A new method for the identification and quantification of magnetite-maghemite mixture using conventional X-ray diffraction technique

A new method for the identification and quantification of magnetite-maghemite mixture using conventional X-ray diffraction technique
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DOI:
10.1016/j.talanta.2012.03.001
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发表时间:
2012-05-30
期刊:
影响因子:
6.1
通讯作者:
Shon, In-Jin
Shon, In-Jin
中科院分区:
化学1区
文献类型:
--
作者:
Kim, Wonbaek;Suh, Chang-Yul;Shon, In-Jin

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铁丝在空气中的电爆炸产生了纳米颗粒,其中含有磁铁矿(Fe3O4)和磁铁矿(Gamma-Fe2O3)的二元混合物。用传统的X射线衍射法对磁铁矿和磁铁矿进行物相鉴定并不是一件简单的事情,因为它们都具有相同的立方结构,并且它们的晶格参数几乎相同。在这里,我们提出了一种简便的方法来评估磁铁矿-磁铁矿混合物的存在,并使用传统的峰值去卷积技术进一步量化其物相组成。在高角度峰(5 1 1)和(4 4 0)周围仔细逐级扫描,发现了指示混合相的清晰的双峰。用市售纯磁铁矿和磁铁矿粉末构建校正曲线,对混合物相进行了定量分析。相关系数。磁铁矿-磁铁矿混合物的R-2为0.9941。根据该方法计算得到的线爆法制备的氧化铁纳米颗粒中含有55.8wt.%的磁铁矿和44.2wt.%的磁铁矿。我们相信,所提出的方法将是研究磁铁矿-磁铁矿混合物的一个方便的工具,否则需要非常复杂的设备和技术。(C)2012爱思唯尔B.V.保留所有权利。
The electrical explosion of Fe wire in air produced nanoparticles containing the binary mixture of magnetite (Fe3O4) and maghemite (gamma-Fe2O3). The phase identification of magnetite and maghemite by the conventional X-ray diffraction method is not a simple matter because both have the same cubic structure and their lattice parameters are almost identical. Here, we propose a convenient method to assess the presence of magnetite-maghemite mixture and to further quantify its phase composition using the conventional peak deconvolution technique. A careful step scan around the high-angle peaks as (5 1 1) and (4 4 0) revealed the clear doublets indicative of the mixture phases. The quantitative analysis of the mixture phase was carried out by constructing a calibration curve using the pure magnetite and maghemite powders commercially available. The correlation coefficients. R-2, for magnetite-maghemite mixture was 0.9941. According to the method, the iron oxide nanoparticles prepared by the wire explosion in this study was calculated to contain 55.8 wt.% maghemite and 44.2 wt.% magnetite. We believe that the proposed method would be a convenient tool for the study of the magnetite-maghemite mixture which otherwise requires highly sophisticated equipments and techniques. (C) 2012 Elsevier B.V. All rights reserved.