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 149 Table (5.7): Ten most intense peaks with corresponding 2θ (observed and theoretical) and Miller indices for deposit left on the silica liner and lid after melting glass MOF005 (70TeO2-10Na2O-20ZnF2, mol. %) for 12 hours at 800°C in glovebox. Observed 2θθθθ / ° Observed intensity / % Theoretical 2θθθθ / ° Theoretical intensity / % hkl JCPDS Card 22.00947 23.0 21.86131 8 101 42-1365 25.90481 17.8 - - - - 26.38511 98.1 26.20208 95 110 42-1365 26.67667 22.3 - - - - 28.93278 20.1 28.75441 14 111 42-1365 30.11162 100.0 29.94866 100 102 " 37.54363 22.2 37.36155 15 200 " 48.69993 64.3 48.52443 47 212 " 55.29621 23.7 55.12931 19 114 / 221 " 62.03630 15.1 61.85459 10 204 / 311 " 5.2.1.3. XRD of glasses which crystallised during processing or characterisation During melting A batch of glass MOF001 (65TeO2-10Na2O-25ZnF2, mol. %) was melted in the fume cupboard, with fluorinating agent (see section 3.4) added to dry the batch further (1 g of (NH4)HF2 to 1 g of batch). However, after melting a 10g batch for 5 hours in a platinum crucible at 800°C, and dropping to 700°C to cast, most of the melt had volatilised, leaving behind around 5g of a white solid deposit in the crucible. Fig. (5.10) shows the XRD trace of this deposit. It can be seen from this trace, that a glass-ceramic has resulted from this treatment. An amorphous ‘halo’ can be seen at around 30° 2θ, and the presence of crystalline material. The closest match to the crystalline peaks was JCPDS card number: 20-1182: sodium zinc fluoride NaZnF3, orthorhombic, space group Pbnm. Table
5. Crystallisation studies; MDO 150 (5.8) shows the ten most intense peaks with corresponding 2θ (observed and theoretical), Miller indices were not available. Lin (Counts) 350 340 330 320 310 300 290 280 270 260 250 240 230 220 210 200 190 180 170 160 150 140 130 120 110 100 90 80 70 60 50 40 30 20 10 0 d=3.82959 d=2.76468 d=2.71648 d=2.41520 d=2.30154 d=2.07505 d=1.92988 d=1.72680 d=1.70674 d=1.66587 d=1.56300 20 30 40 50 60 70 80 90 100 2-Theta - Scale Fluorinated Melt 1 - File: Fluorinated_melt_1.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 ° - Thet Operations: Import 20-1182 (*) - Sodium Zinc Fluoride - NaZnF3 - Y: 50.00 % - d x by: 1. - WL: 1.5406 - Orthorhombic - I/Ic PDF 3. - Fig. (5.10): Deposit which resulted from melting a 10g batch of glass MOF001 (65TeO2- 10Na2O-25ZnF2, mol. %) for 5 hours in a platinum crucible at 800°C, and dropping to 700°C to cast, with fluorinating agent added (⎯ JCPDS card number 20-1182: NaZnF3, orthorhombic, Pbnm). Table (5.8): Ten most intense peaks with corresponding 2θ (observed and theoretical), Miller indices not available for JCPDS card number: 20-1182: NaZnF3. Deposit which resulted from melting a 10g batch of glass MOF001 (65TeO2-10Na2O-25ZnF2, mol. %) for 5 hours in a platinum crucible at 800°C, and dropping to 700°C to cast, with fluorinating agent added. Observed Observed Theoretical Theoretical JCPDS 2θθθθ / ° intensity / % 2θθθθ / ° intensity / % Card 23.22349 57.0 22.88104 100 20-1182 32.36824 34.7 32.04241 25 " 32.95778 45.0 32.58016 80 " 37.20035 60.2 36.86213 6 " 39.10413 35.1 38.47392 10 " 47.00123 100.0 46.64207 50 " 52.87373 70.9 52.46974 25 " 58.83817 31.5 58.50879 20 " 67.95478 30.3 67.69251 8 " 86.51300 62.9 86.08170 1 " d=1.22483 d=1.21491 d=1.10584 d=1.09155
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5. Crystallisation studies; MDO 150<br />
(5.8) shows the ten most intense peaks with corresponding 2θ (observed and theoretical),<br />
Miller indices were not available.<br />
Lin (Counts)<br />
350<br />
340<br />
330<br />
320<br />
310<br />
300<br />
290<br />
280<br />
270<br />
260<br />
250<br />
240<br />
230<br />
220<br />
210<br />
200<br />
190<br />
180<br />
170<br />
160<br />
150<br />
140<br />
130<br />
120<br />
110<br />
100<br />
90<br />
80<br />
70<br />
60<br />
50<br />
40<br />
30<br />
20<br />
10<br />
0<br />
d=3.82959<br />
d=2.76468<br />
d=2.71648<br />
d=2.41520<br />
d=2.30154<br />
d=2.07505<br />
d=1.92988<br />
d=1.72680<br />
d=1.70674<br />
d=1.66587<br />
d=1.56300<br />
20 30 40 50 60 70 80 90 100<br />
2-Theta - Scale<br />
Fluorinated Melt 1 - File: Fluorinated_melt_1.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 ° - Thet<br />
Operations: Import<br />
20-1182 (*) - Sodium Zinc Fluoride - NaZnF3 - Y: 50.00 % - d x by: 1. - WL: 1.5406 - Orthorhombic - I/Ic PDF 3. -<br />
Fig. (5.10): Deposit which resulted from melting a 10g batch of glass MOF001 (65TeO2-<br />
10Na2O-25ZnF2, mol. %) for 5 hours in a platinum crucible at 800°C, and dropping to<br />
700°C to cast, with fluorinating agent added (⎯ JCPDS card number 20-1182: NaZnF3,<br />
orthorhombic, Pbnm).<br />
Table (5.8): Ten most intense peaks with corresponding 2θ (observed and theoretical),<br />
Miller indices not available for JCPDS card number: 20-1182: NaZnF3. Deposit which<br />
resulted from melting a 10g batch of glass MOF001 (65TeO2-10Na2O-25ZnF2, mol. %)<br />
for 5 hours in a platinum crucible at 800°C, and dropping to 700°C to cast, with<br />
fluorinating agent added.<br />
Observed Observed Theoretical Theoretical JCPDS<br />
2θθθθ / ° intensity / % 2θθθθ / ° intensity / % Card<br />
23.22349 57.0 22.88104 100 20-1182<br />
32.36824 34.7 32.04241 25 "<br />
32.95778 45.0 32.58016 80 "<br />
37.20035 60.2 36.86213 6 "<br />
39.10413 35.1 38.47392 10 "<br />
47.00123 100.0 46.64207 50 "<br />
52.87373 70.9 52.46974 25 "<br />
58.83817 31.5 58.50879 20 "<br />
67.95478 30.3 67.69251 8 "<br />
86.51300 62.9 86.08170 1 "<br />
d=1.22483<br />
d=1.21491<br />
d=1.10584<br />
d=1.09155