The preparation of ultra-fine energetic materials still faces great challenges. In order to prepare the ultra-fine NTO crystals with controllable size and morphology, the study proposes a novel ultrasonic-assisted spray technology that can ensure the rapidity and safety of the preparation of ultra-fine NTO crystals. The as-prepared NTO crystals are characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD), and the effects of solvent type, solution concentration, ultrasonic parameters, and anti-solvent on the morphology and average size of NTO crystals are investigated. The results obtained show that NTO ultra-fine crystals with an average particle size of 0.2 μm can be obtained quickly in optimum preparation conditions. The effectiveness of the technique presented for preparing ultra-fine spherical NTO crystals was demonstrated by comparison with baseline experiments. Ultrasonic-assisted spray technology offers a safe and fast route for the preparation of ultra-fine NTO particles and reveals an ideal method for the preparation of other ultra-fine energetic particles.
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