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TiO2-MoO3 composite systems were successfully prepared using a template-assisted microwave method at molar ratios TiO2:MoO3 = 8:2, 5:5 and 2:8. The synthesized material systems were comprehensively characterized, in terms of their crystalline structure (XRD and Raman spectroscopy), morphology (SEM, TEM and HRTEM analysis) and parameters of the porous structure (low-temperature N2 sorption). The materials exhibited highly crystalline phases: anatase and hexagonal molybdenum trioxide. Moreover, TEM analysis revealed hexagonal prism particles of MoO3 and nanocrystalline particles of TiO2. The proposed template-assisted microwave synthesis enabled the incorporation of TiO2 particles on the surface of hexagonal particles of MoO3, which resulted in a stable junction between titania and molybdenum trioxide. The values of BET surface area were 57, 29 and 11 m2/g for samples obtained at molar ratios TiO2:MoO3 = 8:2, 5:5 and 2:8 respectively. In electrochemical applications, titanium dioxide plays a crucial role as an intercalation intensifier, in which MoO3 is responsible for current conduction. Taking account of the potential electrochemical applications, the best system was obtained at the molar ratio TiO2:MoO3 = 5:5. The anode could maintain a capacity of 400 mAh/g at current densities in the range 100–1000 mA/g at potential values ranging from 1.00 to 3.30 V vs. Li/Li+. X-ray photoelectron spectroscopy (XPS) confirmed the effective intercalation of lithium ions into the TiO2-MoO3 composite materials.

Highly Crystalline TiO2-MoO3 Composite Materials Synthesized via a Template-Assisted Microwave Method for Electrochemical Application