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Phase identification in binary mixture of nanopowders from deconvoluted valence band spectra using X-ray photoelectron spectroscopy: Case study with iron oxide and titania polymorphs

机译:利用去射线化的价带光谱,利用X射线光电子能谱鉴定纳米粉末的二元混合物中的相:以氧化铁和二氧化钛多晶型为例

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摘要

We propose a new method of quantifying the phases present in a binary mixture of nanopowder from decon-voluted valence band spectra using X-ray photoelectron spectroscopy (XPS). Polymorphs of iron oxide (gamma-Fe2O3 and alpha-Fe2O3) and titania (anatase and rutile TiO2) nanopowders containing different weight percentages of the polymorphs were chosen for the present study. Pure iron oxide nanopowder (Fe3O4) was prepared by co-precipitation and was air annealed at 250 and 700 degrees C to obtain gamma-Fe2O3 and alpha-Fe2O3 phases, respectively. In addition, anatase and rutile TiO2 were also used in the present study. A linear correlation between the percentage of the phase and the valance band peak area was observed in both the cases. The phase compositions of the nanopowder mixtures identified from the valence band spectra were compared with that of the X-ray Diffraction (XRD) data and the results were found to be in good agreement with each other. For nanoparticles of size 30 nm, no size dependent effect was observed in determining the phase composition but for particle size below 10 nm, size was found to have a detrimental role. These results showed that the phases of polymorphs can be quantified from XPS valence band analysis.
机译:我们提出了一种新的方法,该方法使用X射线光电子能谱(XPS)从解卷积的价带光谱中量化纳米粉体的二元混合物中存在的相。氧化铁(γ-Fe2O3和α-Fe2O3)和二氧化钛(锐钛矿和金红石TiO2)纳米粉的多晶型物含有不同重量百分比的多晶型物,用于本研究。通过共沉淀制备纯氧化铁纳米粉末(Fe3O4),并在250和700摄氏度下进行空气退火,分别获得γ-Fe2O3和α-Fe2O3相。另外,本研究中还使用了锐钛矿和金红石型TiO2。在两种情况下均观察到相的百分比与价带峰面积之间的线性相关性。从价带光谱中鉴定出的纳米粉末混合物的相组成与X射线衍射(XRD)数据的相组成进行了比较,发现结果彼此吻合良好。对于尺寸大于30nm的纳米颗粒,在确定相组成中没有观察到尺寸依赖性的作用,但是对于小于10nm的粒径,发现尺寸具有有害作用。这些结果表明,可以从XPS价带分析中量化多晶型物的相。

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