Preparation of Gd2O3 Ultrafine Nanoparticles by Pulse Electrodeposition Followed by Heat-treatment Method

Document Type: Research Paper


Nuclear Fuel Cycle Research School (NFCRS), Nuclear Science and Technology Research Institute, Tehran.


Gd2O3 nanoparticles were prepared by a two–step process; cathodic electrodeposition followed by heat-treatment method. First, Gd(OH)3 nanoparticles was galvanostatically deposited from nitrate bath on the steel substrate by pulse current (PC) mode. The deposition experiments was conducted at a typical on-time and off-time (ton=1ms and toff=1ms) for 60 min. The electrodeposited precursor was then heat-treated at 600 oC for 3h to obtain oxide product (i.e. Gd2O3). The morphological and structural analyses confirmed that the gadolinium hydroxynitrate nanoparticles with composition of [Gd(OH)2.5(NO3)0.5 yH2O] and uniform size about 10 nm have been prepared during pulse cathodic electrodeposition process. Furthermore, mechanism of the gadolinium hydroxynitrate nanoparticles was explained based on the base (OH–) electrogeneration process on the cathode surface. The morphological observations by SEM and TEM, and structural analyses via XRD and FT-IR revealed that the oxide product is composed of well-dispersed Gd2O3 nanoparticles with pure cubic crystalline structure. It was observed that the calcination process has no effect on the morphology of the Gd2O3 nanoparticles. Mechanism of oxide formation during heat-treatment step was investigated by DSC-TG analysis and discussed in detail. The results of this work showed that pulse current deposition followed by heat–treatment can be recognized as an easy and facile method for preparation of the Gd2O3 fine nanoparticles.


1. Beek WJ, Wienk MM, Janssen RA. Efficient hybrid solar cells from zinc oxide nanoparticles and a conjugated polymer. Advanced Materials. 2004;16(12):1009-13.
2. Oskam G. Metal oxide nanoparticles: synthesis, characterization and application. Journal of Sol-Gel Science and Technology. 2006;37(3):161-4.
3. Tsuzuki T, Pirault E, McCormick PG. Mechanochemical synthesis of gadolinium oxide nanoparticles. Nanostructured Materials. 1999;11(1):125-31.
4. Colussi S, de Leitenburg C, Dolcetti G, Trovarelli A. The role of rare earth oxides as promoters and stabilizers in combustion catalysts. Journal of Alloys and Compounds. 2004;374(1):387-92.
5. Chang C, Kimura F, Kimura T, Wada H. Preparation and characterization of rod-like Eu: Gd2O3 phosphor through a hydrothermal routine. Materials Letters. 2005;59(8):1037-41.
6. Garcıa-Murillo A, Le Luyer C, Garapon C, Dujardin C, Bernstein E, Pedrini C, Mugnier J. Optical properties of europium-doped Gd2O3 waveguiding thin films prepared by the sol–gel method. Optical Materials. 2002;19(1):161-8.
7. Bhattacharyya S, Agrawal DC. Preparation of tetragonal ZrO2- Gd2O3 powders. Journal of Materials Science. 1995;30(6):1495-9.
8. Chen Z. Effects of gadolinia and alumina addition on the densification and toughening of silicon carbide. Journal of the American Ceramic Society. 1996;79(2):530-2.
9. Babić-Stojić B, Jokanović V, Milivojević D, Požek M, Jagličić Z, Makovec D, Arsikin K, Paunović V. Gd2O3 nanoparticles stabilized by hydrothermally modified dextrose for positive contrast magnetic resonance imaging. Journal of Magnetism and Magnetic Materials. 2016;403:118-26.
10. Fang J, Chandrasekharan P, Liu XL, Yang Y, Lv YB, Yang CT, Ding J. Manipulating the surface coating of ultra-small Gd2O3 nanoparticles for improved T 1-weighted MR imaging. Biomaterials. 2014;35(5):1636-42.
11. Faucher L, Guay‐Bégin AA, Lagueux J, Côté MF, Petitclerc É, Fortin MA. Ultra‐small gadolinium oxide nanoparticles to image brain cancer cells in vivo with MRI. Contrast Media & Molecular Imaging. 2011;6(4):209-18.
12. Dehno Khalaji A. Nickel Oxide (NiO) nanoparticles prepared by solid-state thermal decomposition of Nickel (II) schiff base precursor. Journal of Ultrafine Grained and Nanostructured Materials. 2015;48(1):1-4.
13. Farahmandjou M, Zarinkamar M. Synthesis of nano-sized ceria (CeO2) particles via a cerium hydroxy carbonate precursor and the effect of reaction temperature on particle morphology. Journal of Ultrafine Grained and Nanostructured Materials. 2015;48(1):5-10.
14. Khadivi Ayask H, Vahdati Khaki J, Haddad Sabzevar M. Facile synthesis of copper oxide nanoparticles using copper hydroxide by mechanochemical process. Journal of Ultrafine Grained and Nanostructured Materials. 2015;48(1):37-44.
15. Dhananjaya N, Nagabhushana H, Nagabhushana BM, Rudraswamy B, Sharma SC, Sunitha DV, Shivakumara C, Chakradhar RP. Effect of different fuels on structural, thermo and photoluminescent properties of Gd2O3 nanoparticles. Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy. 2012;96:532-40.
16. Rahman AA, Vasilev K, Majewski P. Ultra small Gd2O3 nanoparticles: absorption and emission properties. Journal of Colloid and Interface Science. 2011;354(2):592-6.
17. Yang S, Gao H, Wang Y, Xin S, He Y, Wang Y, Zeng W. A simple way to synthesize well-dispersed Gd2O3 nanoparticles onto reduced graphene oxide sheets. Materials Research Bulletin. 2013;48(1):37-40.
18. Abed F, Aghazadeh M, Arhami B. Preparation of Gd2O3 coral-like nanostructures by pulse electrodeposition–heat-treatment method. Materials Letters. 2013;99:11-3.
19. Aghazadeh M, Yousefi T. Preparation of Gd2O3 nanorods by electrodeposition–heat-treatment method. Materials Letters. 2012;73:176-8.
20. Poudret L, Prior TJ, McIntyre LJ, Fogg AM. Synthesis and crystal structures of new lanthanide hydroxyhalide anion exchange materials, Ln2(OH)5X·1.5H2O(X= Cl, Br; Ln= Y, Dy, Er, Yb). Chemistry of Materials. 2008;20(24):7447-53.
21. Hindocha SA, McIntyre LJ, Fogg AM. Precipitation synthesis of lanthanide hydroxynitrate anion exchange materials, Ln2(OH)5NO3· H2O (Ln= Y, Eu–Er). Journal of Solid State Chemistry. 2009;182(5):1070-4.
22. McIntyre LJ, Jackson LK, Fogg AM. Ln2(OH)5NO3· xH2O(Ln= Y, Gd− Lu): A Novel Family of Anion Exchange Intercalation Hosts. Chemistry of Materials. 2007;20(1):335-40.
23. Fogg AM, Williams GR, Chester R, O’Hare D. A novel family of layered double hydroxides—[MAl4(OH)12](NO3)2 .xH2O (M= Co, Ni, Cu, Zn). Journal of Materials Chemistry. 2004;14(15):2369-71.
24. Louett M, Louer D. The structures of lanthanum hydroxide nitrates investigated by the Rietveltl profile refinement technique. European Journal of Solid State Inorganic Chemistry. 1989;26:241.
25. Kang JG, Min BK, Sohn Y. Synthesis and characterization of Gd(OH)3 and Gd2O3 nanorods. Ceramics International. 2015;41(1):1243-8.
26. Schildermans I, Mullens J, Van der Veken BJ, Yperman J, Franco D, Van Poucke LC. Preparation and thermal decomposition of Cu2(OH)3NO3. Thermochimica Acta. 1993;224:227-32.