A Simple Chemical Precipitation Method of Titanium Dioxide Nanoparticles Using Polyvinyl Pyrrolidone as a Capping Agent and Their Characterization

Authors: V. P. Muhamed Shajudheen, K. Viswanathan, K. Anitha Rani, A. Uma Maheswari, S. Saravana Kumar

Abstract:

In this paper, a simple chemical precipitation route for the preparation of titanium dioxide nanoparticles, synthesized by using titanium tetra isopropoxide as a precursor and polyvinyl pyrrolidone (PVP) as a capping agent, is reported. The Differential Scanning Calorimetry (DSC) and Thermo Gravimetric Analysis (TGA) of the samples were recorded and the phase transformation temperature of titanium hydroxide, Ti(OH)₄ to titanium oxide, TiO₂ was investigated. The as-prepared Ti(OH)₄ precipitate was annealed at 800°C to obtain TiO₂ nanoparticles. The thermal, structural, morphological and textural characterizations of the TiO₂ nanoparticle samples were carried out by different techniques such as DSC-TGA, X-Ray Diffraction (XRD), Fourier Transform Infra-Red spectroscopy (FTIR), Micro Raman spectroscopy, UV-Visible absorption spectroscopy (UV-Vis), Photoluminescence spectroscopy (PL) and Field Effect Scanning Electron Microscopy (FESEM) techniques. The as-prepared precipitate was characterized using DSC-TGA and confirmed the mass loss of around 30%. XRD results exhibited no diffraction peaks attributable to anatase phase, for the reaction products, after the solvent removal. The results indicate that the product is purely rutile. The vibrational frequencies of two main absorption bands of prepared samples are discussed from the results of the FTIR analysis. The formation of nanosphere of diameter of the order of 10 nm, has been confirmed by FESEM. The optical band gap was found by using UV-Visible spectrum. From photoluminescence spectra, a strong emission was observed. The obtained results suggest that this method provides a simple, efficient and versatile technique for preparing TiO₂ nanoparticles and it has the potential to be applied to other systems for photocatalytic activity.

Keywords: TiO2 nanoparticles, chemical precipitation route, phase transition, Fourier Transform Infra-Red spectroscopy, micro Raman spectroscopy, UV-Visible absorption spectroscopy, Photoluminescence spectroscopy, Field Effect Scanning Electron Microscopy.

Digital Object Identifier (DOI): doi.org/10.5281/zenodo.1124139

References:

[1] A. Zaleska, “Doped-TiO2: A review,” Recent Patents on Engineering, vol. 2, no. 3, pp. 157–164, 2008.
[2] Y. Xie, Y. Qian, Y. Zhong, H. Guo, and Y. Hu, “Facile low-temperature synthesis of carbon nanotube/TiO2 nanohybrids with enhanced visible-light-driven photocatalytic activity,” International Journal of Photoenergy, vol. 2012, Article ID 682138, 6 pages, 2012.
[3] F. Sayilkan, M. Asilturk, H. Sayilkan, Y. Onal, M. Akarsu, and E. Arpaç, “Characterization of TiO2 synthesized in alcohol by a sol-gel process: the effects of annealing temperature and acid catalyst,” Turkish Journal of Chemistry, vol. 29, no. 6, pp. 697–706, 2005.
[4] R. Gomez, T. Lopez, and E. Ortiz-Islas, “Effect of sulfation on the photoactivity of TiO2 sol-gel derived catalysts,” Journal of Molecular Catalysis A, vol. 193, no. 1-2, pp. 217–226, 2003.
[5] M. Umadevi, R. Parimaladevi, and M. Sangari, “Synthesis, characterization and photocatalytic activity of fluorine doped TiO2 nanoflakes synthesized using solid state reaction method,” Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy, vol. 120, no.5, pp. 365–369, 2014.
[6] Z. Liu, Z. Jian, J. Fang, X. Xu, X. Zhu, and S. Wu, “Low temperature reverse microemulsion synthesis, characterization and photocatalytic performance of nanocrystalline titanium dioxide,” International Journal of Photoenergy, vol. 2012, Article ID 702503, 8 pages, 2012.
[7] D. Byun, Y. Jin, B. Kim, J. Kee Lee, and D. Park, “Photocatalytic TiO2 deposition by chemical vapor deposition,” Journal of Hazardous Materials, vol.73, no. 4, pp.199-206, 2000.
[8] K. K. Gupta, M. Jassal, and A. K. Agrawal, “Sol-gel derived titanium dioxide finishing of cotton fabric for self cleaning,” Indian Journal of Fibre and Textile Research, vol. 33, no. 4, pp. 443–450, 2008.
[9] F. Cardarelli, Materials Handbook: A Concise Desktop Reference, 2nd edition, 2008.
[10] X. Chen and S. S. Mao, “Titanium dioxide nanomaterials: synthesis, properties, modifications and applications,” Chemical Reviews, vol. 107, no. 7, pp. 2891–2959, 2007.
[11] M. Lal, V. Chhabra, P. Ayyub, and A. Maitra, “Preparation and characterization of ultrafine TiO2 particles in reverse micelles by hydrolysis of titanium di-ethylhexyl sulfosuccinate,” Journal of Materials Research, vol. 13, no. 5, pp. 1249–1254, 1998.
[12] R. R. Basca and M. Gratzel, “Rutile formation in hydrothermally crystallized nanosized titania,” Journal of the American Ceramic Society, vol. 79, no. 8, pp. 2185–2188, 1996.
[13] T. R. N. Kutty, R. Vivekanandan, and P. Murugaraj, “Precipitation of rutile and anatase (TiO2) fine powders and their conversion to MTiO3 (M = Ba, Sr, Ca) by the hydrothermal method,” Materials Chemistry and Physics, vol. 19, no. 6, pp. 533–546, 1988.
[14] L. K. Campbell, B. K. Na, and E. I. Ko, “Synthesis and characterization of titania aerogels,” Chemistry of Materials, vol. 4, no. 6, pp. 1329–1333, 1992.
[15] A. V. Prasada Rao, A. I. Robin, and S. Komarneni, “Bismuth titanate from nanocomposite and sol-gel processes,” Materials Letters, vol. 28, no. 4–6, pp. 469–473, 1996.
[16] E. Scolan, C. Sanchez, Synthesis and characterization of surface-protected nanocrystalline titania particles, Chem. Mater. 10 (1998) 3217–3223.
[17] N. Steunou, F. Robert, K. Boubekeur, F. Ribot, C. Sanchez, Synthesis through an in situ esterification process and characterization of oxo isopropoxo titanium clusters, Inorg. Chim. Acta 279 (1998) 144–151.
[18] F. Bosc, P. Lacroix-Desmazes, A. Ayral, TiO2 anatase-based membranes with hierarchical porosity and photocatalytic properties, J. Colloid Interface Sci. 304 (2006) 545–548.
[19] C. Wang, Z.X. Deng, Y. Li, The synthesis of nanocrystalline anatase and rutile titania in mixed organic media, Inorg. Chem. 40 (2001) 5210–5214.