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一种利用常规 X 射线衍射技术鉴定和定量磁铁矿-磁赤铁矿混合物的新方法。

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

机构信息

Korea Institute of Geoscience & Mineral Resources (KIGAM), Gwahang-no 124, Yuseong-gu, Daejeon, 305- 350, Republic of Korea.

出版信息

Talanta. 2012 May 30;94:348-52. doi: 10.1016/j.talanta.2012.03.001. Epub 2012 Mar 7.

DOI:10.1016/j.talanta.2012.03.001
PMID:22608459
Abstract

The electrical explosion of Fe wire in air produced nanoparticles containing the binary mixture of magnetite (Fe(3)O(4)) and maghemite (γ-Fe(2)O(3)). 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 (511) and (440) 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.

摘要

铁丝在空气中的电爆炸产生了含有磁铁矿(Fe3O4)和磁赤铁矿(γ-Fe2O3)的二元混合物的纳米颗粒。由于两者都具有相同的立方结构且其晶格参数几乎相同,因此通过常规 X 射线衍射法对磁铁矿和磁赤铁矿进行相鉴定并非易事。在这里,我们提出了一种使用常规峰分解技术评估磁铁矿-磁赤铁矿混合物存在并进一步定量其相组成的简便方法。在(511)和(440)等高位峰附近仔细进行分步扫描,揭示了混合相的明显双峰。通过使用市售的纯磁铁矿和磁赤铁矿粉末构建校准曲线对混合相进行定量分析。磁铁矿-磁赤铁矿混合物的相关系数 R2 为 0.9941。根据该方法,计算出本研究中通过电线爆炸制备的氧化铁纳米颗粒含有 55.8wt.%的磁赤铁矿和 44.2wt.%的磁铁矿。我们相信,对于磁铁矿-磁赤铁矿混合物的研究而言,该方法将是一种便捷的工具,因为这种混合物的研究需要高度复杂的设备和技术。

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