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X-rays absorption spectroscopy for local structure determination of magnetolpumbite nanoparticles
Journal of Alloys and Compounds ( IF 5.8 ) Pub Date : 2021-03-01 , DOI: 10.1016/j.jallcom.2021.159350
Sana Mehmood , M.F. Natiq , M. Anis-ur-Rehman

Magnetolpumbite nanoparticles of Cr-doped strontium hexaferrites (SrFe12−xCrxO19 x = 0.0–1.0) were synthesized by using sol-gel method. X-ray diffraction (XRD) pattern of the prepared samples showed hexagonal structure, however in some composition hematite phase α-Fe2O3 was also observed. The average crystallite size was found to be in the range of 31–42 nm. By using Williamson-Hall (W-H) Analysis the compressive strains were observed. The lattice parameters showed non-linear dependence on Cr doping. Fourier Transform Infrared Spectroscopy (FTIR) confirmed the appearance of different Octahedral and Tetrahedral stretching vibrations. Further to understand it deeply, the X-Ray Absorption Fine Spectroscopy (XAFS) analysis has been done. The Structural investigations of Cr doped complex SrFe12−xCrxO19 (x = 0.2, 0.4, 0.6, 0.8, 1.0) and pure SrFe12O19 as model have been studied accurately to conclude the oxidation states, chemical shift and site occupancy for Fe and Cr at K absorption edges. The model SrFe12O19 and sample compositions x = 0.2 showed a single Fe3+ oxidation state for Fe K absorption edge however, for all the rest of the sample compositions x ≥ 0.4, Fe2+ and Fe3+ phases were also observed. Chemical shift for Fe absorption edge have also been determined to quantify the shift in the energies. Positive shift has been observed in all the samples as reference from Fe metal. For Cr K absorption edge, oxidation state is also determined. EXAFS data proved helpful in estimating the bond lengths of RFe-O and RCr-O through calculating distance by first shell, both for Fe and Cr K edges. The atomic distortion in the structure is caused by the Cr doping in SrFe12−xCrxO19 system, in a non-regular way. Finally, the XAFS Analysis revealed the presence of hematite which was not figure out by XRD spectrum.



中文翻译:

X射线吸收光谱法测定磁珠辉石纳米颗粒的局部结构

采用溶胶-凝胶法合成了掺Cr锶铁氧体(SrFe 12-x Cr x O 19 x = 0.0-1.0)的磁珠辉石纳米颗粒。所制备的样品的X射线衍射(XRD)图显示六方晶结构,然而,在一些组合物中赤铁矿相的α-Fe 2 ö 3也被观察到。发现平均晶粒尺寸在31-42 nm范围内。通过使用Williamson-Hall(WH)分析,观察到了压缩应变。晶格参数显示出对Cr掺杂的非线性依赖性。傅立叶变换红外光谱(FTIR)证实了八面体和四面体拉伸振动的出现。为了进一步理解它,已经完成了X射线吸收精细光谱(XAFS)分析。Cr掺杂的SrFe 12-x Cr x O 19(x = 0.2、0.4、0.6、0.8、1.0)和纯SrFe 12 O 19的结构研究作为模型,已经进行了精确的研究,以得出Fe和Cr在K吸收边缘的氧化态,化学位移和位点占有率。SrFe 12 O 19模型和样品组成x = 0.2对Fe K吸收边缘显示单一的Fe 3+氧化态,但是,对于所有其余样品组成x≥0.4,也观察到Fe 2+和Fe 3+相。还已经确定了铁吸收边缘的化学位移,以量化能量的位移。在所有样品中均观察到正位移,作为铁金属的参考。对于Cr K吸收边缘,还确定了氧化态。事实证明,EXAFS数据有助于估算R Fe-O和R的键长通过计算第一壳的距离(对于Fe和Cr K边缘),得出Cr-O。结构中的原子变形是由SrFe 12-x Cr x O 19系统中的Cr掺杂以非规则方式引起的。最后,XAFS分析揭示了赤铁矿的存在,而XRD光谱无法确定赤铁矿的存在。

更新日期:2021-03-07
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