Tellurite And Fluorotellurite Glasses For Active And Passive
Tellurite And Fluorotellurite Glasses For Active And Passive Tellurite And Fluorotellurite Glasses For Active And Passive
7. Surface properties; MDO 259 opposite sides (see section 6.1.1.1), and treated with silver ion-exchange, as described in table (7.2). Table (7.2): Ion-exchange methods used on tellurite glasses. Sample ID T08 ST08 Composition / mol. % 80TeO2-9ZnO- 10Na2O-1Er2O3 79TeO2-5ZnO- 10Na2O-5PbO- 1Yb2O3 T / °C t / hr. 285 12 270 5 Treatment Evaporated silver layer on both flat sides (100 and 300 µm), followed by heat treatment under an inert atmosphere (argon). Dipped one flat side into a molten salt solution of 2AgNO3-49NaNO3-49KNO3 (mol. %). These glasses were then annealed to reduce stresses introduced by the ion-exchange process, and mounted in epoxy resin and cross-sectioned for EDX analysis in the electron microscope. 7.1.3.2. Environmental scanning electron microscopy (ESEM) The concentration profile of the silver ions in the glass was mapped using electron dispersive X-ray (EDX) analysis in an environmental scanning electron microscope (ESEM), using a FEI XL30 FEG-ESEM. This instrument was used in auxiliary mode, with the chamber filled with nitrogen (BOC). This mode enabled the sample to be imaged and analysed without coating the sample. In standard SEM operating under a vacuum, insulating samples must be sputtered with a conductive coating such as carbon or gold. Aperture size, accelerating voltage and scales are displayed on all electron micrographs.
7. Surface properties; MDO 260 Elemental analyses on EDX traces were performed using the ESEM software. The column aperture diameter was 100 µm for EDX analysis and 30 µm for imaging. Theory of operation Images are formed in the SEM by a scanning method. The SEM uses a beam of electrons to image the sample. Fig. (7.1) illustrates a typical SEM setup. Fig. (7.1): Schematic of typical SEM setup, where SE = secondary electron, BSE = backscattered electron, CRT = cathode ray tube, and E-T = Everhart-Thornley [5]. Electrons are produced by thermionic emission from a tungsten filament, and are accelerated to energies of the range 20-40 keV. The beam is focused onto the surface of the sample by a number of magnetic lenses, where the beam diameter is typically 2-10 nm [5]. The electron beam is scanned across the sample surface by the scan coils, and a
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7. Surface properties; MDO 259<br />
opposite sides (see section 6.1.1.1), and treated with silver ion-exchange, as described in<br />
table (7.2).<br />
Table (7.2): Ion-exchange methods used on tellurite glasses.<br />
Sample<br />
ID<br />
T08<br />
ST08<br />
Composition /<br />
mol. %<br />
80TeO2-9ZnO-<br />
10Na2O-1Er2O3<br />
79TeO2-5ZnO-<br />
10Na2O-5PbO-<br />
1Yb2O3<br />
T /<br />
°C<br />
t /<br />
hr.<br />
285 12<br />
270 5<br />
Treatment<br />
Evaporated silver layer on both flat sides (100<br />
and 300 µm), followed by heat treatment<br />
under an inert atmosphere (argon).<br />
Dipped one flat side into a molten salt<br />
solution of 2AgNO3-49NaNO3-49KNO3<br />
(mol. %).<br />
These glasses were then annealed to reduce stresses introduced by the ion-exchange<br />
process, and mounted in epoxy resin and cross-sectioned for EDX analysis in the electron<br />
microscope.<br />
7.1.3.2. Environmental scanning electron microscopy (ESEM)<br />
The concentration profile of the silver ions in the glass was mapped using electron<br />
dispersive X-ray (EDX) analysis in an environmental scanning electron microscope<br />
(ESEM), using a FEI XL30 FEG-ESEM. This instrument was used in auxiliary mode,<br />
with the chamber filled with nitrogen (BOC). This mode enabled the sample to be imaged<br />
and analysed without coating the sample. In standard SEM operating under a vacuum,<br />
insulating samples must be sputtered with a conductive coating such as carbon or gold.<br />
Aperture size, accelerating voltage and scales are displayed on all electron micrographs.