Hostname: page-component-cd9895bd7-jkksz Total loading time: 0 Render date: 2024-12-24T13:05:31.788Z Has data issue: false hasContentIssue false
  • English
  • Français

Characterisation of the phase-transformation behaviour of Ce2O(CO3)2·H2O clusters synthesised from Ce(NO3)3·6H2O and urea

Published online by Cambridge University Press:  21 November 2014

Anita M. D'Angelo ,
Nathan A. S. Webster  and
Alan L. Chaffee
Anita M. D'Angelo
Affiliation:
CRC for Greenhouse Gas Technologies (CO2CRC), School of Chemistry, Monash University, Clayton, VIC 3800Australia
Nathan A. S. Webster
Affiliation:
CSIRO Mineral Resources Flagship, Private Bag 10, Clayton South, VIC 3169, Australia
Alan L. Chaffee*
Affiliation:
CRC for Greenhouse Gas Technologies (CO2CRC), School of Chemistry, Monash University, Clayton, VIC 3800Australia
*
a)Author to whom correspondence should be addressed. Electronic mail: [email protected]
Get access Rights & Permissions [Opens in a new window]

Abstract

X-ray diffraction (XRD) was used to determine the temperature at which the transformation of Ce2O(CO3)2·H2O to ceria (CeO2) occurs under both a flow of nitrogen and air as a function of temperature. The Ce2O(CO3)2·H2O synthesised from Ce(NO3)3·6H2O and urea was further investigated using thermal gravimetric analysis (TGA), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). XRD results indicate that, under a flow of nitrogen, CeO2 is formed at temperatures greater than 500 °C and that this occurs via an as yet unidentified intermediate phase, which is present between 430 and 540 °C. Results obtained by the XRD correspond to those obtained using TGA, which show weight  losses commencing at 430 and at 465 °C. No further weight loss occurs above 540 °C, because of the formation of CeO2 as the stable product. The crystallite size was also determined and observed to increase with increasing temperature. Under a flow of air the transformation occurred at a lower temperature, as CeO2 was formed at 250 °C. SEM and TEM reveal the particles have a rod-shaped morphology which is retained after calcination. These results may be used to optimise synthesis methods to minimise crystallite size growth and reduce sintering that is undesirable in many applications, particularly catalysis.

Keywords

cerium oxidenanorodsvariable-temperature XRDintermediate
Type
Technical Articles
Information
Powder Diffraction , Volume 29 , Issue S1 , December 2014 , pp. S84 - S88
Check for updates
Copyright
Copyright © International Centre for Diffraction Data 2014 

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

Bruker AXS. (2009). TOPAS V4.2 (computer software), Bruker AXS Inc., Madison, USA.Google Scholar
Chen, P. L. and Chen, I. W. (1993). “Reactive cerium (IV) oxide powders by the homogeneous precipitation method,” J. Am. Ceram. Soc. 76, 1577–1583.Google Scholar
da Costa, L. O., da Silva, A. M., Noronha, F. B., and Mattos, L. V. (2012). “The study of the performance of Ni supported on gadolinium doped ceria SOFC anode on the steam reforming of ethanol,” Int. J. Hydrogen Energy 37, 5930–5939.CrossRefGoogle Scholar
Deraz, N. M. and Alarifi, A. (2009). “Structural, surface and catalytic properties of nano-sized ceria catalysts,” Adsorpt. Sci. Technol. 27, 413–422.Google Scholar
Dong, Q., Yin, S., Guo, C., Wu, X., Kimura, T., and Sato, T. (2013). “Aluminium doped ceria–zirconia supported palladium-alumina catalyst with high oxygen storage capacity and CO oxidation activity,” Mater. Res. Bull. 48, 4989–4992.Google Scholar
Florea, I., Feral-Martin, C., Majimel, J., Ihiawakrim, D., Hirlimann, C., and Ersen, O. (2013). “Three-dimentional tomographic analyses of CeO2 nanoparticles,” Cryst. Growth Des. 13, 1110–1121.Google Scholar
Guan, Y., Ligthart, D. A. J. M., Pirgon-Galin, Ö., Pieterse, J. Z., Santen, R., and Hensen, E. M. (2011). “Gold stabilized by nanostructured ceria supports: nature of the active sites and catalytic performance,” Top. Catal. 54, 424–438.Google Scholar
Harshini, D., Kim, Y., Nam, S. W., Lim, T. H., Hong, S. A., and Yoon, C. W. (2013). “Influence of terbium doping on oxygen storage capacity of ceria–zirconia supports: enhanced durability of Ni catalysts for propane steam reforming,” Catal. Lett. 143, 49–57.CrossRefGoogle Scholar
Hirano, M., and Kato, E. (1999a). “Hydrothermal synthesis of nanocrystalline cerium(IV) oxide powders,” J. Am. Ceram. Soc. 82, 786–788.Google Scholar
Hirano, M., and Kato, E. (1999b). “Hydrothermal synthesis of two types of cerium carbonate particles,” J. Mater. Sci. Lett. 18, 403–405.Google Scholar
Hua, G., Zhang, L., Fei, G., and Fang, M. (2012). “Enhanced catalytic activity induced by defects in mesoporous ceria nanotubes,” J. Mater. Chem. 22, 6851–6855.Google Scholar
ICDD (2010). PDF-2 2010 (Database), edited by Kabekkodu, Soorya (International Centre for Diffraction Data, Newtown Square, PA, USA).Google Scholar
Kašpar, J., Fornasiero, P., and Graziani, M. (1999). “Use of CeO2-based oxides in the three-way catalysis,” Catal. Today 50, 285–298.CrossRefGoogle Scholar
Kearney, J., Hernández-Reta, J. C., and Baker, R. T. (2012). “Redox and catalytic properties of Ce–Zr mixed oxide nanopowders for fuel cell applications,” Catal. Today 180, 139–147.Google Scholar
Liu, Z., Ding, D., Liu, M., Li, X., Sun, W., Xia, C., and Liu, M. (2013). “Highly active Sm0.2Ce0.8O1.9 powders of very low apparent density derived from mixed cerium sources,” J. Power Sources 229, 277–284.Google Scholar
Mai, H. X., Sun, L. D., Zhang, Y. W., Si, R., Feng, W., Zhang, H. P., Liu, H. C., and Yan, C. H. (2005). “Shape-selective synthesis and oxygen storage behavior of ceria nanopolyhedra, nanorods, and nanocubes,” J. Phys. Chem. B 109, 24380–24385.Google Scholar
Mamontov, E., Egami, T., Brezny, R., Koranne, M., and Tyagi, S. (2000). “Lattice defects and oxygen storage capacity of nanocrystalline ceria and ceria–zirconia,” J. Phys. Chem. B 104, 11110–11116.CrossRefGoogle Scholar
Nolan, M., Grigoleit, S., Sayle, D. C., Parker, S. C., and Watson, G. W. (2005a). “Density functional theory studies of the structure and electronic structure of pure and defective low index surfaces of ceria,” Surf. Sci. 576, 217–229.CrossRefGoogle Scholar
Nolan, M., Parker, S. C., and Watson, G. W. (2005b). “The electronic structure of oxygen vacancy defects at the low index surfaces of ceria,” Surface Sci. 595, 223–232.Google Scholar
Oikawa, M., and Fujihara, S. (2005). “Crystal growth of Ce2O(CO3)2·H2O in aqueous solutions: film formation and samarium doping,” J. Solid State Chem. 178, 2036–2041.Google Scholar
Paun, C., Safonova, O. V., Szlachetko, J., Abdala, P. M., Nachtegaal, M., Sa, J., Kleymenov, E., Cervellino, A., Krumeich, F., and van Bokhoven, J. A. (2012). “Polyhedral CeO2 nanoparticles: size-dependent geometrical and electronic structure,” J. Phys. Chem. C 116, 7312–7317.Google Scholar
Revoy, M. N., Scott, R. W. J., and Grosvenor, A. P. (2013). “Ceria nanocubes: dependence of the electronic structure on synthetic and experimental conditions,” J. Phys. Chem. C 117, 10095–10105.Google Scholar
Shannon, R. D. (1976). “Revised effective ionic radii and systematic studies of interatomic distances in halides and chalcogenides,” Acta Crystallogr. A 32, 751–767.Google Scholar
Soykal, I. I., Sohn, H., and Ozkan, U. S. (2012). “Effect of support particle size in steam reforming of ethanol over Co/CeO2 catalysts,” ACS Catal. 2, 2335–2348.CrossRefGoogle Scholar
Sun, M., Zou, G., Xu, S., and Wang, X. (2012). “Nonaqueous synthesis, characterization and catalytic activity of ceria nanorods,” Mater. Chem. Phys. 134, 912–920.Google Scholar
Wang, Z. L. and Feng, X. (2003). “Polyhedral shapes of CeO2 nanoparticles,” J. Phys. Chem. B 107, 13563–13566.Google Scholar
Wu, Z., Li, M., Howe, J., Meyer, H. M., and Overbury, S. H. (2010). “Probing defect sites on CeO2 nanocrystals with well-defined surface planes by Raman spectroscopy and O2 adsorption,” Langmuir 26, 16595–16606.CrossRefGoogle ScholarPubMed
Wu, Z., Schwartz, V., Li, M., Rondinone, A. J., and Overbury, S. H. (2012). “Support shape effect in metal oxide catalysis: ceria-nanoshape-supported vanadia catalysts for oxidative dehydrogenation of isobutane,” J. Phys. Chem. Lett. 3, 1517–1522.CrossRefGoogle ScholarPubMed
Zhou, K., Wang, X., Sun, X., Peng, Q., and Li, Y. (2005). “Enhanced catalytic activity of ceria nanorods from well-defined reactive crystal planes,” J. Catal. 229, 206–212.Google Scholar