Tellurite And Fluorotellurite Glasses For Active And Passive
Tellurite And Fluorotellurite Glasses For Active And Passive Tellurite And Fluorotellurite Glasses For Active And Passive
5. Crystallisation studies; MDO 155 (Puratronic, 99.9995%). The crystal structure is hexagonal, space group P63mc, analogous to wurtzite (ZnS). Oxygen anions are hexagonally close packed (hcp) with alternate tetrahedral voids filled with zinc cations [1]. Both zinc and oxygen are four coordinated to one another, therefore the structure can be thought of as interpenetrating hcp sublattices of Zn and O [1]. Na2CO3 Fig. (5.5) shows an XRD trace of the Na2CO3 powder used in this study sourced from Alfa Aesar (Puratronic, 99.997%). There was relatively high background noise on the XRD trace, most likely due to the low atomic weight of the atoms in the powder (Na, C and O, Z = 11, 6 and 8 respectively). This will result in less scattering of the incident X- rays compared to heavier compounds (e.g. TeO2 and ZnF2), and hence less X-ray counts at the detector for the hkl reflections of the NaCO3 crystals. However, the pattern matched that of pure Na2CO3, crystal structure monoclinic, space group C2/m. Na2CO3 decomposes in the glass melt to Na2O, therefore, the crystal structure of the carbonate is unrelated to the final state of the oxide in the glass. As-received ZnF2 Fig. (5.6) shows an XRD trace of the ZnF2 powder used in this study, sourced from Alfa Aesar. Although the quoted purity was high (Puratronic, 99.995%) there was a significant
5. Crystallisation studies; MDO 156 amount of Zn(OH)F, an orthorhombic phase, present (fig. (5.6)) [4]. Only cationic impurities were quoted on the assay sheet, therefore anionic impurities such as OH - were not included by Alfa Aesar for calculating purity. OH - can readily substitute for F - in many inorganic compounds and minerals, due to their similar ionic radius and electronegitivity. There was some tetragonal ZnF2 present (space group P42/mnm) in the powder which was identified on the trace. Fluorinated ZnF2 The XRD trace of the purified ZnF2 powder (fig. (5.7)), shows that the fluorination process was highly effective, removing a high proportion of the hydroxide phase from the batch [4] (see X-ray photoelectron spectroscopy (XPS) spectra in chapter 7 for quantification). The tetragonal phase ZnF2 (space group P42/mnm) has an analogous structure to rutile (TiO2). The zinc cations sit in octahedral holes, between the fluorine anions. Each zinc ion is surrounded by six fluorine ions, with each fluorine surrounded by three zinc ions [1]. 5.3.1.2. XRD of deposits from melting and fluorination Fluorination Fig. (5.8) shows an XRD trace of the deposit left from fluorination of ZnF2 with (NH4)HF2, on the silica liner lid in glovebox. Two crystalline phases can clearly be
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5. Crystallisation studies; MDO 155<br />
(Puratronic, 99.9995%). The crystal structure is hexagonal, space group P63mc,<br />
analogous to wurtzite (ZnS). Oxygen anions are hexagonally close packed (hcp) with<br />
alternate tetrahedral voids filled with zinc cations [1]. Both zinc and oxygen are four<br />
coordinated to one another, therefore the structure can be thought of as interpenetrating<br />
hcp sublattices of Zn and O [1].<br />
Na2CO3<br />
Fig. (5.5) shows an XRD trace of the Na2CO3 powder used in this study sourced from<br />
Alfa Aesar (Puratronic, 99.997%). There was relatively high background noise on the<br />
XRD trace, most likely due to the low atomic weight of the atoms in the powder (Na, C<br />
and O, Z = 11, 6 and 8 respectively). This will result in less scattering of the incident X-<br />
rays compared to heavier compounds (e.g. TeO2 and ZnF2), and hence less X-ray counts<br />
at the detector for the hkl reflections of the NaCO3 crystals. However, the pattern<br />
matched that of pure Na2CO3, crystal structure monoclinic, space group C2/m. Na2CO3<br />
decomposes in the glass melt to Na2O, therefore, the crystal structure of the carbonate is<br />
unrelated to the final state of the oxide in the glass.<br />
As-received ZnF2<br />
Fig. (5.6) shows an XRD trace of the ZnF2 powder used in this study, sourced from Alfa<br />
Aesar. Although the quoted purity was high (Puratronic, 99.995%) there was a significant