ASAXS study of CaF2 nanoparticles embedded in a silicate glass matrix

Armin Hoell, Zoltan Varga, Vikram Singh Raghuwanshi, Michael Krumrey, Christian Bocker, Christian Rüssel

Research output: Contribution to journalArticleResearchpeer-review

Abstract

The formation and growth of nanosized CaF2 crystallites by heat treatment of an oxyfluoride glass of composition 7.65Na2O-7.69K2O-10.58CaO-12.5CaF2-5. 77Al2O3-55.8SiO2 (wt%) was investigated using anomalous small-angle X-ray scattering (ASAXS). A recently developed vacuum version of the hybrid pixel detector Pilatus 1M was used for the ASAXS measurements below the Ca K-edge of 4038 eV down to 3800 eV. ASAXS investigation allows the determination of structural parameters such as size and size distribution of nanoparticles and characterizes the spatial distribution of the resonant element, Ca. The method reveals quantitatively that the growing CaF2 crystallites are surrounded by a shell of lower electron density. This depletion shell of growing thickness hinders and finally limits the growth of CaF2 crystallites. Moreover, in samples that were annealed for 10 h and more, additional very small heterogeneities (1.6 nm diameter) were found.

Original languageEnglish
Pages (from-to)60-66
Number of pages7
JournalJournal of Applied Crystallography
Volume47
Issue number1
DOIs
Publication statusPublished - Feb 2014
Externally publishedYes

Keywords

  • anomalous small-angle X-ray scattering
  • crystallization
  • glass ceramics
  • nanostructures

Cite this

Hoell, Armin ; Varga, Zoltan ; Raghuwanshi, Vikram Singh ; Krumrey, Michael ; Bocker, Christian ; Rüssel, Christian. / ASAXS study of CaF2 nanoparticles embedded in a silicate glass matrix. In: Journal of Applied Crystallography. 2014 ; Vol. 47, No. 1. pp. 60-66.
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abstract = "The formation and growth of nanosized CaF2 crystallites by heat treatment of an oxyfluoride glass of composition 7.65Na2O-7.69K2O-10.58CaO-12.5CaF2-5. 77Al2O3-55.8SiO2 (wt{\%}) was investigated using anomalous small-angle X-ray scattering (ASAXS). A recently developed vacuum version of the hybrid pixel detector Pilatus 1M was used for the ASAXS measurements below the Ca K-edge of 4038 eV down to 3800 eV. ASAXS investigation allows the determination of structural parameters such as size and size distribution of nanoparticles and characterizes the spatial distribution of the resonant element, Ca. The method reveals quantitatively that the growing CaF2 crystallites are surrounded by a shell of lower electron density. This depletion shell of growing thickness hinders and finally limits the growth of CaF2 crystallites. Moreover, in samples that were annealed for 10 h and more, additional very small heterogeneities (1.6 nm diameter) were found.",
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ASAXS study of CaF2 nanoparticles embedded in a silicate glass matrix. / Hoell, Armin; Varga, Zoltan; Raghuwanshi, Vikram Singh; Krumrey, Michael; Bocker, Christian; Rüssel, Christian.

In: Journal of Applied Crystallography, Vol. 47, No. 1, 02.2014, p. 60-66.

Research output: Contribution to journalArticleResearchpeer-review

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