Effects of different reaction parameters in the hydrothermal synthesis of molybdenum oxides (MoO ) were investigated and monoclinic (β-) MoO 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 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 was obtained, while at 240 °C the orthorhombic (α-) MoO 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 , but 6 h led to pure α-MoO . With CTAB the product was bare o-MoO , however, when CrCl was applied, pure metastable m-MoO formed with the well-crystallized nanosheet morphology. The gas sensing of the MoO polymorphs was tested to H , which was the first such gas sensing study in the case of m-WO . Monoclinic MoO was found to be more sensitive in H sensing than o-MoO . This initial gas sensing study indicates that m-MoO has promising gas sensing properties and this MoO polymorph is promising to be studied in detail in the future.
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