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Effects of different reaction parameters in the hydrothermal synthesis of molybdenum oxides (MoO 3 ) were investigated and monoclinic (β-) MoO 3 was prepared hydrothermally for the first time. Various temperatures (90/210 °C, and as a novelty 240 °C) and durations (3/6 h) were used. At 240 °C, cetyltrimethylammonium bromide (CTAB) and CrCl 3 additives were also tested. Both the reaction temperatures and durations played a significant role in the formation of the products. At 90 °C, h-MoO 3 was obtained, while at 240 °C the orthorhombic (α-) MoO 3 formed with hexagonal rod-like and nanofibrous morphology, respectively. The phase transformation between these two phases was observed at 210 °C. At this temperature, the 3 h reaction time resulted in the mixture of h- and α-MoO 3 , but 6 h led to pure α-MoO 3 . With CTAB the product was bare o-MoO 3 , however, when CrCl 3 was applied, pure metastable m-MoO 3 formed with the well-crystallized nanosheet morphology. The gas sensing of the MoO 3 polymorphs was tested to H 2 , which was the first such gas sensing study in the case of m-WO 3 . Monoclinic MoO 3 was found to be more sensitive in H 2 sensing than o-MoO 3 . This initial gas sensing study indicates that m-MoO 3 has promising gas sensing properties and this MoO 3 polymorph is promising to be studied in detail in the future.

Hydrothermal Synthesis and Gas Sensing of Monoclinic MoO3 Nanosheets