This paper reports the first successful synthesis and the structural characterization of nanocrystalline and stacking-disordered β-cristobalite AlPO4 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 31P nuclear magnetic resonance (31P-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 2θ range of 5°–100°.

For the first time evidence is provided that a nanocrystalline and stacking-disordered, chemically stabilized β-cristobalite form of AlPO4 occurs in a sewage sludge ash (SSA). This proof is based on a combined X-ray powder diffraction and X-ray fluorescence investigation of an SSA produced at a large-scale fluidized bed incineration facility serving a catching area with a population of 2 million. The structural and chemical characterization was carried out on ‘as received’ SSA samples as well as on solid residues remaining after leaching this SSA in sodium hydroxide solution. Thus, it was ascertained that the observed nanocrystalline and stacking-disordered cristobalite-like component belongs to the aluminum phosphate component of this SSA, rather than to its silicon dioxide component. In addition, a direct proof is presented that the chemically stabilized β-cristobalite form of AlPO4 does crystallize from X-ray amorphous precursors under conditions that mimic the huge heating rate and short retention time (just seconds at T ≈ 850°C), typical for fluidized bed incinerators.