Photoacoustic Spectroscopy of Titanium Dioxide, Niobium Pentoxide, Titanium:Niobium, and Ruthenium-Modified Oxides Synthesized Using Sol-Gel Methodology.

IF 2.2 3区 化学 Q2 INSTRUMENTS & INSTRUMENTATION Applied Spectroscopy Pub Date : 2024-10-01 Epub Date: 2024-08-11 DOI:10.1177/00037028241268158
Daniele T Dias, Andressa O Rodrigues, Pietra B Pires, Betina C Semianko, Maria E K Fuziki, Giane G Lenzi, Simone R F Sabino
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Abstract

The aim of this work was the development and morphological/chemical, spectroscopic, and structural characterization of titanium dioxide, niobium pentoxide, and titanium:niobium (Ti:Nb) oxides, as well as materials modified with ruthenium (Ru) with the purpose of providing improvement in photoactivation capacity with visible sunlight radiation. The new materials synthesized using the sol-gel methodology were characterized using the following techniques: scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), photoacoustic spectroscopy (PAS), and X-ray diffraction (XRD). The SEM-EDS analyses showed the high purity of the bases, and the modified samples showed the adsorption of ruthenium on the surface with the crystals' formation and visible agglomerates for higher calcination temperature. The nondestructive characterization of PAS in the ultraviolet visible region suggested that increasing calcination temperature promoted changes in chemical structures and an apparent decrease in gap energy. The separation of superimposed absorption bands referring to charge transfers from the ligand to the metal and the nanodomains of the transition metals suggested the possible absorption centers present at the absorption threshold of the analyzed oxides. Through the XRD analysis, the formation of stable phases such as T-Nb16.8O42, o-Nb12O29, and rutile was observed at a lower temperature level, suggesting pore induction and an increase in surface area for the oxides studied, at a calcination temperature below that expected by the related literature. In addition, the synthesis with a higher temperature level altered the previously existing morphologies of the Ti:Nb, base and modified with Ru, forming the new mixed crystallographic phases Ti2Nb10O29 and TiNb2O7, respectively. As several semiconductor oxide applications aim to reduce costs with photoexcitation under visible light, the modified Ti:Ru oxide calcined at a temperature of 800 °C and synthesized according to the sol-gel methodology used in this work is suggested as the optimum preparation point. This study presented the formation of a stable crystallographic phase (rutile), a significant decrease in gap energy (2.01 eV), and a visible absorption threshold (620 nm).

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EXPRESS:利用溶胶-凝胶法合成的二氧化钛、五氧化二铌、钛铌和钌改性氧化物的光声光谱学。
这项研究的目的是开发二氧化钛、五氧化二铌、钛铌(Ti:Nb)氧化物以及用钌(Ru)修饰的材料,并对其进行形态/化学、光谱和结构表征,以提高其在可见光辐射下的光活化能力。采用溶胶-凝胶法合成的新材料通过以下技术进行了表征:扫描电子显微镜(SEM)、能量色散 X 射线光谱(EDS)、光声光谱和 X 射线衍射。SEM-EDS 分析表明碱的纯度很高,改性样品表面吸附了钌,形成了晶体,煅烧温度越高,可见的团聚体越多。紫外-可见(UV-Vis)区光声光谱的无损表征表明,煅烧温度的升高促进了化学结构的变化和间隙能的明显降低。从配体到金属的电荷转移和过渡金属的纳米域的叠加吸收带的分离表明,在所分析的氧化物的吸收阈值处可能存在吸收中心。通过 XRD 分析,在较低温度下观察到 T-Nb16.8O42、o-Nb12O29 和金红石等稳定相的形成,这表明所研究的氧化物在低于相关文献预期的煅烧温度下会诱发孔隙和增加表面积。此外,较高温度下的合成改变了 Ti:Nb、基体和 Ru 改性氧化物先前存在的形态,分别形成了新的混合晶相 Ti2Nb10O29 和 TiNb2O7。由于一些半导体氧化物应用旨在通过可见光下的光激发来降低成本,因此建议将在 800 °C 温度下煅烧的改性 Ti:Ru 氧化物作为最佳制备点,并采用本研究中使用的溶胶-凝胶方法进行合成。这种材料形成了稳定的晶体相(金红石型),间隙能显著降低(2.01 eV),并具有可见光吸收阈值(620 nm)。
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来源期刊
Applied Spectroscopy
Applied Spectroscopy 工程技术-光谱学
CiteScore
6.60
自引率
5.70%
发文量
139
审稿时长
3.5 months
期刊介绍: Applied Spectroscopy is one of the world''s leading spectroscopy journals, publishing high-quality peer-reviewed articles, both fundamental and applied, covering all aspects of spectroscopy. Established in 1951, the journal is owned by the Society for Applied Spectroscopy and is published monthly. The journal is dedicated to fulfilling the mission of the Society to “…advance and disseminate knowledge and information concerning the art and science of spectroscopy and other allied sciences.”
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