10.1007/s40089-021-00338-w

Facile synthesis and characterization of TiO2 nanoparticles: X-ray peak profile analysis using Williamson–Hall and Debye–Scherrer methods

  • S. Mustapha*1,
  • J. O. Tijani1,
  • M. M. Ndamitso1,
  • A. S. Abdulkareem2,
  • D. T. Shuaib3,
  • A. T. Amigun4,
  • H. L. Abubakar5,
  1. Department of Chemistry, Federal University of Technology, Minna, NG Nanotechnology Research Group, Center for Genetic Engineering and Biotechnology, Federal University of Technology, Minna, Niger State, NG
  2. Department of Chemical Engineering, Federal University of Technology, Minna, Niger State, NG Nanotechnology Research Group, Center for Genetic Engineering and Biotechnology, Federal University of Technology, Minna, Niger State, NG
  3. Department of Chemistry, Illinois Institute of Technology, Chicago, IL, 60616, US
  4. Department of Chemical and Geological Sciences, Al-Hikmah University, Ilorin, NG
  5. Department of Chemistry, Nile University of Nigeria, Abuja, NG

Published in Issue 2021-04-27

How to Cite

Mustapha, S., Tijani, J. O., Ndamitso, M. M., Abdulkareem, A. S., Shuaib, D. T., Amigun, A. T., & Abubakar, H. L. (2021). Facile synthesis and characterization of TiO2 nanoparticles: X-ray peak profile analysis using Williamson–Hall and Debye–Scherrer methods. International Nano Letters, 11(3 (September 2021). https://doi.org/10.1007/s40089-021-00338-w
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Abstract

Abstract In this study, TiO 2 nanoparticles were synthesized by a sol–gel method involving the interaction of the titanium isopropoxide precursor and sodium hydroxide followed by calcination at a temperature of 450 °C. The effects of stirring time and solution pH on the morphology, phase types and crystallite sizes were investigated. The prepared TiO 2 nanoparticles were characterized using X-ray diffraction analysis (XRD), high resolution scanning electron microscopy (HRSEM), high-resolution transmission electron microscopy (HRTEM), selective area electron diffraction (SAED), X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared spectroscopy (FTIR). The HRSEM/HRTEM micrograph showed the formation of well distinct TiO 2 nanoparticles with spherical shapes except at pH 2. FTIR spectroscopy showed the presence of the Ti–O stretching modes and Ti–O–Ti vibration modes in the samples. Crystallite size and lattice strain at peak broadening of TiO 2 nanoparticles were studied using Williamson–Hall analysis and Scherrer’s equation. It was found that W–H crystallite sizes were significantly different from the sizes obtained from Scherrer’s equation at basic medium (pH 8–12) under the applied conditions of stirring time and solution pH for TiO 2 nanoparticles. XRD pattern demonstrated the formation of pure anatase phase of TiO 2 irrespective of the solution pH and stirring time. XPS analysis showed the existence of the Ti 2p orbital in the oxidation states of + 4. The study demonstrated that stirring time and solution pH determined the crystallite sizes and not the phase types. Graphic abstract

Keywords

  • TiO2 nanoparticles,
  • Williamson–Hall,
  • Debye Scherrer,
  • Crystalline size,
  • Reflection peaks

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