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

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4 Results and discussion Vads / cm 3 g -1 200 150 100 50 0,0 0,2 0,4 0,6 0,8 1,0 p/p0 0 Figure 49 N2 isotherms TiO2 calcined at 400ºC (◊), 500ºC (○) and 600ºC (□). Open symbols present the adsorption and closed symbols the desorption points. Exo uV/mg 0,2 0,1 0,0 -0,1 -0,2 -0,3 400ºC 500ºC 0 100 200 300 400 500 600 Temperature [ºC] 83 DTA TG Figure 50 DTA-TG curves of dried TiO2 sol. 600ºC A gradual anatase to rutile TiO2 transformation in combination with removal of the remaining organics might explain the weight stabilisation above ~450ºC. Similar results have been found by Zou et al. 116 A mixture of anatase and rutile TiO2 is formed when the 120 100 80 60 40 20 weight loss %
4 Results and discussion dried TiO2 sol is calcined at 600ºC. Xu et al. 112 found rutile phase transformation temperature higher than 600ºC. This might be explained by the difference in sol synthesis or 30 minutes dwell time instead of 2 hours. A combination of rutile and anatase TiO2 was observed at 500ºC when the ketone approach was applied. DEA seems to prevent the anatase rutile transformation compared to the ketone approach and might be explained by the stronger bonded precursor modifier. TiO2 layers prepared similar as the powder discussed above might have the same microstructural properties and form crystalline mesoporous TiO2 membranes. However, the microstructural properties of the layers can differ from the powders due to i) the formation of thin layers instead of agglomerated particles and ii) capillary forces when a thin layer is applied on a porous substrate. 10 20 30 40 50 60 2Theta [º] Figure 51 XRD diffraction patterns of dried TiO2 sols calcined at 140, 400, 500, 600ºC. The crystal size determined with the Scherrer relationship is presented in the inlay. 4.3.2.3 Amine approach - ZrO2 Type I N2-sorption isotherms are obtained when the dried ZrO2 DEA sols were calcined at 400, 500 and 600ºC (Figure 52). The specific surface area seems to be stable in the temperature range of 400-500ºC and decreases at higher calcination temperatures (Table 24). The ZrO2 type I N2 sorption isotherm indicates lower specific surface area values than TiO2 but are similar to the results published in literature. 116 84 600ºC Crystal size [nm] 500ºC 30 25 20 15 10 5 0 400ºC 140ºC 400 500 600 T [ºC]
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Mitglied der Helmholtz-Gemeinschaft
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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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1 Introduction and aims Candidate m
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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 2.1.2 Micr
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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 the materi
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2 Theoretical background Figure 9 D
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2 Theoretical background Figure 11
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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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Page 56 and 57: 3 Experimental 3.4 Characterisation
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Page 102 and 103: 4 Results and discussion In pure Ti
Page 104 and 105: 4 Results and discussion In summary
Page 106 and 107: 4 Results and discussion Intensity
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Page 126 and 127: 6 References 22. Shao, Z., Dong, H.
Page 128 and 129: 6 References 65. Van den Berg, A. W
Page 130 and 131: 6 References 108. Wen, T. L., Heber
Page 132 and 133: Curriculum Vitae - George van der D
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Page 137: Band | Volume 8 ISBN 978-3-89336-52
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Inorganic Microporous Membranes for Gas Separation in Fossil Fuel ...

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