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

• Published in: International nano letters 2021-09, Vol.11 (3), p.241-261
• Main Authors: Mustapha, S., Tijani, J. O., Ndamitso, M. M., Abdulkareem, A. S., Shuaib, D. T., Amigun, A. T., Abubakar, H. L.
• Format: Article
• Language: English
• Subjects: Anatase; Chemistry and Materials Science; Crystallites; Electron diffraction; Fourier transforms; High resolution; High resolution electron microscopy; Infrared spectroscopy; Lattice strain; Lattice vibration; Materials Science; Microscopy; Morphology; Nanochemistry; Nanoparticles; Nanoscale Science and Technology; Nanotechnology; Original Article; Oxidation; Photoelectrons; Photomicrographs; Sodium hydroxide; Sol-gel processes; Spectrum analysis; Stirring; Titanium; Titanium dioxide; Vibration mode; X ray photoelectron spectroscopy; X-ray diffraction
• ISSN: 2008-9295; 2228-5326
• DOI: 10.1007/s40089-021-00338-w

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