Details
| Original language | English |
|---|---|
| Pages (from-to) | 45-53 |
| Number of pages | 9 |
| Journal | Solid State Sciences |
| Volume | 77 |
| Early online date | 31 Jan 2018 |
| Publication status | Published - Mar 2018 |
Abstract
The paper deals with the mechanochemical synthesis of lead containing alkaline earth metal fluoride solid solutions MxPb1-xF2 (M = Ca, Sr, Ba) by high-energy ball milling. Several metal precursors and fluorinating agents were tested for synthesizing M0.5Pb0.5F2. Metal acetates and ammonium fluoride as precursors show the most promising results and were therefore used for the formation of MxPb1-xF2 with different metal cationic ratios. The characterization of the local fluorine coordination and the crystal structure was performed by 19F MAS NMR spectroscopy and X-ray diffraction. Additional calculations of 19F chemical shifts using the superposition model allows a deeper insight into the local structure of the compounds. The fluoride ion conductivity was followed by temperature dependent DC conductivity measurements. Significantly higher conductivities were found in comparison with those of the corresponding binary fluorides. The highest values were be observed for samples with high lead content M0.25Pb0.75F2, bearing in mind the much higher conductivity of PbF2 compared to MF2.
Keywords
- F MAS NMR spectroscopy, Impedance spectroscopy, Mechanochemical synthesis, Solid solutions
ASJC Scopus subject areas
- Chemistry(all)
- General Chemistry
- Materials Science(all)
- General Materials Science
- Physics and Astronomy(all)
- Condensed Matter Physics
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In: Solid State Sciences, Vol. 77, 03.2018, p. 45-53.
Research output: Contribution to journal › Article › Research › peer review
}
TY - JOUR
T1 - Mechanochemical synthesis, structure and properties of lead containing alkaline earth metal fluoride solid solutions MxPb1-xF2 (M = Ca, Sr, Ba)
AU - Heise, M.
AU - Scholz, G.
AU - Düvel, André
AU - Heitjans, Paul
AU - Kemnitz, E.
N1 - Funding Information: The authors thank the research training network GRK 1582/2 / HU-TP 31208402 “Fluorine as a Key Element” of DFG (Deutsche Forschungsgemeinschaft) for financial support. Paul Heitjans is supported by a Niedersachsen Professorship.
PY - 2018/3
Y1 - 2018/3
N2 - The paper deals with the mechanochemical synthesis of lead containing alkaline earth metal fluoride solid solutions MxPb1-xF2 (M = Ca, Sr, Ba) by high-energy ball milling. Several metal precursors and fluorinating agents were tested for synthesizing M0.5Pb0.5F2. Metal acetates and ammonium fluoride as precursors show the most promising results and were therefore used for the formation of MxPb1-xF2 with different metal cationic ratios. The characterization of the local fluorine coordination and the crystal structure was performed by 19F MAS NMR spectroscopy and X-ray diffraction. Additional calculations of 19F chemical shifts using the superposition model allows a deeper insight into the local structure of the compounds. The fluoride ion conductivity was followed by temperature dependent DC conductivity measurements. Significantly higher conductivities were found in comparison with those of the corresponding binary fluorides. The highest values were be observed for samples with high lead content M0.25Pb0.75F2, bearing in mind the much higher conductivity of PbF2 compared to MF2.
AB - The paper deals with the mechanochemical synthesis of lead containing alkaline earth metal fluoride solid solutions MxPb1-xF2 (M = Ca, Sr, Ba) by high-energy ball milling. Several metal precursors and fluorinating agents were tested for synthesizing M0.5Pb0.5F2. Metal acetates and ammonium fluoride as precursors show the most promising results and were therefore used for the formation of MxPb1-xF2 with different metal cationic ratios. The characterization of the local fluorine coordination and the crystal structure was performed by 19F MAS NMR spectroscopy and X-ray diffraction. Additional calculations of 19F chemical shifts using the superposition model allows a deeper insight into the local structure of the compounds. The fluoride ion conductivity was followed by temperature dependent DC conductivity measurements. Significantly higher conductivities were found in comparison with those of the corresponding binary fluorides. The highest values were be observed for samples with high lead content M0.25Pb0.75F2, bearing in mind the much higher conductivity of PbF2 compared to MF2.
KW - F MAS NMR spectroscopy
KW - Impedance spectroscopy
KW - Mechanochemical synthesis
KW - Solid solutions
UR - http://www.scopus.com/inward/record.url?scp=85041491136&partnerID=8YFLogxK
U2 - 10.15488/4942
DO - 10.15488/4942
M3 - Article
AN - SCOPUS:85041491136
VL - 77
SP - 45
EP - 53
JO - Solid State Sciences
JF - Solid State Sciences
SN - 1293-2558
ER -