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

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4 Results and discussion<br />

nanonic YSZ<br />

γ-Al2O3<br />

α-Al2O3<br />

Figure 63 SEM photograph of a coated nanonic YSZ sol α-and γ-Al2O3 substrate and calc<strong>in</strong>ed at 450ºC.<br />

Figure 64 presents the TEM study of the supported 8YSZ layer that <strong>in</strong>cluded acetyl<br />

acetone, caproic acid and F127. The substrate was prepared from α-Al2O3 and is highly<br />

crystall<strong>in</strong>e. The γ-Al2O3 <strong>in</strong>termediate layer has a thickness of 6 µm (Figure 64-A). The<br />

YSZ functional layer presents a nanocrystall<strong>in</strong>e phase and has a thickness of only 20-30<br />

nm (Figure 64-B). Nanostructur<strong>in</strong>g due to the addition of F127 could not be observed <strong>in</strong><br />

this analysis. Clearly th<strong>in</strong> cubic YSZ layers can be prepared us<strong>in</strong>g the ketone approach.<br />

The cubic phase was identified by Raman spectroscopy (Figure 65). The band at 1155<br />

cm -1 can be assigned to the <strong>in</strong>organic bond<strong>in</strong>g of ZrO2 with the Al2O3 support<strong>in</strong>g layer.<br />

A B<br />

6µm γ-Al2O3<br />

Figure 64 TEM analysis of a membrane: electron diffraction pattern of the (A) α-Al2O3 and (B) γ-Al2O3,<br />

and TEM images of (C) a 6 µm γ-Al2O3 <strong>in</strong>termediate layer and (D) detail of the top 8YSZ layer that<br />

conta<strong>in</strong>ed F127, acetyl acetone and caproic acid <strong>in</strong> the sol (20-30 nm <strong>in</strong> thickness) on the <strong>in</strong>termediate<br />

layer.<br />

97<br />

γ-Al2O3<br />

8YSZ+F

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