Nanocrystalline and stacking-disordered β -cristobalite AlPO 4 chemically stabilized at room temperature: synthesis, physical characterization, and X-ray powder diffraction data

• Published in: Powder diffraction 2017-09, Vol.32 (S1), p.S193-S200
• Main Authors: Peplinski, B., Adamczyk, B., Formanek, P., Meyer, C., Krüger, O., Scharf, H., Reinsch, S., Ostermann, M., Nofz, M., Jäger, C., Adam, C., Emmerling, F.
• Format: Article
• Language: English
• ISSN: 0885-7156; 1945-7413
• DOI: 10.1017/S0885715617000537

This paper reports the first successful synthesis and the structural characterization of nanocrystalline and stacking-disordered β -cristobalite AlPO 4 that is chemically stabilized down to room temperature and free of crystalline impurity phases. Several batches of the title compound were synthesized and thoroughly characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy, selected area electron diffraction, energy dispersive X-ray spectroscopy mapping in SEM, solid-state 31 P nuclear magnetic resonance ( 31 P-NMR) spectroscopy including the TRAPDOR method, differential thermal analysis (DTA), gas-sorption methods, optical emission spectroscopy, X-ray fluorescence spectroscopy, and ion chromatography. Parameters that are critical for the synthesis were identified and optimized. The synthesis procedure yields reproducible results and is well documented. A high-quality XRD pattern of the title compound is presented, which was collected with monochromatic copper radiation at room temperature in a wide 2 θ range of 5°–100°.