A facile thermal-treatment route was successfully used to synthesize ZnO nanosheets. Morphological, structural, and optical properties of obtained nanoparticles at different calcination temperatures were studied using various techniques. The FTIR, XRD, EDX, SEM and TEM images confirmed the formation of ZnO nanosheets through calcination in the temperature between 500 to 650°C. The SEM images showed a morphological structure of ZnO nanosheets, which inclined to crumble at higher calcination temperatures. The XRD and FTIR spectra revealed that the samples were amorphous at 30°C but transformed into a crystalline structure during calcination process. The average particle size and degree of crystallinity increased with increasing calcination temperature. The estimated average particle sizes from TEM images were about 23 and 38 nm for the lowest and highest calcination temperature i.e. 500 and 650°C, respectively. The optical properties were determined by UV–Vis reflection spectrophotometer and showed a decrease in the band gap with increasing calcination temperature.
In this research, a thermal treatment method was used to synthesize cadmium oxide nanoparticles. The metal precursor, cadmium nitrate and a capping agent were dissolved in deionized water, which later was dried and crushed into powder. The powder underwent calcination treatment of 500, 550, 600, and 650 °C to crystallize the nanoparticles and to remove organic compounds. The structural studies of CdO nanoparticles have been carried out using EDAX, FTIR, XRD, SEM and TEM. The FTIR and XRD spectra showed that the crystalline structure formation of metal oxide nanoparticles has only occurred after been exposed to calcination. The optical properties which were determined using a UV-vis spectrophotometer showed a decrease in the band gap with increasing calcination temperature. These results prove that the thermal treatment method is a simple technique that can produce pure metal oxide nanoparticles with no other chemicals added.
a b s t r a c tClose-packed cubic copper ferrites (CuFe 2 O 4 ) nanoparticles were synthesized using an effective thermaltreatment method directly from an aqueous solution containing copper and iron nitrates as metal precursors and poly(vinyl pyrrolidone) as a capping agent. The FTIR spectra of the calcined samples revealed the vibration bands of Fe-O and Cu-O at 315 and 535 nm respectively. The structural, morphological, optical and magnetic properties of the nanocrystal powder samples were analyzed using various characterization techniques. The powder X-ray diffraction unveiled the formation of spinel phase of CuFe 2 O 4 with the average particle size determined from TEM images increased from 24 to 34 nm at the calcination temperatures between 773 and 1173 K. The band gap calculated using Kubelka-Munk function from the UV-visible diffuse reflectance spectra decreased from 2.64 to 2.45 eV with increasing calcination temperature. The electron spin resonance (ESR) spectroscopy confirmed the presence of unpaired electrons in the calcined samples. The g-factor increased from 2.10497 to 2.57056 and the resonance magnetic field decreased from 3.11599 Â 10 À 7 to 2.55161 Â 10 À 7 A/m with increasing calcination temperature.
SnO2 nanoparticle production using thermal treatment with tin(II) chloride dihydrate and polyvinylpyrrolidone capping agent precursor materials for calcination was investigated. Samples were analyzed using X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), energy dispersive X-ray (EDX), transmission electron microscopy (TEM), Fourier Transform Infrared Spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), diffuse UV-vis reflectance spectra, photoluminescence (PL) spectra and the electron spin resonance (ESR). XRD analysis found tetragonal crystalline structures in the SnO2 nanoparticles generated through calcination. EDX and FT-IR spectroscopy phase analysis verified the derivation of the Sn and O in the SnO2 nanoparticle samples from the precursor materials. An average nanoparticle size of 4–15.5 nm was achieved by increasing calcination temperature from 500 °C to 800 °C, as confirmed through TEM. The valence state and surface composition of the resulting nanoparticle were analyzed using XPS. Diffuse UV-vis reflectance spectra were used to evaluate the optical energy gap using the Kubelka-Munk equation. Greater calcination temperature resulted in the energy band gap falling from 3.90 eV to 3.64 eV. PL spectra indicated a positive relationship between particle size and photoluminescence. Magnetic features were investigated through ESR, which revealed the presence of unpaired electrons. The magnetic field resonance decreases along with an increase of the g-factor value as the calcination temperature increased from 500 °C to 800 °C. Finally, Escherichia coli ATCC 25922 Gram (–ve) and Bacillus subtilis UPMC 1175 Gram (+ve) were used for in vitro evaluation of the tin oxide nanoparticle’s antibacterial activity. This work indicated that the zone of inhibition of 22 mm has good antibacterial activity toward the Gram-positive B. subtilis UPMC 1175.
Abstract:A simple thermal treatment method, utilizing only zinc nitrate, polyvinyl pyrrolidone (PVP), and deionized water, was used to synthesize ZnO nanoparticles, and their characteristics were investigated by various techniques. The TGA measurement demonstrated that the bulk of the capping agent PVP can be removed at temperatures higher than 500 °C and is consistent with the absence of the majority of PVP absorption peaks in the FT-IR spectra. The formation of almost pure ZnO nanoparticles was established by the presence of single absorption peak in the FT-IR spectra due to being only Zn-O bonds at calcination temperatures of 500 °C and above. The TEM images revealed that the nanoparticles have a spherical shape and the particle size increased from 60.1-83.1 nm with an increase in calcination temperatures from 500-600 °C. The XRD diffraction patterns indicated that the particles are of a wurzite lattice structure. The optical properties were determined by UV-Vis spectrophotometer, and it was found that the band gap of ZnO nanoparticles decreased from 3.249-3.239 eV with an increase in calcination temperature from 500-600 °C.
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