Preparation and characterization of superfine ammonium perchlorate (AP) crystals through ceramic membrane anti-solvent crystallization

• Published in: Journal of crystal growth Vol. 311; no. 21; pp. 4575 - 4580
• Main Authors: Ma, Zhenye, Li, Cheng, Wu, Rujun, Chen, Rizhi, Gu, Zhenggui
• Format: Journal Article
• Language: English
• Published: Amsterdam Elsevier B.V 15.10.2009; Elsevier
• Subjects: A1. Crystal structure; A2. Growth from solutions; B1. Ammonium perchlorate (AP); B3. Ceramic membrane anti-solvent crystallization (CMASC); Condensed matter: structure, mechanical and thermal properties; Cross-disciplinary physics: materials science; rheology; Equations of state, phase equilibria, and phase transitions; Exact sciences and technology; General studies of phase transitions; Materials science; Methods of crystal growth; physics of crystal growth; Nucleation; Physics; Solid-solid transitions; Specific phase transitions; Structure of solids and liquids; crystallography; Structure of specific crystalline solids; Theory and models of crystal growth; physics of crystal growth, crystal morphology and orientation; 62.23.St; B1. Ammonium perchlorate (AP); A1. Crystal structure; B3. Ceramic membrane anti-solvent crystallization (CMASC); A2. Growth from solutions; 82.40.Py; 61.46.Bc; 81.10.Dn; Crystal growth; Scanning electron microscopy; Particle size; Nucleation; Growth rate; Pore structure; Crystallization; XRD; Electron microscopy; Perchlorates; Acetates; Temperature effects; Morphology; Growth from solution; Acetone; Crystal structure
• ISSN: 0022-0248; 1873-5002
• DOI: 10.1016/j.jcrysgro.2009.06.008

In this paper, a novel ceramic membrane anti-solvent crystallization (CMASC) method was proposed for the safe and rapid preparation ammonium perchlorate (AP) crystals, in which the acetone and ethyl acetate were chosen as solvent and anti-solvent, respectively. Comparing with the conventional liquid anti-solvent crystallization (LASC), CMASC which successfully introduces ceramic membrane with regular pore structure to the LASC as feeding medium, is favorable to control the rate of feeding rate and, therefore, to obtain size and morphology controllable AP. Several kinds of micro-sized AP particles with different morphology were obtained including polyhedral-like, quadrate-like to rod-like. The effect of processing parameters on the crystal size and shape of AP crystals such as volume ratio of anti-solvent to solvent, feeding pressure and crystallization temperature were investigated. It is found that higher volume ratio of anti-solvent to solvent, higher feeding pressure and higher temperature result in smaller particle size. Scaning electron microscopy (SEM) and X-ray diffraction (XRD) were used to characterize the resulting AP crystals. The nucleation and growth kinetic of the resulting AP crystals were also discussed.