇和水的混合溶液中，随后加入氨水和正硅酸四乙酯(TEOS)，室温下搅拌反应，反应完成后清洗，高速离心得到所述FeOOH@SiO2复合物。
9.根据权利要求8所述的一种水相中制备中空棒状纳米Fe3O4的方法，其特征在于：所述FeOOH纳米棒与TEOS的用量比为100mg:10-20μL。
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