Controlling the crystal phase of a material using solution-based method is a challenging task and has significant consequence to the material’s properties. Herein we report the phase and size-controlled synthesis of tungsten oxide hydrates at room temperature via a simple precipitation method. In the absence and presence of oxalic acid, orthorhombic WO3·H2O and monoclinic WO3·2H2O nanoplates of size in the range of 200–600 (thickness <50 nm) and 40–200 nm (thickness <20 nm) were respectively synthesized. Oxalic acid is found to play the central role in the phase transition due to its chelating nature that facilitates bonding of oxalate ions to tungsten cations leading to formation of WO3·2H2O. Upon annealing at 400 °C for 2 h under air, both WO3·H2O and WO3·2H2O nanoplates were converted to monoclinic WO3 nanoplates. These nanoplates were demonstrated to be highly efficient for the photocatalytic detoxification of toxic Cr­(VI) in the acidic pH under the visible light irradiation. The best Cr­(VI) reduction performance was obtained with WO3·2H2O nanoplates due to its smaller band gap and larger effective surface area. In addition, a lower pH value is found to facilitates the Cr­(VI) reduction. Furthermore, highly concentrated methylene blue was efficiently removed (>95%) by adsorption on the nanoplates within a minute, suggesting the importance and potential of a material that can be synthesized at room temperature.

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Aluminum oxide (Al2O3) has abundantly been used as a catalyst, and its catalytic activity has been tailored by loading transition metals. Herein, γ-Al2O3 nanosheets were prepared by the solvothermal method, and transition metals (M = Co, Ni, Cu, Rh, Pd, Ag, Ir, Pt, and Au) were loaded onto the nanosheets. Big data sets of thermal CO oxidation and photocatalytic CO2 reduction activities were fully examined for the transition metal-loaded Al2O3 nanosheets. Their physicochemical properties were examined by scanning electron microscopy, high-resolution transmission electron microscopy, X-ray diffraction crystallography, and X-ray photoelectron spectroscopy. It was found that Rh, Pd, Ir, and Pt-loading showed a great enhancement in CO oxidation activity while other metals negated the activity of bare Al2O3 nanosheets. Rh-Al2O3 showed the lowest CO oxidation onset temperature of 172 °C, 201 °C lower than that of bare γ-Al2O3. CO2 reduction experiments were also performed to show that CO, CH3OH, and CH4 were common products. Ag-Al2O3 nanosheets showed the highest performances with yields of 237.3 ppm for CO, 36.3 ppm for CH3OH, and 30.9 ppm for CH4, 2.2×, 1.2×, and 1.6× enhancements, respectively, compared with those for bare Al2O3. Hydrogen production was found to be maximized to 20.7 ppm during CO2 reduction for Rh-loaded Al2O3. The present unique pre-screening test results provided very useful information for the selection of transition metals on Al2O3-based energy and environmental catalysts.

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