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

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3 Experimental Element analysis The carbon content of the DOH crystals and sol-gel derived sols and bulk materials was obtained by combusting the sample with the use of radiofrequency heating (2300ºC) in an oxygen flow with combusting additives. The quantity of combusted carbon was determined by means of Infrared (Leco CS 600). Nitrogen content in the DOH crystals and sol-gel derived bulk materials was determined by thermal conductivity detection, the inorganic samples were heated in helium flow by means of resistance heating (Leco TCH 600). The metal ion impurities in the DOH zeolite crystals were studied with Inductively Coupled Plasma with Optical Emission Spectroscopy (TJA-IRIS-INTREPID). Static corrosion tests were performed in nitric acid and sodium hydroxide at a pH ranging from 1 to 13 by stirring the suspension of the sol/gel derived bulk materials fired at 400, 500 and 600ºC. Corrosion tests were carried out at room temperature for 8 days. 3.4.2 Microporous membrane characterisation Scanning and Transmission Electron Microscopy (SEM-TEM) Surface and cross section SEM analysis were performed using a LEO 1530 (Gemini) electron microscope. Electron energy dispersive X-ray analysis (EDX) was used for qualitative analysis of the powder. TEM investigations were performed using a Philips CM200 or a Tecnai F20 G 2 operating at 200 kV. Secondary Ion Mass Spectroscopy The infiltration depth of DEA sols was studied by means of Secondary Ion Mass Spectroscopy (SIMS). By repeatedly sputtering the membrane surface with argon the chemical composition could be determined at various depths. Profiles were obtained with a resolution of ~0.4 nm. The chemical composition was determined to be in an area of 0.01 mm 2 inside a crater of 0.09-0.16 mm 2 excluding edge effects. Raman spectroscopy The Raman spectroscopy measurements were made using a Horiba Jobin Yvon SpexT64000 system equipped with two scanning mechanisms, one for the foremonochromator and another one for the spectrograph. The SpexT64000 is equipped with 1800 grooves/mm gratings. The 488 nm line of an Ar + ion laser (COHERENT Innova® 300C Series) was used for the probes excitation. The spectra were collected in a backscattering geometry with a confocal Raman microscope equipped with an Olympus MPlan 50x objective. The detection of the Raman signal was carried out with a CCD detector operating at -196°C. The probes were also measured using a Raman micro spectrometer (Horiba Jobin Yvon, model LabRam) using the 514.5 nm excitation line 47
3 Experimental from an Ar + laser (model 2213) and the 632.8 nm excitation line from a He-Ne laser. The spectra were collected in a backscattering geometry with a Raman microscope equipped with an Olympus LMPlanFl 50x/0.50 objective. The acquisition time was set at 5 cycles/20 seconds. X-Ray Photoelectron Spectroscopy X-Ray Photoelectron Spectroscopy (XPS) were performed using a XPS/AES spectrometer based on Physical Electronics components. In-depth profiling is obtained with a 4kV Ar-sputter gun for 2 min. Quantification of the results was done using the program MultiPak resulting in at% with 15% relative accuracy. Mass transport Gas permeation characteristics of the sol-gel derived membranes were determined in a setup at the University of Twente and at the University of Eindhoven as schematically outlined in Figure 20. This was done with pure gasses at pressures and temperatures ranging from 2 to 5 bars and 100 to 200°C, respectively. In this setup the rate of permeation is measured at atmospheric conditions using a thermal mass flow controller (MFC). Feed pressure and temperature were controlled with a mechanical pressure reducer (PR) and programmable electrical heater. Upon installation of the membranes in a stainless steel, they were first degassed for at least 60 h at 200°C (heating rate 1 ºC/min) under helium flush. During all measurements feed pressure, transmembrane pressure and temperature were logged automatically. All gasses, i.e. hydrogen (H2), helium (He), nitrogen (N2), argon (Ar) and carbon dioxide (CO2), were used with a minimum purity of 99.999%. Only sulphur hexafluoride (SF6) was used with a minimum purity of 99.8%. Pressure reducer PR P Membrane in sample holder 48 Valve V ∆∆∆∆P ∆∆∆∆P Mass Flow MFC Controller Figure 20 Schematic outline of the setup for the determination of gas permeation characteristics. P presents the feed pressure and ∆P the pressure difference over the membrane.
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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
Page 8 and 9: Summary CO2 capture and storage mig
Page 10 and 11: Zusammenfassung Die Abtrennung und
Page 12 and 13: Content Content CONTENT............
Page 14 and 15: 1 Introduction and aims 1 Introduct
Page 16 and 17: 1 Introduction and aims Candidate m
Page 18 and 19: 2 Theoretical background 2 Theoreti
Page 20 and 21: 2 Theoretical background Despite th
Page 22 and 23: 2 Theoretical background Table 2 Ox
Page 24 and 25: 2 Theoretical background 2.1.2 Micr
Page 26 and 27: 2 Theoretical background Poly-cryst
Page 28 and 29: 2 Theoretical background membranes
Page 30 and 31: 2 Theoretical background Dry or wet
Page 32 and 33: 2 Theoretical background the materi
Page 34 and 35: 2 Theoretical background Figure 9 D
Page 36 and 37: 2 Theoretical background Figure 11
Page 38 and 39: 2 Theoretical background due to its
Page 40 and 41: 2 Theoretical background 2.3.3.2 Mi
Page 42 and 43: 2 Theoretical background 2.4 Microp
Page 44 and 45: 2 Theoretical background Figure 15
Page 46 and 47: 2 Theoretical background wall inter
Page 48 and 49: 3 Experimental 3 Experimental The m
Page 50 and 51: 3 Experimental vacuum sample holder
Page 52 and 53: 3 Experimental o of as-made DOH cry
Page 54 and 55: 3 Experimental Another solution was
Page 56 and 57: 3 Experimental 3.4 Characterisation
Page 60 and 61: 3 Experimental Additionally, the hy
Page 62 and 63: 4 Results and discussion Abundance
Page 64 and 65: 4 Results and discussion 4.2 Zeolit
Page 66 and 67: 4 Results and discussion Table 14 D
Page 68 and 69: 4 Results and discussion hours usin
Page 70 and 71: 4 Results and discussion Intensity
Page 72 and 73: 4 Results and discussion The carbon
Page 74 and 75: 4 Results and discussion DOH crysta
Page 76 and 77: 4 Results and discussion 900 [ºC]
Page 78 and 79: 4 Results and discussion characteri
Page 80 and 81: 4 Results and discussion without a
Page 82 and 83: 4 Results and discussion 4.3.1.1 Ke
Page 84 and 85: 4 Results and discussion Solid Cont
Page 86 and 87: 4 Results and discussion difference
Page 88 and 89: 4 Results and discussion V [cm ads
Page 90 and 91: 4 Results and discussion The averag
Page 92 and 93: 4 Results and discussion DTA µV/mg
Page 94 and 95: 4 Results and discussion Vads / cm
Page 96 and 97: 4 Results and discussion The increa
Page 98 and 99: 4 Results and discussion 20 30 40 5
Page 100 and 101: 4 Results and discussion V micro /V
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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4 Results and discussion nanonic YS
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4 Results and discussion ~50nm TiO2
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4 Results and discussion Raman Inte
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4 Results and discussion Tungsten 5
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4 Results and discussion Mol% Carbo
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4 Results and discussion Permeance
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4 Results and discussion He Permean
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5 Conclusions and recommendations m
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5 Conclusions and recommendations m
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6 References 22. Shao, Z., Dong, H.
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6 References 65. Van den Berg, A. W
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6 References 108. Wen, T. L., Heber
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Curriculum Vitae - George van der D
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Last but not least, I would like to
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Band | Volume 8 ISBN 978-3-89336-52
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