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

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4 Results and discussion<br />

characterised with XRD which showed highly crystall<strong>in</strong>e DOH (XRD pattern not shown).<br />

Microscopic images clearly show hexagonal crystals on the surface (Photos not shown).<br />

A B<br />

Figure 38 DOH Zeolite layer by sp<strong>in</strong> coat<strong>in</strong>g (A) followed by hydrothermal growth. B is deposited wet<br />

followed by hydrothermal growth and f<strong>in</strong>ally calc<strong>in</strong>ed.<br />

A similar suspension of DOH nuclei <strong>in</strong> H2O was deposited and subsequently dried at<br />

200ºC <strong>for</strong> 2 hours <strong>for</strong> seed attachment. The DOH nuclei on the substrates were grown<br />

hydrothermally <strong>in</strong> a 100SiO2:5.9ADA:69EN:3506H2O (<strong>in</strong> molar ratio) gel composition at<br />

200ºC <strong>for</strong> 24 hours. This gel composition was selected as described <strong>in</strong> 125 <strong>for</strong> preparation<br />

of th<strong>in</strong> DDR membrane layers. DDR layers are grown with this gel composition at 160-<br />

170ºC, DOH layer crystallisation temperature is selected at 200ºC. F<strong>in</strong>ally, the washed<br />

membranes were calc<strong>in</strong>ed <strong>for</strong>m<strong>in</strong>g a brown layer like Figure 38-B.<br />

Figure 39 presents the surface of membrane B. 10-20 µm hexagonal DOH crystals are<br />

clearly present.<br />

Figure 39 Optical microscope image of DOH membrane A’s surface<br />

Figure 40-A presents a cross section of DOH membrane B consist<strong>in</strong>g of an α-Al2O3<br />

support with the delam<strong>in</strong>ated DOH layer on top. Some areas <strong>in</strong>dicate attachment between<br />

67<br />

Hexagonal<br />

DOH crystals<br />

50 µm

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