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Inorganic Microporous Membranes for Gas Separation in Fossil Fuel ...

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4 Results and discussion<br />

Solid Content,<br />

8YSZ wt%<br />

0<br />

2.5<br />

5.0<br />

10<br />

15<br />

Max §<br />

73<br />

Carboxylic Acid<br />

Acetic Propanoic Caproic Nanonic<br />

12 6.6 3.2 2<br />

Viscosity (mPa·s)<br />

Figure 42 Viscosity of the obta<strong>in</strong>ed sols as a function of the type of carboxylic acid and the solid<br />

concentration.<br />

4.3.1.2 Am<strong>in</strong>e approach<br />

The synthesis of sols from diethanolam<strong>in</strong>e (DEA) modified precursors results <strong>in</strong> 0, 25,<br />

50, 66, 75, 90, 100 mol% TiO2 <strong>in</strong> ZrO2 sols that are stable at least <strong>for</strong> several weeks. The<br />

particle sizes of these DEA sols as measured by means of dynamic light scatter<strong>in</strong>g (DLS)<br />

and small angle X-ray scatter<strong>in</strong>g (SAXS). These results <strong>in</strong>dicate that all sol particles are<br />

similar <strong>in</strong> size (2-5 nm) and that their size does not depend significantly on the Ti to Zr<br />

ratio (Table 21-Figure 43).<br />

Replac<strong>in</strong>g the precursor modifier DEA with diisopropanolam<strong>in</strong>e (DIPA) resulted <strong>in</strong><br />

similar average particle sizes (Figure 44).<br />

Table 21 Particle sizes with errors between brackets and fractal dimensions of mol % TiO2 <strong>in</strong> ZrO2 DEAsols<br />

Sample Concentration Particle size by SAXS <strong>in</strong> nm Fractal dimension<br />

TiO2 2 wt% 3.8 (±0.5) 1.37 (±0.01)<br />

Ti0.5Zr0.5O2 2 wt% 2.8 (±1.0) 1.04 (±0.01)<br />

Ti0.5Zr0.5O2 4 wt% 3.6 (±1.0) 1.16 (±0.01)<br />

ZrO2 2 wt% 2.0 (±0.5) -

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