Synthesis of Ce2O3 and characterization of hydrogen insertion using neutron diffraction and spectroscopic methods
1
조회
0
다운로드
0
인용
0
참고문헌
키워드
초록
The catalytic activity of ceria originates from oxygen vacancies. Ce2O3 is the most oxygen-deficient end-member of nonstoichiometricceria, CeO2-x. A new method of synthesizing air-stable Ce2O3 from the micron- and nano-sized CeO2 powderwas developed. The key part of this synthetic process is to reduce the sample in a low-pressure H2 gas (10 Torr) under vacuumat 1300°C. The percentage of the Ce2O3 phase in the reduced sample ranges from 55% ~ 96 wt.% according to the powdersize and reduction time. Hydrogen incorporation in reduced ceria was confirmed by secondary ion mass spectrometry depthprofile analysis and vibrational spectroscopic techniques, such as Raman and Fourier transform infrared spectroscopy. Thesurface region (zero depth) showed the highest H concentration that decreased with increasing profiling depth. The locationsof hydrogen incorporated in the Ce2O3 phase in the reduced sample were revealed by calculating the nuclear densitydistribution. The maximum entropy method-based pattern fitting and Dysnomia program were combined to calculate thenuclear density map using the neutron diffraction data.
Abstract
The catalytic activity of ceria originates from oxygen vacancies. Ce2O3 is the most oxygen-deficient end-member of nonstoichiometricceria, CeO2-x. A new method of synthesizing air-stable Ce2O3 from the micron- and nano-sized CeO2 powderwas developed. The key part of this synthetic process is to reduce the sample in a low-pressure H2 gas (10 Torr) under vacuumat 1300°C. The percentage of the Ce2O3 phase in the reduced sample ranges from 55% ~ 96 wt.% according to the powdersize and reduction time. Hydrogen incorporation in reduced ceria was confirmed by secondary ion mass spectrometry depthprofile analysis and vibrational spectroscopic techniques, such as Raman and Fourier transform infrared spectroscopy. Thesurface region (zero depth) showed the highest H concentration that decreased with increasing profiling depth. The locationsof hydrogen incorporated in the Ce2O3 phase in the reduced sample were revealed by calculating the nuclear densitydistribution. The maximum entropy method-based pattern fitting and Dysnomia program were combined to calculate thenuclear density map using the neutron diffraction data.
참고문헌 (48)
- G. Jacobs, , Catal. Lett., 96(1-2), pp.97~105 (2004)
- K. Polychronopoulou, , Recent Pat. Mater. Sci, 4(2), pp.122~145 (2011)
- F. Dvorak, , ACS Catal, 8(5), pp.4354~4363 (2018)
- K. Sohlberg, , J. Am. Chem. Soc, 123(27), pp.6609~6611 (2001)
- L. Jalowiecki-Duhamel, , Catal. Today, 138(3-4), pp.266~271 (2008)
- K. Werner, , J. Am. Chem. Soc, 139(48), pp.17608~17616 (2017)
- Y. Lara-López, "Synthesis and characterization of TiO2, CeO2, and TiO2-CeO2 particles forapplication in the treatment of phenol", Journal of Ceramic Processing Research, 20(1), pp.24~29 (2019), 청정에너지연구소[DOI]
- R. Ma, , Ceram. Int, 42(16), pp.18495~18502 (2016)
- Eun-Hui Hyeong, "Sonochemical synthesis of highly sinterable", nanocrystalline CeO2-based electrolyte powders for intermediatetemperature solid oxide fuel cells, 2012, pp.13(3), 349~352[DOI]
- J-W. Bae, , J. Eur. Ceram. Soc, 34(15), pp.3763~3768 (2014)
- Ji Young Park, "Enhanced ionic conductivity and suppressed electronic conductivity of an Al- and Mn-added ceria solid electrolyte", Journal of Ceramic Processing Research, 21, pp.63~67 (2020), 청정에너지연구소[DOI]
- Joo-Sin Lee, "Effects of lithium oxide addition on sintering behavior and electrical conductivity of yttria-doped ceria", Journal of Ceramic Processing Research, 17(10), pp.1078~1081 (2016), 청정에너지연구소[DOI]
- S. Masahiro, , Bull. Chem. Soc. Jpn, 78(5), pp.752~767 (2005)
- Mahsa. Zarinkamar, "One-step synthesis of ceria (CeO2) nano-spheres by a simple wet chemical method", Journal of Ceramic Processing Research, 17(3), pp.166~169 (2016), 청정에너지연구소[DOI]
- X. Zhang, , J. Eur. Ceram. Soc, 40(12), pp.4366~4372 (2020)
- M. B. Watkins, , J. Phys. Chem. C, 111(42), pp.15337~15341 (2007)
- L. Brugnoli, , J. Phys. Chem. C, 123(42), pp.25668~25679 (2019)
- J. Liu, , Ceram. Int, 46(5), pp.5976~5982 (2020)
- K. Werner, , J. Am. Chem. Soc, 139(48), pp.17608~17616 (2017)
- E. A. KuKmmerle, , J. Solid State Chem, 147(2), pp.485~500 (1999)
- O. Matz, , Top. Catal, 62(12-16), pp.956~967 (2019)
- V. Stetsovych, , J. Phys. Chem. Lett, 4(6), pp.866~871 (2013)
- M. García-Melchor, , J. Phys. Chem. C, 118(20), pp.10921~10926 (2014)
- S. Abanades, , Sol. Energy, 80(12), pp.1611~1623 (2006)
- T. Ishida, , Energy Procedia, 49, pp.1970~1979 (2014)
- J. Valle-Hernández, , AIP Conf. Proc, 1734, pp.120008~ (2016)
- J. Höcker, , Nanoscale, 9(27), pp.9352~9358 (2017)
- T. Sata, , J. Ceram. Assoc. Japan, 76(872), pp.116~122 (1968)
- J. L. G. Fierro, , J. Solid State Chem, 66(1), pp.154~162 (1987)
- A. Trovarelli, , Catal. Rev, 38(4), pp.439~520 (1996)
- V. Perrichon, , Appl. Catal. A-Gen, 129(1), pp.69~82 (1995)
- D. J. M. Bevan, , J. Inorg. Nucl. Chem, 26(9), pp.1509~1523 (1964)
- C. M. Hamm, , Z. Anorg. Allg. Chem, 640(6), pp.1050~1053 (2014)
- F. Izumi, , IOP Conf. Ser. : Mater. Sci. Eng, 18(2), pp.022001~ (2011)
- K. Momma, , Z. Kristallogr. Proc, 1, pp.195~200 (2011)
- K. Momma, , Powder Diffr, 28(3), pp.184~193 (2013)
- A. Kumar, , Langmuir, 25(18), pp.10998~11007 (2009)
- M. F. Bekheet, , CrystEngComm, 21(1), pp.145~154 (2019)
- T. Hryniewicz, , Surf. Coat. Technol, 205(17-18), pp.4228~4236 (2011)
- G. Righi, , J. Phys. Chem. C, 123(15), pp.9875~9883 (2019)
- A. Furrer, "Neutron Scattering from Hydrogen in Materials", pp.264~ (1994), World Scientific Press
- V. A. Sadykov, , Open Chem, 14(1), pp.363~376 (2016)
- M. Grünbacher, , Phys. Chem. Chem. Phys, 20(34), pp.22099~22113 (2018)
- D. Mukherjee, , Top Catal., 60(19-20), pp.1673~1681 (2017)
- A. Fujimori, , Phys. Stat. Sol. B, 99(2), pp.673~681 (1980)
- Z. Wu, , Am. Chem. Soc, 139(28), pp.9721~9727 (2017)
- A. M. Chippindale, , J. Solid State Chem, 92(2), pp.526~533 (1991)
- K. -W. Chae, , Sci. Adv. Mater, 8, pp.1~5 (2016)