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

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4 Results and discussion Intensity (a.u.) Ti 0,5 Zr 0,5 O 2 at 600ºC 10 20 30 40 50 60 70 2Theta [º] 95 Diethanolamine Diisopropanolamine Orthorhombic TiZrO 4 Figure 61 XRD diffraction patterns of 50 mol % TiO2 in ZrO2 dried sols calcined at 600ºC when diethanolamine and diisopropanolamine are compared. 4.3.2.7 Static corrosion tests A static corrosion test is preformed as a simplified test to study the chemical stability of these powders. The results of these tests can be informative but not conclusive on the hydrothermal stability of membrane layers. The TiO2, ZrO2 and Ti0.5Zr0.5O2 bulk materials that are calcined at 400, 500 and 600ºC powders showed to be stable at a pH of 13 for 8 days. The chemical stability of Ti0.5Zr0.5O2 bulk materials is slightly lower than that of the single oxides at a pH of 1 for 8 days. However, only a few Ti and Zr ppms are dissolved in the acid. The chemical stability of these microporous inorganic materials in acids indicates that they are promising candidates for the formation of hydrothermally stable membranes. 4.3.2.8 Microstructure properties comparison by the Ketone and Amine approach The sol syntheses of the Ketone and Amine-approach are different in the concentration, pH, raw material and hydrolysing agents. Despite that, the crystallisation temperature and the microstructure properties of calcined and dried ketone and amine sols are compared. The amine-approach offered membrane materials with generally higher crystallisation temperatures, higher specific surface areas and smaller pore sizes. This makes the amineapproach used in this study more interesting for membrane materials than the ketoneapproach. However, both approaches can be applied for the formation of microporous TiO2, ZrO2 or binary oxides. Mesoporous materials were made by templating 8YSZ or by synthesising TiO2 rich powders. TiO2 – (Y2O3)ZrO2 membranes and membrane layers are characterised in the next section.
4 Results and discussion 4.3.3 Sol-Gel derived membrane characterisation Supported 8YSZ layers were prepared from the ketone sols and characterised with scanning electron microscopy (SEM), transmission electron microscopy (TEM) and single gas permeance measurement. Similar analyses are performed on TiO2, ZrO2 and binary oxide layers that were prepared by amine sols. Additional, X-ray photoelectron spectroscopy (XPS), Raman spectroscopy and Secondary Ion Mass Spectroscopy (SIMS) measurements are prepared on the latter. 4.3.3.1 Ketone approach - 8YSZ layers 8YSZ was prepared on glass substrates and on graded porous alumina supports (γ-Al2O3). Figure 62-B shows a coating applied by simple drying of a film composed of 8YSZ sol using acetyl acetone, caproic acid and block copolymer F127 (YSZ/F127 ~ 1/4 wt/wt). In this case, the substrate was a microscope glass slip and the calcination temperature was 500ºC for 2 hours. The obtained film has a thickness of about 200 nm, and a fine porosity can be observed, although the primary particles cannot be recognized due to the resolution of SEM technique. A B YSZ Glass Substrate Figure 62 Cross section SEM image of a coated YSZ sol blended with a block copolymer on a glass slip and calcined at 500ºC. Two kinds of 8YSZ layers have been prepared on graded porous γ-Al2O3 membranes being i) 8YSZ sol using acetyl acetone in combination with nanonic acid and ii) 8YSZ sol using acetyl acetone, caproic acid and F127. A ~50 nm thin 8YSZ layer is obtained on a γ-Al2O3 membrane after calcining at 450ºC an 8YSZ sol that included nanonic acid. The surface and cross section of the membrane indicate a homogeneous layer (Figure 63). 96
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Mitglied der Helmholtz-Gemeinschaft
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Forschungszentrum Jülich GmbH Inst
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List of Abbreviations Ac Acetyl Ace
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Summary CO2 capture and storage mig
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Zusammenfassung Die Abtrennung und
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Content Content CONTENT............
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1 Introduction and aims 1 Introduct
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2 Theoretical background 2 Theoreti
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2 Theoretical background Table 2 Ox
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2 Theoretical background Poly-cryst
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2 Theoretical background membranes
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2 Theoretical background Dry or wet
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2 Theoretical background due to its
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2 Theoretical background 2.3.3.2 Mi
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2 Theoretical background 2.4 Microp
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2 Theoretical background Figure 15
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2 Theoretical background wall inter
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3 Experimental 3 Experimental The m
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3 Experimental vacuum sample holder
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3 Experimental o of as-made DOH cry
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3 Experimental Another solution was
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Page 126 and 127: 6 References 22. Shao, Z., Dong, H.
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Page 137: Band | Volume 8 ISBN 978-3-89336-52
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