Preparation and growth mechanism of micro spherical ammonium dinitramide crystal based on ultrasound-assisted solvent-antisolvent method

Abstract

Micro-sized spherical ammonium dinitramide (ADN) crystals are successfully prepared by a facile ultrasound-assisted solvent-antisolvent recrystallization method without introducing any additives. The influences of the volume ratio of solvent to antisolvent, the antisolvent temperature and the ultrasound power on the micro-morphologies and properties of ADN crystals are studied systematically. The changes of morphology, particle size, crystal structure and melting point of the ADN crystals are characterized through scanning electron microscopy (SEM), laser particle size analyzer (LPSA), X-ray diffraction (XRD) and differential scanning calorimetry (DSC), respectively. The results show that the optimal experimental parameters for the ADN crystal of spherical morphology are as follows: the volume ratio of solvent to antisolvent is 1:50, the antisolvent temperature is 20 ℃, and the ultrasound power is 70 W. The predicted hexagonal-flake and spherical morphologies for the ADN are close to the experimental morphologies. The growth mechanism of the spherical ADN crystal changes with supersaturation of the ADN solution. As the degree of supersaturation increases, the growth models of the spherical ADN change from the spiral growth to the rough growth, and the morphologies of ADN change from the large-sized ADN ball to the small-sized ADN ball.