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 147 Lin (Counts) 17000 16000 15000 14000 13000 12000 11000 10000 9000 8000 7000 6000 5000 4000 3000 2000 1000 0 d=5.66260 d=4.06262 d=3.81913 d=3.56584 d=3.37999 d=3.31475 d=2.84605 d=2.61629 d=2.22306 d=2.21507 d=2.26889 d=2.02414 d=1.91594 d=1.88452 d=1.85366 10 20 30 40 50 60 70 80 90 100 2-Theta - Scale DEP01 - File: DEP01.RAW - Type: 2Th/Th locked - Start: 10.000 ° - End: 100.000 ° - Step: 0.020 ° - Step time: 1. s - Temp.: 239 °C - Time Started: 0 s - 2-Theta: 10.000 ° - Theta: 5.000 ° - Chi: 0.00 ° - Phi: Operations: Import 74-0944 (C) - Ammonium Silicon Fluoride - (NH4)3SiF6F - Y: 50.00 % - d x by: 1. - WL: 1.5406 - Tetragonal - a 8.04000 - b 8.04000 - c 5.84500 - alpha 90.000 - beta 90.000 - gamma 90.000 - Primitive - P4/ 35-0758 (*) - Ammonium Fluoride - NH4F - Y: 50.00 % - d x by: 1. - WL: 1.5406 - Hexagonal - a 4.4408 - b 4.44080 - c 7.1726 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - P63mc (186) - 2 - 12 Fig. (5.8): Deposit from fluorination on silica liner lid in glovebox (⎯ JCPDS card number 74-0944 (NH4)3SiF6F, tetragonal; ⎯ JCPDS card number 35-0758 NH4F, hexagonal, P63mc). Table (5.6): Ten most intense peaks with corresponding 2θ (observed and theoretical) and Miller indices for deposit from fluorination on silica liner lid in glovebox. Observed 2θθθθ / ° Observed intensity / % Theoretical 2θθθθ / ° Theoretical intensity / % Phase hkl JCPDS Card 15.64860 5.7 15.58618 100 (NH4)3SiF6F 110 74-0944 21.87498 7.5 21.80589 65 (NH4)3SiF6F 111 " 23.28796 54.0 23.11875 100 NH4F 100 35-0758 24.96701 100.0 24.81206 44 NH4F 002 " 26.36295 40.8 26.27801 53 NH4F 101 " 34.25556 16.7 34.16474 22 NH4F 102 " 40.53863 31.6 40.56329 42 NH4F 110 " 40.69070 20.6 40.40954 12 (NH4)3SiF6F 320 74-0944 44.70528 14.0 44.57491 30 NH4F 103 35-0758 48.19427 10.7 48.11534 17 NH4F 112 " d=1.42275 d=1.28553 d=1.24208
5. Crystallisation studies; MDO 148 Glass melting During glass melting the melt volatilised, particularly for the fluorotellurite melts, due to the presence of volatile fluoride compounds. The deposit left on the silica liner and lid was collected after melting glass MOF005 (70TeO2-10Na2O-20ZnF2, mol. %) for 12 hours at 800°C in the glovebox under nitrogen. Fig. (5.9) shows the XRD trace of this deposit. Lin (Counts) 1500 1400 1300 1200 1100 1000 900 800 700 600 500 400 300 200 100 0 d=4.03809 d=3.37720 d=3.08511 d=2.96683 d=2.39384 d=2.06142 d=1.89726 d=1.86598 d=1.69532 d=1.65589 10 20 30 40 50 60 70 80 90 100 2-Theta - Scale lindep - File: Melt_Deposit.RAW - Type: 2Th/Th locked - Start: 10.000 ° - End: 100.000 ° - Step: 0.020 ° - Step time: 1. s - Temp.: 25 °C (Room) - Time Started: 0 s - 2-Theta: 10.000 ° - Theta: 5.000 ° - Aux1: Operations: Import 42-1365 (*) - Paratellurite, syn - TeO2 - Y: 50.00 % - d x by: 1. - WL: 1.54056 - Tetragonal - a 4.81011 - b 4.81011 - c 7.6122 - alpha 90.000 - beta 90.000 - gamma 90.000 - Primitive - P41212 (92) - 4 - 176. Fig (5.9): XRD trace of deposit left on the silica liner and lid after melting glass MOF005 (70TeO2-10Na2O-20ZnF2, mol. %) for 12 hours at 800°C in glovebox under nitrogen (⎯ JCPDS card number 42-1365: TeO2, tetragonal, P41212). The deposit was identified using JCPDS card number 42-1365: TeO2, tetragonal, space group P41212. Table (5.7) shows the ten most intense peaks with corresponding 2θ (observed and theoretical) and Miller indices. d=1.51705 d=1.48850 d=1.47395 d=1.26612 d=1.25684 d=1.18642
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5. Crystallisation studies; MDO 148<br />
Glass melting<br />
During glass melting the melt volatilised, particularly for the fluorotellurite melts, due to<br />
the presence of volatile fluoride compounds. The deposit left on the silica liner and lid<br />
was collected after melting glass MOF005 (70TeO2-10Na2O-20ZnF2, mol. %) for 12<br />
hours at 800°C in the glovebox under nitrogen. Fig. (5.9) shows the XRD trace of this<br />
deposit.<br />
Lin (Counts)<br />
1500<br />
1400<br />
1300<br />
1200<br />
1100<br />
1000<br />
900<br />
800<br />
700<br />
600<br />
500<br />
400<br />
300<br />
200<br />
100<br />
0<br />
d=4.03809<br />
d=3.37720<br />
d=3.08511<br />
d=2.96683<br />
d=2.39384<br />
d=2.06142<br />
d=1.89726<br />
d=1.86598<br />
d=1.69532<br />
d=1.65589<br />
10 20 30 40 50 60 70 80 90 100<br />
2-Theta - Scale<br />
lindep - File: Melt_Deposit.RAW - Type: 2Th/Th locked - Start: 10.000 ° - End: 100.000 ° - Step: 0.020 ° - Step time: 1. s - Temp.: 25 °C (Room) - Time Started: 0 s - 2-Theta: 10.000 ° - Theta: 5.000 ° - Aux1:<br />
Operations: Import<br />
42-1365 (*) - Paratellurite, syn - TeO2 - Y: 50.00 % - d x by: 1. - WL: 1.54056 - Tetragonal - a 4.81011 - b 4.81011 - c 7.6122 - alpha 90.000 - beta 90.000 - gamma 90.000 - Primitive - P41212 (92) - 4 - 176.<br />
Fig (5.9): XRD trace of deposit left on the silica liner and lid after melting glass MOF005<br />
(70TeO2-10Na2O-20ZnF2, mol. %) for 12 hours at 800°C in glovebox under nitrogen (⎯<br />
JCPDS card number 42-1365: TeO2, tetragonal, P41212).<br />
The deposit was identified using JCPDS card number 42-1365: TeO2, tetragonal, space<br />
group P41212. Table (5.7) shows the ten most intense peaks with corresponding 2θ<br />
(observed and theoretical) and Miller indices.<br />
d=1.51705<br />
d=1.48850<br />
d=1.47395<br />
d=1.26612<br />
d=1.25684<br />
d=1.18642