Abstract
The paper presents a study on the preparation of Co2SiO4/SiO2 nanocomposites by a new modified sol–gel method. We have prepared gels starting from tetraethylorthosilicate (Si(OC2H5)4), cobalt nitrate Co(NO3)2·6H2O and some diols: ethylene glycol (C2H6O2), 1,2propanediol (C3H8O2) and 1,3propanediol (C3H8O2), for a final composition: 30% CoO/70% SiO2. During the heating of the gels at 140 °C, a redox reaction takes place between NO3 − ions and diol with formation of some carboxylate anions. These carboxylate anions react with the Co(II) ions to form coordination compounds embedded in silica matrix, as evidenced by FT-IR spectrometry and thermal analysis. These Co(II) coordinative compounds thermally decompose in the range 250–300 °C to the corresponding oxides: CoO and/or Co3O4 inside the matrices pores. When CoO results, it reacts with SiO2 at low temperature leading to Co2SiO4, which crystallizes at 700 °C. XRD patterns of the samples annealed at temperatures lower than 700 °C were characteristic to amorphous phases. The samples annealed at temperatures ≥700 °C, contain Co2SiO4 (olivine) as unique crystalline phase inside the amorphous silica matrix, according to XRD patterns. As evidenced by TEM images, Co2SiO4 nanoparticles are homogenously dispersed inside the silica matrix.
Similar content being viewed by others
References
Lin H-K, Chiu H-C, Tsai H-C, Chien S-H, Wang C-B (2003) Synthesis, characterization and catalytic oxidation of carbon monoxide over cobalt oxide. Catal Lett 88:169–174
Ortega G, Araujo-Andrade C, Compean-Jasso ME, Martinez JR, Ruiz F (2002) Cobalt oxide/silica xerogels powders: X-ray diffraction, infrared and visible absorption studies. J Sol-Gel Sci Tech 24:23–29
Martucci A, Busso D, Guglielmi M, Zbroniec L, Koshizaki N, Post M (2004) Optical gas sensing properties of silica film doped with cobalt oxide nanocrystals. J Sol-Gel Sci Tech 32:243–246
Cui H, Zayat M, Levi D (2006) Effect of HCl on the PPO assisted sol-gel synthesis of olivine-type Co2SiO4 ultrafine particles. J Sol-Gel Sci Techn 40:83–87
Yan J, Buckley AM, Greenblatt M (1995) The preparation and characterization of silica gels doped with copper complexes. J Non-Cryst Solids 180:180–190
Esposito S, Turco M, Ramis G, Bagnasco G, Pernice P, Pagliuca C, Bevilacqua M, Aronne A (2007) Cobalt-silicon mixed oxide nanocomposites by modified sol-gel method. J Solid State Chem 180:3341–3350
Taguchi H, Takeda Y, Shibahara H (2002) Synthesis of olivine-type Co1.6SiO4 at low temperature. Mat Lett 52:412–416
Stefanescu M, Dippong T, Stoia M, Stefanescu O (2008) Study on the obtaining of cobalt oxides by thermal decomposition of some complex combinations, undispersed and dispersed in SiO2 matrix. J Therm Anal Cal 94:389–393
Stefanescu M, Stoia M, Stefanescu O, Popa A, Simon M, Ionescu C (2007) The interaction between teos and some polyols. Thermal analysis and FTIR. J Therm Anal Cal 88:19–26
Brinker CJ, Scherrer GW (1990) Sol-gel science: the physics and chemistry of sol-gel Processing. Academic Press, New York
Lenza RFS, Vasconcelos WL (2003) Study of the influence of some DCCAs on the structure of sol–gel silica membranes. J Non-Cryst Solids 330:216
Ocotlan-Flores J, Saniger JM (2006) Catalyst-free SiO2 sonogels. J Sol-Gel Sci Techn 39:235–240
Shinde VR, Mahadik SB, Gujar TP, Lokhande CD (2006) Supercapacitive cobalt oxide (C03O4) thin films by spray pyrolysis. Appl Surf Sci 252:7487–7492
Joint Committee on Powder Diffraction Standards-International Center for Diffraction Data (1999)
Stefanescu M, Stoia M, Stefanescu O (2007) The interaction between TEOS and some polyols. Thermal analysis and FT-IR. J Sol-Gel Sci Techn 41:71–78
Acknowledgments
This work was supported by the National Project No. 71-026 NANOPART and financed by CNMP-ANCS through Romanian Ministry of Education and Research.
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Stoia, M., Stefanescu, M., Dippong, T. et al. Low temperature synthesis of Co2SiO4/SiO2 nanocomposite using a modified sol–gel method. J Sol-Gel Sci Technol 54, 49–56 (2010). https://doi.org/10.1007/s10971-010-2156-2
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s10971-010-2156-2