BaMoO4 was obtained via facile mechanochemical synthesis at room temperature and a solid-state reaction. An evaluation of the phase composition and structural and optical properties of BaMoO4 was conducted. The influence of different milling speeds on the preparation of BaMoO4 was explored. A shorter reaction time for the phase formation of BaMoO4 was achieved using a milling speed of 850 rpm. A milling speed of 500 rpm led to partial amorphization of the initial reagents and to prolongation of the synthesis time of up to 3 h of milling time. Solid-state synthesis was performed via heat treatment at 900 °C for 15 h. X-ray diffraction analysis (XRD), infrared (IR) and UV diffuse reflectance (UV-Vis) and photoluminescence (PL) spectroscopy were carried out to characterize the samples. Independently of the method of preparation, the obtained samples had tetragonal symmetry. The average crystallite sizes of all samples, calculated using Scherrer’s formula, were in the range of 240 to 1540 Å. IR spectroscopy showed that more distorted structural MoO4 units were formed when the compound was synthesized via a solid-state reaction. The optical band gap energy of the obtained materials was found to decrease from 4.50 to 4.30 eV with increasing crystallite sizes. Green- and blue-light emissions were observed for BaMoO4 phases under excitation wavelengths of 330 and 488 nm. It was established that the intensity of the PL peaks depends on two factors: the symmetry of MoO4 units and the crystallite sizes.
CaWO4 nanoparticles were obtained by facile mechanochemical synthesis at room temperature, applying two different milling speeds. Additionally, a solid-state reaction was employed to assess the phase composition, structural, and optical characteristics of CaWO4. The samples were analyzed by X-ray diffraction (XRD), transition electron microscopy (TEM), and Raman, infrared (IR), ultraviolet–visible (UV–Vis) reflectance, and photoluminescence (PL) spectroscopies. The phase formation of CaWO4 was achieved after 1 and 5 h of applied milling speeds of 850 and 500 rpm, respectively. CaWO4 was also obtained after heat treatment at 900 °C for 12 h. TEM and X-ray analyses were used to calculate the average crystallite and grain size. The Raman and infrared spectroscopies revealed the main vibrations of the WO4 groups and indicated that more distorted structural units were formed when the compound was synthesized by the solid-state method. The calculated value of the optical band gap of CaWO4 significantly increased from 2.67 eV to 4.53 eV at lower and higher milling speeds, respectively. The determined optical band gap of CaWO4, prepared by a solid-state reaction, was 5.36 eV. Blue emission at 425 (422) nm was observed for all samples under an excitation wavelength of 230 nm. CaWO4 synthesized by the solid-state method had the highest emission intensity. It was established that the intensity of the PL peak depended on two factors: the morphology of the particles and the crystallite sizes. The calculated color coordinates of the CaWO4 samples were located in the blue region of the CIE diagram. This work demonstrates that materials with optical properties can be obtained simply and affordably using the mechanochemical method.
This study focuses on the influence of electrospray deposition parameters on the morphology, topography, optical and sensing properties of ZnO films deposited on gold electrodes of quartz crystal resonators. The substrate temperature, precursor feed rate and emitter’s voltage were varied. Zinc acetate dehydrate dissolved in a mixture of deionized water, ethanol and acetic acid was used as a precursor. The surface morphology and average roughness of the films were studied by scanning electron microscopy (SEM) and 3D optical profilometry, respectively, while the optical properties were investigated by diffuse reflectance and photoluminescence measurements. The sensing response toward ammonia was tested and verified by the quartz crystal microbalance (QCM) method. The studies demonstrated that electrospray deposition parameters strongly influence the surface morphology, roughness and gas sensing properties of the films. The deposition parameters were optimized in order for the highest sensitivity toward ammonia to be achieved. The successful implementation of the electrospray method as a simple, versatile and low-cost method for deposition of ammonia-sensitive and selective ZnO films used as a sensing medium in QCM sensors was demonstrated and discussed.
Nanocrystalline CoWO4 sampled were synthesized using a simple mechanochemical approach and a solid-state reaction, respectively. The formation of nanocrystalline CoWO4 was characterized by X-ray diffraction (XRD) and infrared spectroscopy (IR). The optical properties of the obtained samples were explored by diffuse reflectance UV–visible (DRS) and photoluminescence (PL) techniques. A milling speed of 850 rpm led to the direct synthesis of monoclinic CoWO4 with a short reaction time (1 h). The complete reaction did not occur in the solid-state synthesis. The obtained samples had monoclinic crystal systems with different lattice parameters. The average crystallite sizes of CoWO4 were in the range of 20 to 180 nm. The TEM investigation showed that the morphology of the CoWO4 particles differed depending on the preparation conditions. The values of the determined optical bandgap of CoWO4 were the range of 1.89 to 2.18 eV, according to diffusion reflectance spectroscopy in the ultraviolet-to-visible range. Broader blue–green emission spectra with peaks at 430 nm were observed for samples prepared via both routes. The CIE color coordinates of the CoWO4 samples lay in the blue and purple regions. The quantum yields of the CoWO4 samples synthesized after 1 h and 5 h milling times at 850 rom were 0.34 and 0.67%, respectively. This study proposes an affordable mechanochemical approach for blue–green phosphors that could possibly be used in various light-emitting diodes (LEDs).
Two modifications of ZnMoO4 were successfully obtained by mechanochemical treatment with two milling speeds applied at 500 and 850 rpm. The phase formation was monitored by XRD analysis. The metastable monoclinic ß-ZnMoO4 was directly synthesized at room temperature using the higher milling speed of 850 rpm. The thermodynamically stable triclinic α-ZnMoO4 was obtained by combining heat treatment t 600 °C and ball milling at the lower milling speed of 500 rpm. The IR spectra contain typical vibration bands and confirm the formation of both ZnMoO4 polymorphs. UV-Vis absorption and photoluminescence (PL) spectroscopy are used to study the optical properties of the as-prepared samples. The calculated optical band gaps for α- and ß-ZnMoO4 are 4.09 and 3.02 eV. The photoluminescence emission spectrum of both samples shows peaks with different maximum intensity at 615 and 403 nm for α and ß phase, respectively. CIE co-ordinates are located in the orange and blue range of the color diagram.