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Crystallization in Nonaqueous Media of Co- and Mn-Substituted Microporous Aluminophosphates Investigated by in Situ Synchrotron X-ray Powder Diffraction.

In situ synchrotron X-ray powder diffraction was used to investigate the crystallization of microporous transition metal-substituted aluminophosphates from nonaqueous media. The gels contained ethylene glycol and triethylamine as the template and were heated in quartz glass capillaries at temperatures up to 200 degrees C. The following crystalline products were formed: MnAPO-5, [AFI], CoAPO-5, [AFI], and AlPO(4)-5, [AFI]. Three nonaqueous systems were investigated in situ, where the crystallization of MAPO-5-type materials were followed. Solvothermal crystallization of MnAPO-5 and CoAPO-5 was studied, and the effect of adding HF as a mineralizing agent was investigated. Time-resolved powder diffraction data were collected using a translating imaging plate (TIP) camera, and crystallization curves were extracted using integrated diffraction peaks. Kinetic analysis of the crystallization curves was performed using an Avrami-type expression, alpha(t) = exp(-(kt)(n)()). Apparent activation energies were determined from Arrhenius plots: MnAPO-5, 94 kJ/mol; MnAPO-5(HF), 68 kJ/mol; CoAPO-5, 61 kJ/mol. Crystallization of CoAPO-5 is faster than for MnAPO-5, and the values for n obtained by fitting with the Avrami-type expression were significantly lower for CoAPO-5 than for MnAPO-5.