Synthesis and Characterisation of Pure Zirconium Oxide (ZrO2) Nanoparticle by Conventional Precipitation Method

In this paper, the synthesis of Zirconium oxide (ZrO2) nanoparticles was carried out by the Conventional precipitation method. Ultraviolet, visible spectroscopy (UV-Vis), and dynamic light scattering analysis (DLS) were performed to find the particles' bandgap and size. Fourier transform infrared spectroscopy (FT-IR) observed the characteristic bands of Zirconium oxide nanoparticles. Dynamic light scattering analysis showed that the size of the particle was found to be 119 nm.

X-ray fluorescence determination of small quantities of hafnium in nuclear pure zirconium materials

An important chemical impurity in the composition of zirconium materials for nuclear power engineering is hafnium, the content of which should not exceed 0.05 and 0.01% for domestic and foreign alloy grades, respectively. Hafnium, being an analogue of zirconium in its chemical properties, is difficult to be analyzed using classical methods of analytical chemistry. Among the physical methods, the X-ray fluorescence method is the most expressive, which is important in conditions of continuous production. The method of X-ray fluorescence for measuring the content of hafnium in zirconium-containing material has been tested on the example of potassium fluorozirconate, a precursor for obtaining alloys. With various combinations of crystal analyzers, detectors, and collimators of the wave-dispersive spectrometer, the ratios of the intensities of the analytical lines of Hf and Zr in the second order of reflection were refined, and the degree of decrease in the fluorescence intensity of those lines was determined. The X-ray fluorescence spectra of hafnium lines in potassium fluorozirconate at the content characteristic of nuclear-pure zirconium are studied. The possibility of recording the intensity of the Hf analytical lines and methods of eliminating the interference from the Zr lines in the second order of reflection are considered. The metrological characteristics are calculated for Hf analytical lines. It is shown that the smallest error and the lowest detection limit (0.001%) is provided when using the HfLβ1 line at certain settings of the wave-dispersive spectrometer, including the X-ray tube operation mode, a combination of a crystal analyzer, a detector and a collimator, as well as the amplitude discriminator settings. The method of accounting for the background is recommended. The proposed method of hafnium determination is applicable to the materials with a constant content of zirconium.

Insight of precursor concentration, particle size and band gap of zirconia nanoparticles synthesized by co-precipitation method

Zirconia (ZrO2), an inorganic material, is a very fascinating material due to its high mechanical strength and fracture toughness. The synthesis is carried out by using co-precipitation method using optimum content of zirconium oxychloride octahydrate (ZrOCl2.8H2O) with NaOH solution at calcination temperature of 700°C. The synthesized samples were characterized to ensure structural, functional, morphological and chemical composition by several techniques. The monoclinic structure has been confirmed from XRD, SAED and Raman spectra. The Zr-O stretching vibration and Zr-O2-Zr bending vibrations were confirmed through FTIR analysis. The well dispersed particles with spherical morphology were established through SEM and TEM analyses. EDX spectra confirmed the formation of pure zirconium oxide. The band gap was calculated with the help of UV-Vis spectra and particle size was determined form XRD data using Debye Scherrer’s equation. The variation of band gap and particle size compared with different concentrations of precursor solution was studied. BIBECHANA 18 (2021) 1-9