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Nanocrystalline and stacking-disordered β-cristobalite AlPO4 chemically stabilized at room temperature: synthesis, physical characterization, and X-ray powder diffraction data

Published online by Cambridge University Press:  07 June 2017

B. Peplinski ,
B. Adamczyk ,
P. Formanek ,
C. Meyer ,
O. Krüger ,
H. Scharf ,
S. Reinsch ,
M. Ostermann ,
M. Nofz  and
C. Jäger
...Show all authors
B. Peplinski*
Affiliation:
BAM Federal Institute for Materials Research and Testing, Berlin, Germany
B. Adamczyk
Affiliation:
BAM Federal Institute for Materials Research and Testing, Berlin, Germany
P. Formanek
Affiliation:
Leibniz-Institut für Polymerforschung Dresden e.V., Dresden, Germany
C. Meyer
Affiliation:
BAM Federal Institute for Materials Research and Testing, Berlin, Germany
O. Krüger
Affiliation:
BAM Federal Institute for Materials Research and Testing, Berlin, Germany
H. Scharf
Affiliation:
BAM Federal Institute for Materials Research and Testing, Berlin, Germany
S. Reinsch
Affiliation:
BAM Federal Institute for Materials Research and Testing, Berlin, Germany
M. Ostermann
Affiliation:
BAM Federal Institute for Materials Research and Testing, Berlin, Germany
M. Nofz
Affiliation:
BAM Federal Institute for Materials Research and Testing, Berlin, Germany
C. Jäger
Affiliation:
BAM Federal Institute for Materials Research and Testing, Berlin, Germany
C. Adam
Affiliation:
BAM Federal Institute for Materials Research and Testing, Berlin, Germany
F. Emmerling
Affiliation:
BAM Federal Institute for Materials Research and Testing, Berlin, Germany
*
a)Author to whom correspondence should be addressed. Electronic mail: burkhard_peplinski@web.de
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Abstract

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°.

Keywords

stabilization of high-temperature phase at RTnanocrystalline AlPO4β-cristobalite structure typehigh-cristobalite formcristobalite formaluminum phosphate
Type
Technical Articles
Information
Powder Diffraction , Volume 32 , Supplement S1 , September 2017 , pp. S193 - S200
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Copyright
Copyright © International Centre for Diffraction Data 2017 

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References

Bergmann, J., Friedel, P., and Kleeberg, R. (1998). “BGMN – a new fundamental parameters based Rietveld program for laboratory X-ray sources, it's use in quantitative analysis and structure investigations,” CPD Newsl. 20, 5–8.Google Scholar
Bruker-AXS GmbH (2007). DiffracPLUS, V. 2007, Karlsruhe, Germany.Google Scholar
Cheary, W. and Coelho, A. A. (1992). “A fundamental parameters approach of X-ray line-profile fitting,” J. Appl. Cryst. 25(2), 109–121.CrossRefGoogle Scholar
FIZ and NIST (2016). Inorganic Crystal Structure Data Base (ICSD) (Karlsruhe, Germany, Gaithersburg, USA).Google Scholar
Graetsch, H. A. (2003). “Thermal expansion and thermally induced variations of the crystal structure of AlPO4 low cristobalite,” N. Jb. Miner. Mh. Jg. 2003(7), 289–301.Google Scholar
Guthrie, G. D., Bish, D. L., and Reynolds, R. C. (1995). “Modelling the X-ray diffraction pattern of opal-CT,” Am. Mineral. 80, 869–872.Google Scholar
ICDD (2015). PDF-4 + 2015 (Database), edited by Dr. Soorya Kabekkodu (International Centre for Diffraction Data, Newtown Square, PA, USA).Google Scholar
Kraus, W. and Nolze, G. (1996). “ POWDER CELL – a program for the representation and manipulation of crystal structures and calculation of the resulting X-ray powder patterns,” J. Appl. Crystallogr. 29, 301–303.Google Scholar
Migdal-Mikuli, A., Hetmanczyk, J., and Hetmanczyk, L. (2007). “Thermal behaviour of [Ca(H2O)4](NO3)2 ,” JTAC 89, 499–503.Google Scholar
Peplinski, B., Adam, C., Adamczyk, B., Müller, R., Michaelis, M., Krahl, Th., and Emmerling, F. (2014). “Nanocrystalline and stacking-disordered β-cristobalite AlPO4: the now deciphered main constituent of a municipal sewage sludge ash from a full-scale incineration facility,” in 14. European Powder Diffraction Conference (EPDIC14), Aarhus, Denmark, 15.-18. June 2014, Book of Abstracts, MS09-P115.Google Scholar
Peplinski, B., Adam, C., Adamczyk, B., Müller, R., Michaelis, M., Krahl, Th., and Emmerling, F. (2015). “Nanocrystalline and stacking-disordered β-cristobalite AlPO4: the now deciphered main constituent of a municipal sewage sludge ash from a full-scale incineration facility,” Powder Diffr. J. 30(S1), S31–S35.Google Scholar
Perrotta, J. A., Grubbs, D. K., Martin, E. S., Dando, N. R., McKinstry, H. A., and Huang, C.-Y. (1989). “Chemical stabilization of β-cristobalite,” J. Am. Ceram. Soc. 72, 441–447.Google Scholar
Petzet, S., Peplinski, B., Bodkhe, S. Y., and Cornell, P. (2011). “Recovery of phosphorus and aluminium from sewage sludge ash by a new wet chemical elution process (SESAL-Phos – recovery process),” Water Sci.Technol. 64, 693–699.Google Scholar
Petzet, S., Peplinski, B., and Cornel, P. (2012). “On the wet chemical phosphorus recovery from sewage sludge ashes by acidic or alkaline leachings and by an optimized combination of both,” Water Res. 46, 3769–3780.CrossRefGoogle ScholarPubMed
Phillips, B. L., Thompson, J. G., Xiao, Y., and Kirkpatrick, R. J. (1993). “Constraints on the structure and dynamics of the β-cristobalite polymorphs of SiO2 and AlPO4 from 31P, 27Al, and 29Si NMR spectroscopy to 770 °C,” Phys. Chem. Miner. 20, 341–352.Google Scholar
Querner, G., Bergmann, J., and Blau, W. (1991). “A method for data reduction and optimal experimental design in XPD,” Mater. Sci. Forum 79–82, 107–112.CrossRefGoogle Scholar
Spearing, D. R., Farnan, I., and Stebbing, J. G. (1992). “Dynamics of the α-β phase transition in quartz and cristobalite as observed by in situ high temperature 29Si and 17O NMR,” Phys. Chem. Miner. 19, 307–321.Google Scholar
Wilson, A. J. C. and Price, E. (1999). International Tables for Crystallography, vol. C Mathematical, Physical and Chemical Tables (Kluwer, Dordrecht), 2nd ed., p. 203.Google Scholar
Wright, A. F. and Leadbetter, A. J. (1975). “The structure of the β-cristobalite phases of SiO2 and AlPO4 ,” Philos. Mag. 31, 1391–1401.Google Scholar
Yuan, F. and Huang, L. (2012). “ α-β transformation and disorder in β-cristobalite silica,” Phys. Rev. B 85, 134114-1–134114-7.Google Scholar
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