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MoO3 nanobelts were prepared by a one-step hydrothermal method and then assembled with aluminum nanoparticles using polyvinylpyrrolidone as a binder. The physicochemical properties of the as-prepared samples were carefully characterized by scanning electron microscopy, transmission electron microscopy, X-ray diffraction, thermogravimetric analysis/differential scanning calorimetry, and drop weight impact test. The results showed that the Tonset of Mo-Al-0, Mo-Al-1, Mo-Al-2, and Fe-Al-0 are 474.8°C, 484.2°C, 478.5°C, and 514.8°C, respectively, which are 66.0°C, 56.6°C, 62.3°C, and 26.0°C lower than that of pure Al-NPs (540.8°C). The total exothermic heat of selfassembled MoO3/Al during DSC test is about 2626.9 J/g, which is 229.6, 420.8, and 11.1 J/g higher than that of Al/commercial MoO3, Al/hydrothermal MoO3, and Al/referenced Fe2O3. Furthermore, the high exothermic self-assembled MoO3/Al thermite is totally insensitive to impact. [ABSTRACT FROM AUTHOR]