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

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4 Results and discussion V [cm ads 3 /g] 150 120 90 60 30 V ads / cm 3 g -1 dV/d2r (cm 3 /g·nm) 60 50 40 30 20 10 0.05 0.04 0.03 0.02 0.01 8YSZAcCa+F 8YSZAcCA 0,0 0,2 0,4 0,6 0,8 1,0 p/p0 0 C16 CTA C10 F127 0.00 0.1 1 10 100 diameter in [nm] B1 B2 0 0.0 0.2 0.4 0.6 0.8 1.0 P/P 0 77 F127 C10 CTA C16 Figure 45 N2-sorption isotherms of different calcined sols A) isotherms of the 8YSZ powders calcined at 500ºC that contained acetyl acetone and caproic acid in the sols (grey dots) and with the additional SDA F127 (black dots) 500ºC. B1) Pore size distribution and B2) isotherms of 8YSZ powders calcined at 450ºC with different SDA’s C10, C16, CTA and F127 added to the 8YSZ sols. A
4 Results and discussion The addition of the combination acetyl acetone as precursor modifier and caproic acid as catalyst to the 8YSZ sol resulted in a decrease of specific surface area (70 to 49 m 2 /g) of the powders but increased the relative absorbed microporous volume. One could state that the material is becoming more microporous due to the addition of this combination of acetyl acetone and caproic acid. Similar powder that were synthesised without the addition of the SDA F127 resulted in even higher relative absorbed microporous volume. Figure 45-A clearly indicates the effect of the SDA F127 to 8YSZ sols. The pore diameter of this powder was estimated at 1.0 nm using the HK-SF method. The 8YSZ powder that was synthesised with the combination of acetyl acetone and caproic acid is the most microporous material found in this test. In spite its microporosity, it is believed that microporous material with 57 m 2 /g will likely result in layers with low permeation. The uncalcined 8YSZ powder was totally XRD-amorphous, as expected from the polymeric nature of the particles and the remaining organics embedded and bonded within the Zr-O / Y-O branches. The 8YSZ sol with the addition of the SDA F127 that was dried and followed by leaching procedure with n-propanol/n-heptane (see chapter 3.3.2.) is referred as the extracted sample. The extracted sample is almost amorphous but showed some weak order, deduced from the broad peak at 30º (main peak of the fluorite structure, see Figure 46). The samples calcined at 450ºC and 500ºC show already the pattern corresponding to the fluorite (cubic) structure without any other phase impurity (such as tetragonal or monoclinic zirconia phases), as expected from the stabilization effect of yttria (8 mol%). Intensity (a.u.) 25 30 35 40 45 50 55 60 65 70 75 2Theta [º] 78 CubicYSZ 500ºC Acetyl acetone+Caproic acid 500ºC 450ºC Extracted Figure 46 XRD diffraction patterns of the 8YSZ powders that were extracted or calcined at 450 and 500ºC. The upper line presents the 8YSZ powder calcined at 500º with the addition of the carboxylic caproic acid and acetyl acetone to the sol. All peaks are assigned to cubic ZrO2 structure (JCPDS card #30-1468).
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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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1 Introduction and aims Candidate m
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2 Theoretical background 2 Theoreti
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2 Theoretical background Despite th
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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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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 58 and 59: 3 Experimental Element analysis The
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
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Page 76 and 77: 4 Results and discussion 900 [ºC]
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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
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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
Page 108 and 109: 4 Results and discussion nanonic YS
Page 110 and 111: 4 Results and discussion ~50nm TiO2
Page 112 and 113: 4 Results and discussion Raman Inte
Page 114 and 115: 4 Results and discussion Tungsten 5
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Page 122 and 123: 5 Conclusions and recommendations m
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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
Page 134: Last but not least, I would like to
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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