Study of Gel Growth Cobalt (II) Oxalate Crystals as Precursor of Co3O4 Nano Particles

*Yuniar Ponco Prananto -  Department of Chemistry, Faculty of Mathematics and Natural Sciences, Brawijaya University, Jl. Veteran 01 Malang, 65145, Indonesia
Mohammad Misbah Khunur -  Department of Chemistry, Faculty of Mathematics and Natural Sciences, Brawijaya University, Jl. Veteran 01 Malang, 65145, Indonesia
Dini Tri Wahyuni -  Department of Chemistry, Faculty of Mathematics and Natural Sciences, Brawijaya University, Jl. Veteran 01 Malang, 65145, Indonesia
Rizky Arief Shobirin -  Department of Chemistry, Faculty of Mathematics and Natural Sciences, Brawijaya University, Jl. Veteran 01 Malang, 65145, Indonesia
Yoga Rizky Nata -  Department of Chemistry, Faculty of Mathematics and Natural Sciences, Brawijaya University, Jl. Veteran 01 Malang, 65145, Indonesia
Efiria Riskah -  Department of Chemistry, Faculty of Mathematics and Natural Sciences, Brawijaya University, Jl. Veteran 01 Malang, 65145, Indonesia
Received: 25 Oct 2012; Published: 9 Feb 2013.
Open Access
Citation Format:
bcrec_4066
Article Info
Section: Original Research Articles
Language: EN
Full Text:
Statistics: 1346 895
Abstract

Crystal growth of cobalt (II) oxalate in silica gel at room temperature as precursor of Co3O4 nano particles has been studied. Specifically, this project is focusing on the use of two different reaction tube types toward crystallization of cobalt (II) oxalate in gel. The gel was prepared at pH 5 by reacting sodium metasilicate solution with dilute nitric acid (for U-tube) and oxalic acid (for straight tube), with gelling time of 4 days and crystal growth time of 8 (for straight tube) and 12 (for U-tube) weeks. Result shows that pink crystalline powder was directly formed using straight tube method. The use of different solvents in straight tube method affects crystallization and could delay direct precipitation of the product. In contrast, bigger and better shape of red block crystal was yielded from U-tube method; however, longer growth time was needed. FTIR studies suggest that both growth method produces identical compound of hydrated cobalt (II) oxalate. © 2013 BCREC UNDIP. All rights reserved

Received: 25th October 2012; Revised: 30th November 2012; Accepted: 5th December 2012

[How to Cite: Y.P. Prananto, M.M. Khunur, D.T. Wahyuni, R.A. Shobirin, Y.R. Nata, E. Riskah, (2013). Study of Gel Growth Cobalt (II) Oxalate Crystals as Precursor of Co3O4 Nano Particles. Bulletin of Chemical Reaction Engineering & Catalysis, 7 (3): 198-204. (doi:10.9767/bcrec.7.3.4066.198-204)]

[Permalink/DOI: http://dx.doi.org/10.9767/bcrec.7.3.4066.198-204 ]

View in  |

Keywords
cobalt (II) oxalate; silica gel; reaction tube type; nano particles

Article Metrics:

  1. Singh, B. P. and Singh, B. (2000). Synthesis and Magnetic Properties of One-Dimensional Metal Oxalate Networks as Molecular-Based Magnets. Bulletin of Material Science, 23(1): 11–16. CrossRef
  2. Mullens, J., Vos, A., De Backer, A., Franco, D., Yperman, J., and Van Poucke, L. C. (1993). The Decomposition of the Oxalate Precursor and The Stability and Reduction of the YBa2Cu4O8 Superconductor Studied by TG Coupled with FTIR and by XRD. Journal of Thermal Analysis and Calorimetry, 40(1): 303-311 CrossRef
  3. Gabal, M.A., Hameed, S.A., and Obaid, A.Y. (2012). CoTiO3 via Cobalt Oxalate–TiO2 Precursor, Synthesis and Characterization. Materials Characterization, 71: 87-94. CrossRef
  4. Wang, D., Wang, Q., and Wang, T. (2011). Morphology-Controllable Synthesis of Cobalt Oxalates and Their Conversion to Mesoporous Co3O4 Nanostructures for Application in Supercapacitors. Inorganic Chemistry, 50; 6482–6492. CrossRef
  5. Ahmed, J., Ahmad, T., Ramanujachary, K.V., Lofland, S.E., and Ganguli, A.K. (2008). Development of A Microemulsion-Based Process for Synthesis of Cobalt (Co) and Cobalt Oxide (Co3O4) Nanoparticles from Submicrometer Rods of Cobalt Oxalate. Journal of Colloid and Interface Science, 321(2): 434–441. CrossRef
  6. Thota, S., Kumar, A., and Kumar, J. (2009). Optical, Electrical and Magnetic Properties of Co3O4 Nanocrystallites Obtained by Thermal Decomposition of Sol–Gel Derived Oxalates. Materials Science and Engineering: B, 164(1): 30–37. CrossRef
  7. Salavati-Niasari, M., Mir, N., and Davar, F. (2009). Synthesis and Characterization of Co3O4 Nanorods by Thermal Decomposition of Cobalt Oxalate. Journal of Physics and Chemistry of Solids, 70(5): 847–852. CrossRef
  8. Liu, B., Peng, J., Zhang, L., Wan, R., Guo, S., and Zhou, L. (2010). Optimization of Preparation for Co3O4 by Calcination from Cobalt Oxalate using Response Surface Methodology. Chemical Engineering Research and Design, 88(8): 971–976. CrossRef
  9. De Rivas, B., López-Fonseca, R., Jiménez-González, C., and Gutiérrez-Ortiz, J.I. (2012). Highly Active Behavior of Nanocrystalline Co3O4 from Oxalate Nanorods in the Oxidation of Chlorinated Short Chain Alkanes. Chemical Engineering Journal, (184): 184–192. CrossRef
  10. Yang, Y., Huang, K., Liu R., Wang, L., Zeng, W., and Zhang P. (2007). Shape-controlled Synthesis of Nanocubic Co3O4 by Hydrothermal Oxidation Method. Transactions of Nonferrous Metals Society of China, 17(5): 1082–1086. CrossRef
  11. Cheng, J.P., Chen, X., Ma, R., Liu, F., and Zhang, X.B. (2011). A Facile Method to Fabricate Porous Co3O4 Hierarchical Microspheres. Materials Characterization, 62(8): 775–780. CrossRef
  12. Bacsa, J., Eve, D., and Dunbar, K. R. (2005). Catena-poly[[diaquacobalt(II)]-μ-oxalato]. Acta Crystallographica, C61: m58–m60. CrossRef
  13. Bowen, P., Pujol, O., Jongen, N., Lemaitre, J., Fink, A., Stadleman, P., Hofmann, H. (2010). Control of Morphology and Nanostructure of Copper and Cobalt Oxalates: Effect of Complexing Ions, Polymeric Additives and Molecular Weight. Nanoscale, 2: 2470–2477. CrossRef
  14. Baco-Charles, V., Arnal, A., Poquillon, D. and Tailhades, P. (2008). Correlation between the Morphology of Cobalt Oxalate Precursors and the Microstructure of Metal Cobalt Powders and Compacts. Powder Technology, 185(3): 231–238. CrossRef
  15. Liu, Z., Liu, Z., Li, Q., Yang, T., and Zhang, D. (2011). Formation Mechanism of Fibrous Cobalt Oxalate Precipitated from Alkaline Co2+–NH3–C2O42−–H2O System. Materials Chemistry and Physics, 131(1–2): 102–107. CrossRef
  16. Khan, A.S., Devore, T.C., and Reed, W.F. (1976). Growth of the Transition Metal Oxalates in Gels, Journal of Crystal Growth, 35(3): 337–339. CrossRef
  17. Khunur, M. M., Wahyuni, D. T., and Prananto, Y. P. (2011). Synthesis of Lead(II) Oxalate Hydrate (PbC2O4.xH2O) Crystal in Silica Gel. Advances in Natural and Applied Science, 5(5): 467-472. View at Publisher
  18. Raj, A.M.E., Jayanthi, D.D., and Jothy, V.B. (2008). Optimized Growth and Characterization of Cadmium Oxalate Single Crystals in Silica Gel. Solid State Sciences, 10: 557–562. CrossRef
  19. Henisch, H. K. (1988). Crystal in Gel and Liesegang Rings. Australia: Cambridge, University Press.
  20. Shajan, X. S. and Mahadevan, C. (2004). On the Growth of Calcium Tartrate Tetrahydrate Single Crystal. Bulletin of Material Science, 27(4): 327–331. CrossRef
  21. Lide, D. R. (2010). CRC Handbook of Chemistry and Physics, 90th ed. Boca Raton, Florida: CRC Press.