Fluorine-doped ZnO (ZnO:F) thin films were deposited by ultrasonic spray pyrolysis (USP) at 475°C using zinc acetate precursors subjected to controlled planetary ball milling (0–300 min). Unlike conventional approaches that rely on precursor aging or post-deposition annealing to enhance conductivity, this work demonstrates that mechanochemical activation of the Zn precursor provides an effective route to modulate the microstructural evolution and optoelectronic performance of ZnO:F transparent conductive films. X-ray diffraction and SEM analyses reveal that intermediate milling times (45–60 min) promote improved crystallinity and grain coalescence, whereas prolonged milling (≥120 min) induces structural disorder and limits grain growth. The results identify 60 min as the optimal precursor milling time, thereby enhancing optoelectronic performance by simultaneously improving electrical conductivity and optical transparency. As a result, the films milled for 60 min exhibit the most favorable convergence of optical transparency and electrical transport properties, achieving a sheet resistance of 80 Ω/□, Hall mobility up to 3.6 cm2V−1s−1, and an average transmittance above 70% at 550 nm. A maximum Haacke figure of merit of 5.02 × 10−4 Ω−1 was achieved without precursor aging or post-deposition annealing, demonstrating a significant reduction in processing complexity. Compared to previous studies based on prolonged aging or extended deposition processes, the proposed approach achieves comparable optoelectronic performance with shorter processing time and fewer fabrication steps. These findings establish precursor milling as a practical tuning parameter to optimize ZnO:F thin films for optoelectronic, photovoltaic, and smart-window applications.
Fluorine-doped ZnO (ZnO:F) thin films were deposited by ultrasonic chemical spray, using a mechanically milled zinc precursor. We systematically assessed the effect of film thickness (controlled via deposition time: 4-24 min) on the structural, morphological, optical, and electrical properties. X-ray diffraction confirmed hexagonal wurtzite ZnO with predominant (002) orientation, with lattice compression associated to F-substitution. SEM/AFM analy ses revealed a transition from discontinuous surfaces with compact, well-connected grains as thickness increased, accompanied by reduced roughness. Optically, thinner films exhibited higher visible transmittance, while the band gap slightly widened (3.30-3.42 eV) with thickness. Hall measurements confirmed n-type behavior for all samples. The sample deposited for 14 min achieved the best trade-off between transmittance and conductiv ity (FoM approximate to 2.0 & times;10-4 Omega-1), competitive with state-of-the-art spray-deposited TCOs. These results demonstrate that combining precursor mechanical activation with thickness control is an effective low-cost route to fabricate indium-free transparent electrodes suitable for optoelectronic and solar-energy devices.
The CIGS-based thin film solar cells (TFSCs) are favorable in the photovoltaic market for their suitable material properties and potential to achieve a high efficiency-to-cost ratio. Here, the thickness and doping concentration of CISe, CdS and CGS BSF materials used in CISe TFSCs were simulated through SCAPS software. The greater CISe absorber thickness improves the absorption of photons; on the other hand, higher CISe doping concentration can enhance recombination centers. The CdS thickness ranging from 50 to 100 nm and CdS doping concentration greater than that of the absorber layer are preferred. Similarly, the maximum open circuit voltage was found for a BSF thickness of 500 nm and higher BSF concentrations were positive to reduce recombination centers. The efficiency is drastically increased from 22.46 to 32.60 % for CISe TFSCs after using the CGS BSF layer. The experimental results of the CISe and CdS are also analyzed through this simulation. It was confirmed that the device performance is directly related to CdS thickness; however, a negligible difference in efficiency value was noticed for CISe TFSCs with BSF even when the CdS thickness increases. Therefore, this theoretical modeling can provide valuable information for experimental activities in designing novel and efficient PV devices.
GaN thin films were obtained by RF sputtering using a reactive atmosphere consisting of a nitrogen/argon mixture, varying the nitrogen nominal concentration. The structural properties were evaluated as a function of the nitrogen nominal concentration. Structural characterization was performed by X-ray diffraction, high-resolution transmission electron microscopy, and Raman spectroscopy. The structural characterization showed that GaN films deposited using an atmosphere of pure Ar have an amorphous nature. As the nitrogen content in the atmosphere increases, GaN thin films become polycrystalline. GaN thin films deposited by $\mathbf{R F}$ sputtering have a hexagonal crystalline structure.
Titanium dioxide (TiO2) nanoparticles were synthesized via a chemical precipitation method. The study employed the Taguchi statistical approach to optimize synthesis parameters for enhanced photocatalytic activity. Results identified the solvent and reflux time as the most influential factors affecting both particle size and photocatalytic performance. Characterization by X-ray diffraction (XRD) confirmed that most samples exhibited the anatase phase, while scanning electronic microscopy (SEM) analysis revealed agglomerates of spherical and oval nanoparticles with sizes ranging from 35 to 77 nm. The bandgap was calculated using diffuse reflectance spectroscopy, and all samples exhibited a consistent value of 3.35 eV. No significant variations in bandgap were observed among the samples. Photocatalytic activity was evaluated through photodegradation of aqueous aniline solutions under UV irradiation, achieving degradation efficiencies between 82% and 95.5%. Optimization via the Taguchi method led to a maximum aniline removal efficiency of over 98%, confirming the effectiveness of the approach. SEM images of the optimal sample displayed a porous surface morphology with an average particle size of 40 nm, which could be verified by transmission electron microscopy (TEM) micrographs. The results showed the effectiveness of the Taguchi statistical approach in the optimization of synthesis conditions to enhance photocatalytic performance.
In this study, the MO3 (MoO3 and WO3) nanoparticles are synthesized using the thermo-mechanical method made from agate material. The material and sensing properties of MO3 samples prepared at different milling times are analyzed using different characterization techniques. The orthorhombic crystal structure and reduced crystalize size with milling times for MO3 samples are found from the X-ray diffraction and Raman spectroscopy results. Uniform and nano-sized grains after the thermo-mechanical process are seen from SEM and TEM results. From EDS analysis, the oxygen content diminishes at higher milling times by forming oxygen-vacancy pairs. The bandgap values are comparatively higher for milled MO3 samples than unmilled samples. The average pore size of less than 50 nm confirms the existence of mesoporous particles. Finally, relatively better sensing response is noticed for milled MO3 samples than unmilled samples, showing promising to monitor CO gas in different fields.
In this work, an analysis on the physicochemical properties of materials based on NiTe-Ni2Te3 synthesized through a mechanosynthesis process by using a planetary ball mill, at ambient conditions, was carried out. Pure nickel and tellurium powders with a mass ratio of 1:1 were used as precursors. The milling speed was kept constant at 500 rpm, and the effective milling time was varied, 2, 4, 6, 8 and 10 h. The structural, morphological, optical and electrical properties of NiTe-Ni2Te3 materials were studied. The crystallographic properties by X-ray powder diffraction (DRX) were analyzed, and it was determined that the materials present a mix of two different compounds; a hexagonal phase of NiTe and a monoclinic phase of Ni2Te. From scanning electron microscopy (SEM) the presence of agglomerates of particles with irregular morphologies and others in disc form were evidenced. From reflectance measurements the bandgap energies, Eg, were estimated, and it was found an Eg increase with milling time. From the infrared spectroscopy analysis (FTIR), the characteristic vibrational frequencies, 425 and 672 cm−1, of the NiTe-Ni2Te3 system were observed. The electrical properties were measured by Hall effect, using the Van Der Pauw contacts confiration, confirming the n-type conductivity in all the samples, and obtaining that sample synthesized with 8 h of milling presented the best electrical properties, resistivity of 0.77 Ωcm, electron concentration of 2.0 × 1017 cm−3 and mobility 53.08 cm2V−1s−1. The Seebeck coefficient and power factor were estimated to evaluate the thermoelectric properties of the samples. The sample synthesized with 4 h of milling presented the highest Seebeck coefficient and power factor, − 74.56 µVK−1 and 4.27 µWcm−1 K−2, respectively. The obtained results showed promising properties of synthesized NiTe-Ni2Te3 powders and its possible application as thermoelectrical materials.
In this work, the characterization and testing of sensing properties of ZnTe powders for detecting carbon monoxide were investigated. The ZnTe synthesis was reached by a solvothermal process, using three different green solvents, methanol, ethanol, and isopropanol. The structural, morphological, and compositional properties of ZnTe powders were analyzed by X-ray diffraction, XRD, scanning electron microscopy, SEM, and atomic force microscopy, AFM, and X-ray energy dispersion (EDS), respectively. XRD confirmed the zincblende-type cubic phase of ZnTe, with crystallite sizes of the order of 69 nm. SEM images of all synthesized samples showed a surface covered with particles of different sizes and irregular morphologies. Finally, the sensing response of ZnTe samples to CO was measured for concentrations varying from 1 to 500 ppm at different operating temperatures, 100, 200, and 300 °C. The highest sensitivity, 18.4, was obtained for ZnTe samples synthesized from isopropanol as solvent, so ZnTe powders showed a good response for CO detection, resulting these materials promising to be applied as gas sensors.
The development of semitransparent CdS/CdTe ultrathin solar cells has been delayed as a result of the activation annealing to which the device must be subjected, which may involve problems such as the sublimation of ultrathin films and the diffusion of Cd and S at the interface. In this work, CdS/CdTe ultrathin devices on soda-lime glass/SnO2:F/ZnO substrates were obtained by RF magnetron sputtering. CdS/CdTe ultrathin heterostructures were obtained with the following thicknesses for the CdS thin film: 70, 110, and 135 nm. The CdTe thickness film was kept constant at 620 nm. Subsequently, activation annealing with CdCl2 was carried out at 400 °C. Surface characterization was performed by scanning electron microscopy, which indicated that the CdCl2 annealing tripled the CdTe thin films’ grain size. Raman characterization showed that CdS thin films deposited by RF sputtering present the first, the second, and the third longitudinal optical modes, indicating the good crystallinity of the CdS thin films. The study showed that the photovoltaic properties of the CdS/CdTe ultrathin devices improved as the CdS thicknesses decreased.
The thermal oxidation of evaporated titanium-vanadium thin films was carried out at different post-annealing temperatures. The structural, morphological, compositional, optical, electrical, and gas sensing properties of titanium-vanadium oxide thin films were primarily investigated. The results of the XRD study and Raman spectroscopy verified the presence of the orthorhombic V2O5, tetragonal TiO2, and monoclinic V2Ti3O9 phases. The crystallinity of TVO thin films was improved at higher annealing temperatures. The grain size (seen from SEM images) and oxygen compositions (obtained from EDS measurement) of TVO samples are also enhanced when the post-annealing temperature is increased from 500 to 575 degrees C. From the transmittance curves, the bandgap values for TVO samples were estimated and found in the range of 2.14-2.36 eV. The n-type conductivity of TVO films was confirmed by the negative Hall coefficient values. At last, the CO gas sensing response of TVO thin films was analyzed by monitoring the change in the surface electrical resistances at different operating temperatures and CO gas concentrations. The dynamic and static resistances were assessed at different operating temperatures varying from 100 to 300 degrees C. The TVO sample prepared at 550 degrees C showed the best conditions by examining the materials and CO sensing properties.
In this work, the results of the study of ZnO:F (FZO) films deposited on glass substrates using the ultrasonic chemical spray technique are reported. For the preparation of the films, starting solutions were used at a concentration of 0.2 M of zinc acetate dihydrate [Zn(CH3COO)2.2H2O]) dissolved in a mixture of deionized water:methanol:acetic acid. The precursor was previously ground in a planetary ball mill at 500 rpm at different times. For the addition of the dopant, a 1.6 M solution of ammonium fluoride in deionized water was prepared NH4F. The atomic ratio of [F]/[F + Zn] remained constant at 30 at
One-dimensional (1D) nanomaterials have garnered significant scientific and technological attention due to their potential applications in electronics devices, gas sensing, energy conversion, and photocatalysis. However, the development of a simple and low-cost technique for 1D nanostructure synthesis remains a challenge. The doping of ZnO nanostructures has proven to be an effective way to improve their internal properties. In this work, one-dimensional ZnO and Ce-doped ZnO nanorods and nanonails were synthesized by a simple thermal evaporation method using different weight ratios of ZnS and CeO2 precursor powders in a catalyst-free process. The effects of cerium doping concentration on the structural, morphological, and optical properties of the as-prepared samples were investigated. XRD analysis confirmed that the crystal structure was converted from the cubic ZnS phase to the hexagonal ZnO phase with increasing annealing temperatures. The UV-Vis spectra showed that the optical absorption edge of Ce-doped ZnO samples was slightly red-shifted. Additionally, the band gap energy decreases with increasing cerium concentration. SEM images showed that the morphology of the structures obtained changed from nanorods to nanonails as the Ce content increased. The incorporation of Ce ions into the ZnO matrix has been successfully confirmed by HRTEM, Raman, and EDX analysis. Photocatalytic activity studies showed that Ce-doped ZnO samples exhibited significantly enhanced photocatalytic performance compared to pure ZnO for the degradation of rhodamine B under UV radiation. These results may suggest the use of heterogeneous photocatalysis as an efficient, cheap, and environment-friendly alternative for the removal of pollutants from water and the use of Ce-doped ZnO as a promising candidate.
BiCuOSe systems are proposed as candidates to develop transparent p-type semiconductors in the visible region. This work reports the characterization results obtained for the BiCuOSe powders, synthesized by the solid-state reaction (SSR) method through mechanical milling, and nanostructured thin films deposited from the same processed powders using the pulsed laser deposition (PLD) technique. Structural characterization through X-ray diffraction (XRD) showed that the material presents a tetragonal structure with an average crystallite size of 21 nm and a preferential orientation in the (1 0 2) plane. The morphological and particle size evolution of BiCuOSe powders is presented as a function of the milling time. Transmission and scanning electron microscopies confirmed the spherical geometry of the particles in the powders and nanosheets like structure for the films. Particle sizes were also estimated, ranging from 10 to 100 nm for powders and 60 to 70 nm for films. The bandgap values, EG, for BiCuOSe powders were estimated from diffuse reflectance spectra using the Kubelka–Munk method, yielding values close to 0.7 eV. For thin films, EG values were estimated using the Tauc method, obtaining values in the range of 0.8–3.5 eV, depending on the annealing treatment. Additionally, electrical properties were measured in all deposited thin films, confirming the p-type conductivity, a minimal resistivity of 0.0735 Ω cm, hole mobility on the order of 88 cm2/Vs, and carrier concentration of 9.7 × 1018 cm−3.
Fluorine-doped zinc oxide (ZnO:F) thin films are valued for their potential as transparent conductive materials, particularly in optoelectronic applications. In this work, the deposition of highly conductive and transparent fluorine-doped ZnO thin films, deposited by chemical spray on glass substrates is reported. The effect of acetic (AcAc) in the initial fresh solution on Haacke's Figure of Merit ( Phi ) of both zinc oxide (ZnO) and fluorine-doped zinc oxide (ZnO:F) thin films was studied. The substrate temperature was fixed to 450 degrees C, and two deposition times (8 and 14 min) were tested. Accordingly, the optical and transport properties, as well as the structural and morphological characteristics of the films were measured. The results indicate that the samples are polycrystalline in all cases and exhibit a wurtzite-type structure of ZnO. The variation of AcAc in the starting solution causes a switch in preferential growth from (002) to (001). As the AcAc content increases, the surface morphology of the films reveals the formation of well-defined hexagonal grains, and the grain size increases. Conversely, the transmittance decreases as the acetic acid increases, which can attributed to carbon incorporation into the film. In addition, the band gap values of the films varied from 3.2 to 3.4 eV. Also, as the acetic acid concentration increased, a drop in the electrical resistivity of ZnO thin films on the order of 0.016 Omega & sdot; cm was found for the ZnO:F films deposited with fresh solution for 14 min. This can be ascribed to a dense acetic cloud formed during the synthesis process, trapping volatile F species that incorporate into the ZnO lattice. This enhances Haacke's Figure of Merit of ZnO:F films deposited with a fresh solution, demonstrating their potential use for application as transparent conductive films. This contrasts with other synthesis methods that require longer aging time in the precursor solution, making these findings useful for large-scale and more efficient production of transparent conductive films.
Graphene oxides (GOs), synthesized with different oxidation degrees and associated with Titanium dioxide (TiO2) nanoparticles show efficient adsorption processes for dye molecules in solution. The structural, morphology, electronic and optical features of the nanocomposites were investigated by dedicated methods. Water remediation was investigated through the adsorption efficiency of methylene blue (MB) dye as a function of the nanocomposites concentration from 1 to 5 g/L in solutions. While pristine TiO2 showed a maximum removal of similar to 44%, the incorporation of the GO ensures the fast and complete elimination of MB within 9 min. The ball milling process contributed to the increase in the number of defects and surface area in the nano-composites, which was demonstrated by ID/IG ratios by Raman spectroscopy and surface areas by BET. Pseudosecond-order and mechanistic kinetic models were considered, and the performed analysis points out the relevance of the pseudo-second-order model to account for the adsorption kinetics. The Langmuir and Freundlich isotherm models were applied to the experimental data to find an adequate model to describe the adsorption equilibrium, as well as the intra-particle diffusion model during the different adsorption stages involved in the TiO2/GO nanocomposites. The role of the oxidation degree of GO was clarified through their respective efficiency in the removal of the dyes.
A LaCuOS target was obtained through a two-step route: first, the synthesis of the CuLaO2 compound by solidstate reaction, and subsequently its sulfurization under a sulfur atmosphere. The LaCuOS powder was used to deposition films by pulsed laser deposition at different growth times: 10, 15, 20, and 25 min. The films were deposited in vacuum at a substrate temperature of 400 degrees C and a wavelength of 266 nm. The structural characterization showed that the dislocation density and stress in LaCuOS films increase as the deposition time increases. The LaCuOS films exhibit optical transmittance of 52-81 % in the visible region. Electrical measurements indicate high values of hole mobility and carrier densities up to 1019 cm-3, with a p-type electrical conductivity of 0.74 S/cm; these properties suggest that LaCuOS films have the potential to be integrated as transparent material in devices.
A Bi1.6Pb0.4Sr2Ca2Cu3Oy superconductor target was obtained by a solid-state reaction at 860 °C by 130 h. Afterward, Bi1.6Pb0.4Sr2Ca2Cu3Oy thin films were grown by pulsed laser deposition at room temperature, from pellets of the synthesized target, on (111) silicon substrates. Bi1.6Pb0.4Sr2Ca2Cu3Oy films were deposited using an Nd:YAG laser with two different incident wavelengths (532 and 1064 nm) and by varying the distance between the target and the substrate: 20, 25, and 30 mm. X-ray diffraction results showed that Bi1.6Pb0.4Sr2Ca2Cu3Oy films were obtained with Bi-2223 and Bi-2212 superconductor phases.
Indium doped zinc oxide films, IZO, deposited onto soda-lime glass substrates by the ultrasonic spray pyrolysis, USP, were prepared from milled Zn precursor. The influence of the In content (at%) in the starting solution and grinding process was analyzed. 0.2 M starting solutions with different In concentrations, 1, 2, and 3 at% were prepared. The deposition conditions were kept constant, substrate temperature of 450°C, and a deposition time of 7 min. The milling process was carried out in a planetary ball mill, with a ball/powder ratio of 4:1, and a speed of 300 RPM.The structural, morphological, optical and electrical properties of the ZO and IZO were analyzed by X-ray diffraction, XRD, field emission scanning electron microscopy, FESEM, UV-Vis spectroscopy, and sheet resistance and Hall effect measurements, respectively.From XRD analysis was found that both ZO and IZO films present a preferential orientation along the (002) planes. The FESEM images confirm that all deposited films present hexagonal nanostructures with different size. The average optical transmission oscillated in the range of 82-87%, confirming the high transparency of all the deposited films. The lowest resistivity value, 3.72 × 10 –3 Ωcm, was obtained in the 3 at% film (3IZO-M) and a figure of merit of 3.22 × 10 –3 ( Ω / square ) –1 . According to the obtained results, it can be stated that IZO films deposited by the USP technique, are potentially applicable in the optoelectronics field.
Bi(1.6)Pb(0.4)Sb(0.0)6Sr(2)Ca(2)Cu(3)O(y) superconductors were processed by the solid-state reaction at 860 degrees C, varying the sintering time from 100 to 160 h. The structural characterization was carried out by X-ray diffraction and Raman spectroscopy, which showed that Bi(1.6)Pb(0.4)Sb(0.0)6Sr(2)Ca(2)Cu(3)O(y) samples have a mixture of interest B-2212 and Bi2223 phases. The sintering time strongly influences structural, morphological and electrical properties; the sample sintered by 130 h presents a volume fraction of 62% for the Bi-2223 phase, large grains (between 5 and 20 mu m) and a critical temperature of 107 K.