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Effective Inclusion of Sizable Amounts of Mo within TiO₂ Nanoparticles Can Be Obtained by Reverse Micelle Sol-Gel Synthesis.

ABSTRACT: Six Mo/TiO₂ samples (with 0, 1.0, 2.5, 5.0, 7.5, and 10 wt % Mo nominal contents) were obtained by reverse micelle sol-gel synthesis, followed by calcination at 500 °C. The samples were characterized by means of powder X-ray Diffraction (PXRD), quantitative phase analysis as obtained by Rietveld refinement, field-emission scanning electron microscopy (FE-SEM) coupled with energy-dispersive X-ray analysis, N₂ adsorption/desorption at -196 °C, X-ray photoelectron spectroscopy, and diffuse reflectance (DR) UV-vis spectroscopy. As a whole, the adopted characterization techniques showed the inclusion of a sizeable Mo amount, without the segregation of any MoO _x phase. Specifically, PXRD showed the occurrence of anatase and brookite with all the studied samples; notwithstanding the mild calcination temperature, the formation of rutile occurred at Mo wt % ?2.5 likely due to the presence of brookite favoring, in turn, anatase to rutile transition. DR UV-vis and XP spectroscopies allowed determining the samples' band gap energy (E _g) and valence band energy, respectively, from which the conduction band energy was calculated; and the observed E _g value increase at 10 wt % Mo was ascribed to the Moss-Burstein effect.

SUBMITTER: Esposito S

PROVIDER: S-EPMC7931434 | biostudies-literature | 2021 Mar

REPOSITORIES: biostudies-literature

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Effective Inclusion of Sizable Amounts of Mo within TiO2 Nanoparticles Can Be Obtained by Reverse Micelle Sol-Gel Synthesis.

Esposito Serena S Ditaranto Nicoletta N Dell'Agli Gianfranco G Nasi Roberto R Rivolo Paola P Bonelli Barbara B

ACS omega 20210219 8

Six Mo/TiO2 samples (with 0, 1.0, 2.5, 5.0, 7.5, and 10 wt % Mo nominal contents) were obtained by reverse micelle sol-gel synthesis, followed by calcination at 500 °C. The samples were characterized by means of powder X-ray Diffraction (PXRD), quantitative phase analysis as obtained by Rietveld refinement, field-emission scanning electron microscopy (FE-SEM) coupled with energy-dispersive X-ray analysis, N2 adsorption/desorption at -196 °C, X-ray photoelectron spectroscopy ...[more]

PMID: 33681577

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Project description:Titanium dioxide (TiO2) in the form of thin films has attracted enormous attention for photocatalysis. It combines the fundamental properties of TiO2 as a large bandgap semiconductor with the advantage of thin films, making it competitive with TiO2 powders for recycling and maintenance in photocatalytic applications. There are many aspects affecting the photocatalytic performance of thin film structures, such as the nanocrystalline size, surface morphology, and phase composition. However, the quantification of each influencing aspect needs to be better studied and correlated. Here, we prepared a series of TiO2 thin films using a sol-gel process and spin-coated on p-type, (100)-oriented silicon substrates with a native oxide layer. The as-deposited TiO2 thin films were then annealed at different temperatures from 400 °C to 800 °C for 3 h in an ambient atmosphere. This sample synthesis provided systemic parameter variation regarding the aspects mentioned above. To characterize thin films, several techniques were used. Spectroscopic ellipsometry (SE) was employed for the investigation of the film thickness and the optical properties. The results revealed that an increasing annealing temperature reduced the film thickness with an increase in the refractive index. Atomic force microscopy (AFM) was utilized to examine the surface morphology, revealing an increased surface roughness and grain sizes. X-ray diffractometry (XRD) and UV-Raman spectroscopy were used to study the phase composition and crystallite size. The annealing process initially led to the formation of pure anatase, followed by a transformation from anatase to rutile as the annealing temperature increased. An overall enhancement in crystallinity was also observed. The photocatalytic properties of the thin films were tested using the photocatalytic decomposition of acetone gas in a home-built solid (photocatalyst)-gas (reactant) reactor. The composition of the gas mixture in the reaction chamber was monitored using in situ Fourier transform infrared spectroscopy. Finally, all of the structural and spectroscopic characteristics of the TiO2 thin films were quantified and correlated with their photocatalytic properties using a correlation matrix. This provided a good overview of which film properties affect the photocatalytic efficiency the most.

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Effective Inclusion of Sizable Amounts of Mo within TiO₂ Nanoparticles Can Be Obtained by Reverse Micelle Sol-Gel Synthesis.

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Effective Inclusion of Sizable Amounts of Mo within TiO<sub>2</sub> Nanoparticles Can Be Obtained by Reverse Micelle Sol-Gel Synthesis.

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