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Bach S, Celinski VR, Dietzsch M, et al. Thermally highly stable amorphous zinc phosphate intermediates during the formation of zinc phosphate hydrate. J Am Chem Soc. 2015;137(6):2285-94doi: 10.1021/ja5103663.
Bach, S., Celinski, V. R., Dietzsch, M., Panthöfer, M., Bienert, R., Emmerling, F., Schmedt auf der Günne, J., & Tremel, W. (2015). Thermally highly stable amorphous zinc phosphate intermediates during the formation of zinc phosphate hydrate. Journal of the American Chemical Society, 137(6), 2285-94. https://doi.org/10.1021/ja5103663
Bach, Sven, et al. "Thermally highly stable amorphous zinc phosphate intermediates during the formation of zinc phosphate hydrate." Journal of the American Chemical Society vol. 137,6 (2015): 2285-94. doi: https://doi.org/10.1021/ja5103663
Bach S, Celinski VR, Dietzsch M, Panthöfer M, Bienert R, Emmerling F, Schmedt auf der Günne J, Tremel W. Thermally highly stable amorphous zinc phosphate intermediates during the formation of zinc phosphate hydrate. J Am Chem Soc. 2015 Feb 18;137(6):2285-94. doi: 10.1021/ja5103663. Epub 2015 Feb 05. PMID: 25602353.
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J Am Chem Soc. 2015 Feb 18;137(6):2285-94. doi: 10.1021/ja5103663. Epub 2015 Feb 05.

Thermally highly stable amorphous zinc phosphate intermediates during the formation of zinc phosphate hydrate.

Journal of the American Chemical Society

Sven Bach, Vinicius R Celinski, Michael Dietzsch, Martin Panthöfer, Ralf Bienert, Franziska Emmerling, Jörn Schmedt auf der Günne, Wolfgang Tremel

Affiliations

  1. Institute of Inorganic Chemistry and Analytical Chemistry, Johannes Gutenberg University Mainz , Duesbergweg 10-14, D-55128 Mainz, Germany.

PMID: 25602353 DOI: 10.1021/ja5103663

Abstract

The mechanisms by which amorphous intermediates transform into crystalline materials are still poorly understood. Here we attempt to illuminate the formation of an amorphous precursor by investigating the crystallization process of zinc phosphate hydrate. This work shows that amorphous zinc phosphate (AZP) nanoparticles precipitate from aqueous solutions prior to the crystalline hopeite phase at low concentrations and in the absence of additives at room temperature. AZP nanoparticles are thermally stable against crystallization even at 400 °C (resulting in a high temperature AZP), but they crystallize rapidly in the presence of water if the reaction is not interrupted. X-ray powder diffraction with high-energy synchrotron radiation, scanning and transmission electron microscopy, selected area electron diffraction, and small-angle X-ray scattering showed the particle size (≈20 nm) and confirmed the noncrystallinity of the nanoparticle intermediates. Energy dispersive X-ray, infrared, and Raman spectroscopy, inductively coupled plasma mass spectrometry, and optical emission spectrometry as well as thermal analysis were used for further compositional characterization of the as synthesized nanomaterial. (1)H solid-state NMR allowed the quantification of the hydrogen content, while an analysis of (31)P{(1)H} C rotational echo double resonance spectra permitted a dynamic and structural analysis of the crystallization pathway to hopeite.

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