Single crystalline ammonium trivanadate NH 4 V 3 O 8 with variable morphologies, including shuttles, flowers, belts, and plates, was synthesized by the hydrothermal treatment of NH 4 VO 3 with acetic acid. The crystals optimally grow under gentle conditions of 140°C for 48 h. The resulting NH 4 V 3 O 8 microcrystals were characterized by means of X-ray diffraction, scanning electron microscopy, infrared and Raman spectroscopy, static magnetization studies, and thermal analysis. The key factors

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... o control the size and morphology of the crystals are the pH value and the vanadium concentration. A tentative microscopic growth mechanism is proposed and it is demonstrated how shape and morphology of the resulting microcrystalline material can be tuned by appropriate synthesis parameters.