Search results for: zinc oxide sub-microparticles

Authors: Fahima Djefaflia, M. Loutfi Benkhedir

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The aim of this work was to development and characterisation of iron oxide thin films by spray pyrolysis technique. Influences of deposition parameters pile temperature on structural and optical properties have been studied Thin films are analysed by various techniques of materials. The structural characterization of films by analysis of spectra of X-ray diffraction showed that the films prepared at T=350,400,450 are crystalline and amorphous at T=300C. For particular condition, two phases hematiteFe2O3 and magnetite Fe3O4 have been observed.The UV-Visible spectrophotometer of this films confirms that it is possible to obtain films with a transmittance of about 15-30% in the visible range. In addition, this analysis allowed us to determine the optical gap and disorder of films. We conclude that the increase in temperature is accompanied by a reduction in the optical gap with increasing in disorder. An ab initio calculation for this phase shows that the results are in good agreement with the experimental results.

Keywords: spray pyrolysis technique, iron oxide, ab initio calculation, optical properties

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Authors: Qinglei Liu, Ali Charkhesht, Tiva Sharifi, Ashkan Bahadoran

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Graphene sheets are promising nanoscale building blocks as a support material for the dispersion of nanoparticles. In this work, a solvothermal method employed to directly grow Co1-xZnxFe2O4 ferrite nanospheres on graphene oxide support that is subsequently reduced to graphene. The samples morphology, structure and crystallography were investigated using field-emission scanning electron microscopy (FE-SEM) and powder X-ray diffraction (XRD). The influences of the Zn2+ content on photocatalytic activity, electrical conductivity and magnetic property of the samples are also investigated. The results showed that Co1-x Znx Fe2 O4 nanoparticles are dispersed on graphene sheets and obtained nanocomposites are soft magnetic materials. In addition the samples showed excellent photocatalytic activity under visible light irradiation.

Keywords: reduced graphene oxide, ferrite, magnetic nanocomposite, photocatalytic activity, solvothermal method

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Authors: Neetu Malik, Sharad Shrivastava, Subrata Bandhu Ghosh

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Biocomposite materials were fabricated using mixing biodegradable polymer polycaprolactone (PCL) and Thermally Exfoliated Graphene Oxide (TEGO) through solution casting. Various samples of biocomposite films were prepared by varying the TEGO wt% composition by 0.1%, 0.5%, 1% and 1.5%. Thereafter, the density and water absorption of the composites were investigated with respect to immersion time in water. The moisture absorption results show that with an increase in weight percentage (from 0.1 to wt 1.5%) of TEGO within the biopolymer films, the absorption value of bio-nanocomposite films reduced rapidly from 27.4% to 14.3%. The density of hybrid composites also increased with increase in weight percentage of TEGO. These results indicate that the optimized composition of constituents in composite membrane could effectively reduce the anhydrous conditions of bio-composite film.

Keywords: thermally exfoliated graphene oxide, PCL, water absorption, density

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Authors: J. O. Ajayi, S. S. Oluyamo, D. B. Agunbiade

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In this work, tin oxide thin films (SnO2) were prepared using the spin coating technique. The effects of precursor concentration on the thin film properties were investigated. Tin oxide was synthesized from anhydrous Tin (II) Chloride (SnCl2) dispersed in Methanol and Acetic acid. The metallic oxide (SnO2) films deposited were characterized using the UV Spectrophotometer and the Scanning Electron Microscope (SEM). From the absorption spectra, absorption increases with decrease in precursor concentration. Absorbance in the VIS region is lower than 0 % at higher concentration. The optical transmission spectrum shows that transmission increases as the concentration of precursor decreases and the maximum transmission in visible region is about 90% for films prepared with 0.2 M. Also, there is increase in the reflectance of thin films as concentration of precursor increases. The films have high transparency (more than 85%) and low reflectance (less than 40%) in the VIS region. Investigation showed that the direct band gap value increased from 3.79eV, to 3.82eV as the precursor concentration decreased from 0.6 M to 0.2 M. Average direct bandgap energy for all the tin oxide films was estimated to be 3.80eV. The effect of precursor concentration was directly observed in crystal outgrowth and surface particle densification. They were found to increase proportionately with higher concentration.

Keywords: anhydrous TIN (II) chloride, densification, NIS- VIS region, spin coating technique

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Authors: Jan Luxa, Vlastimil Mazanek, Petr Malinsky, Alexander Romanenko, Mariapompea Cutroneo, Vladimir Havranek, Josef Novak, Eva Stepanovska, Anna Mackova, Zdenek Sofer

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Using accelerated energetic ions is an interesting method for the introduction of structural changes in various carbon-based materials. This way, the properties can be altered in two ways: a) the ions lead to the formation of conductive pathways in graphene oxide structures due to the elimination of oxygen functionalities and b) doping with selected ions to form metal nanoclusters, thus increasing the conductivity. In this work, energetic beams were employed in two ways to prepare capacitor structures in graphene oxide (GO), reduced graphene oxide (rGO) and polyimide (PI) on a micro-scale. The first method revolved around using ion beam writing with a focused ion beam, and the method involved ion implantation via a polymeric mask. To prepare the polymeric mask, a direct spin-coating of PMMA on top of the foils was used. Subsequently, proton beam writing and development in isopropyl alcohol were employed. Finally, the mask was removed using acetone solvent. All three materials were exposed to ion beams with an energy of 2.5-5 MeV and an ion fluence of 3.75x10¹⁴ cm-² (1800 nC.mm-²). Thus, prepared microstructures were thoroughly characterized by various analytical methods, including Scanning electron microscopy (SEM) with Energy-Dispersive X-ray spectroscopy (EDS), X-ray Photoelectron spectroscopy (XPS), micro-Raman spectroscopy, Rutherford Back-scattering Spectroscopy (RBS) and Elastic Recoil Detection Analysis (ERDA) spectroscopy. Finally, these materials were employed and tested as sensors for humidity using electrical conductivity measurements. The results clearly demonstrate that the type of ions, their energy and fluence all have a significant influence on the sensory properties of thus prepared sensors.

Keywords: graphene, graphene oxide, polyimide, ion implantation, sensors

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Authors: Nadine Raidl, Benjamin Kaufmann, Michael Hofstätter, Peter Supancic

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If polycrystalline ZnO is properly doped and sintered under very specific conditions, it shows unique electrical properties, which are indispensable for today’s electronic industries, where it is used as the number one overvoltage protection material. Under a critical voltage, the polycrystalline bulk exhibits high electrical resistance but becomes suddenly up to twelve magnitudes more conductive if this voltage limit is exceeded (i.e., varistor effect). It is known that these peerless properties have their origin in the grain boundaries of the material. Electric charge is accumulated in the boundaries, causing a depletion layer in their vicinity and forming potential barriers (so-called Double Schottky Barriers, or DSB) which are responsible for the highly non-linear conductivity. Since ZnO is a piezoelectric material, mechanical stresses induce polarisation charges that modify the DSB heights and as a result the global electrical characteristics (i.e., piezotronic effect). In this work, a finite element method was used to simulate emerging stresses on individual grains in the bulk. Besides, experimental efforts were made to testify a coherent model that could explain this influence. Electron back scattering diffraction was used to identify grain orientations. With the help of wet chemical etching, grain polarization was determined. Micro lock-in infrared thermography (MLIRT) was applied to detect current paths through the material, and a micro 4-point probes method system (M4PPS) was employed to investigate current-voltage characteristics between single grains. Bulk samples were tested under uniaxial pressure. It was found that the conductivity can increase by up to three orders of magnitude with increasing stress. Through in-situ MLIRT, it could be shown that this effect is caused by the activation of additional current paths in the material. Further, compressive tests were performed on miniaturized samples with grain paths containing solely one or two grain boundaries. The tests evinced both an increase of the conductivity, as observed for the bulk, as well as a decreased conductivity. This phenomenon has been predicted theoretically and can be explained by piezotronically induced surface charges that have an impact on the DSB at the grain boundaries. Depending on grain orientation and stress direction, DSB can be raised or lowered. Also, the experiments revealed that the conductivity within one single specimen can increase and decrease, depending on the current direction. This novel finding indicates the existence of asymmetric Double Schottky Barriers, which was furthermore proved by complementary methods. MLIRT studies showed that the intensity of heat generation within individual current paths is dependent on the direction of the stimulating current. M4PPS was used to study the relationship between the I-V characteristics of single grain boundaries and grain orientation and revealed asymmetric behavior for very specific orientation configurations. A new model for the Double Schottky Barrier, taking into account the natural asymmetry and explaining the experimental results, will be given.

Keywords: Asymmetric Double Schottky Barrier, piezotronic, varistor, zinc oxide

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Authors: M. K. Deore

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The thick films of undoped and Al2O3 doped- ZnO were prepared by screen printing technique. AR grade (99.9 % pure) Zinc Oxide powder were mixed mechanochemically in acetone medium with Aluminium Chloride (AlCl2) material in various weight percentages such as 0.5, 1, 3 and 5 wt % to obtain Al2O3 - ZnO composite. The prepared materials were sintered at 1000oC for 12h in air ambience and ball milled to ensure sufficiently fine particle size. The electrical, structural and morphological properties of the films were investigated. The X-ray diffraction analysis of pure and doped ZnO shows the polycrystalline nature. The surface morphology of the films was studied by SEM. The final composition of each film was determined by EDAX analysis. The gas response of undoped and Al2O3- doped ZnO films were studied for different gases such as CO, H2, NH3, and H2S at operating temperature ranging from 50 oC to 450 o C. The pure film shows the response to H2S gas (500ppm) at 300oC while the film doped with 3 wt.% Al2O3 gives the good response to H2S gas(ppb) at 350oC. The selectivity, response and recovery time of the sensor were measured and presented.

Keywords: thick films, ZnO-Al2O3, H2S gas, sensitivity, selectivity, response and recovery time

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Authors: R. A. C. H. Seneviratne, M. Gunawardana, R. P. N. P. Rajapakse

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To address the micronutrient deficiencies in the Asian region, the World Food Program in its current mandate highlights the requirement of employing efficient fortification of micronutrients in rice, under the program 'Scaling-up Rice Fortification in Asia'. The current industrial methods of rice fortification with micronutrients are not promising due to poor permeation or retention of fortificants. This study was carried out to develop a method to improve fortification of micronutrients in rice by removing the air barriers for diffusing micronutrients through the husk. For the purpose, soaking stage of paddy was coupled with vacuum (- 0.6 bar) for different time periods. Both long and short grain varieties of paddy (BG 352 and BG 358, respectively) initially tested for water uptake during hot soaking (70 °C) under vacuum (28.5 and 26.15%, respectively) were significantly (P < 0.05) higher than that of non-vacuum conditions (25.24 and 25.45% respectively), exhibiting the effectiveness of water diffusion into the rice grains through the cleared pores under negative pressure. To fortify the selected micronutrients (iron and zinc), paddy was vacuum-soaked in Fe2+ or Zn2+ solutions (500 ppm) separately for one hour, and continued soaking for another 3.5 h without vacuum. Significantly (P<0.05) higher amounts of Fe2+ and Zn2+ were observed throughout the soaking period, in both short and long grain varieties of rice compared to rice treated without vacuum. To achieve the recommended limits of World Food Program standards for fortified iron (40-48 mg/kg) and zinc (60-72 mg/kg) in rice, soaking was done with different concentrations of Fe2+ or Zn2+ for varying time periods. For both iron and zinc fortifications, hot soaking (70 °C) in 400 ppm solutions under vacuum (- 0.6 bar) during the first hour followed by 2.5 h under atmospheric pressure exhibited the optimum fortification (Fe2+: 46.59±0.37 ppm and Zn2+: 67.24±1.36 ppm) with a greater significance (P < 0.05) compared to the controls (Fe2+: 38.84±0.62 ppm and Zn2+: 52.55±0.55 ppm). This finding was further confirmed by the XRF images, clearly showing a greater fixation of Fe2+ and Zn2+ in the rice grains under vacuum treatment. Moreover, there were no significant (P>0.05) differences among both Fe2+ and Zn2+ contents in fortified rice even after polishing and washing, confirming their greater retention. A seven point hedonic scale showed that the overall acceptability for both iron and zinc fortified rice were significantly (P < 0.05) higher than the parboiled rice without fortificants. With all the drawbacks eliminated, per kilogram cost will be less than US$ 1 for both iron and zinc fortified rice. The new method of rice fortification studied and developed in this research, can be claimed as the best method in comparison to other rice fortification methods currently deployed.

Keywords: fortification, vacuum assisted diffusion, micronutrients, parboiling

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Authors: Mohamed A. Deyab, Omnia El-Shamy

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The main objective of this case study is to integrate the advantages of cathodic protection technologies in order to lessen chloride-induced corrosion in reinforced concrete. This research employs potentiodynamic polarisation, impedance spectroscopy (EIS), and surface characteristics. The results showed how effectively the new cathodic control strategy is preventing corrosion of the concrete iron rods. Over time, the protective system becomes more reliable and effective. The potentials of the zinc electrode persist still more negative after 30 days, implying that the zinc electrode can maintain powerful electrocatalytic behavior for a long period of time. As per the electrochemical impedance spectroscopy (EIS), using the CP technique reduces the rate of corrosion of rebar iron in cementitious materials over time.

Keywords: cathodic protection, corrosion, reinforced concrete, chloride

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Authors: Jadranka Blazhevska Gilev

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IR laser-induced ablation of poly(butylacrylate-methylmethacrylate/hydroxyl ethyl methacrylate)/reduced graphene oxide (p(BA/MMA/HEMA)/rGO) was examined with 0.5, 0.75 and 1 wt% reduced graphene oxide content in relation to polymer. The irradiation was performed with TEA (transversely excited atmosphere) CO₂ laser using incident fluence of 15-20 J/cm², repetition frequency of 1 Hz, in an evacuated (10-3 Pa) Pyrex spherical vessel. Thin deposited nanocomposites films with large specific area were obtained using different substrates. The properties of the films deposited on these substrates were evaluated by TGA, FTIR, (Thermogravimetric analysis, Fourier Transformation Infrared) Raman spectroscopy and SEM microscopy. Homogeneous distribution of graphene sheets was observed from the SEM images, making polymer/rGO deposit an ideal candidate for SERS application. SERS measurements were performed using Rhodamine 6G as probe molecule on the substrate Ag/p(BA/MMA/HEMA)/rGO.

Keywords: laser ablation, reduced graphene oxide, polymer/rGO nanocomposites, thin deposited film

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Authors: Shyam Ranjan Kumar, Shashikant Rajpal

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Zinc Telluride (ZnTe) is a binary II-VI direct band gap semiconducting material. This semiconducting material has several applications in sensors, photo-electrochemical devices and photovoltaic solar cell. In this study, Zinc telluride (ZnTe) thin films were deposited on nickel substrate by electrodeposition technique using potentiostat/galvanostat at -0.85 V using AR grade of Zinc Chloride (ZnCl2), Tellurium Tetrachloride (TeCl4) in non-aqueous bath. The developed films were physically stable and showed good adhesion. The as deposited ZnTe films were annealed at 400ºC in air. The solid state properties and optical properties of the as deposited and annealed films were carried out by XRD, EDS, SEM, AFM, UV–Visible spectrophotometer, and photoluminescence spectrophotometer. The diffraction peak observed at 2θ = 49.58° with (111) plane indicate the crystalline nature of ZnTe film. Annealing improves the crystalline nature of the film. Compositional analysis reveals the presence of Zn and Te with tellurium rich ZnTe film. SEM photograph at 10000X shows that grains of film are spherical in nature and densely distributed over the surface. The average roughness of the film is measured by atomic force microscopy and it is nearly equal to 60 nm. The direct wide band gap of 2.12 eV is observed by UV-Vis spectroscopy. Luminescence peak of the ZnTe films are also observed in as deposited and annealed case.

Keywords: annealing, electrodeposition, optical properties, thin film, XRD, ZnTe

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Authors: Christopher Mkirema Maghanga, Maurice Mghendi Mwamburi

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Parametric modeling provides a means to deeper understand the properties of materials. Drude, Brendel, Lorentz and OJL incorporated in SCOUT® software are some of the models used to study dielectric films. In our work, we utilized Brendel and Drude models to extract the optical constants from spectroscopic data of fabricated undoped and niobium doped titanium oxide thin films. The individual contributions by the two models were studied to establish how they influence the dielectric function. The effect of dopants on their influences was also analyzed. For the undoped films, results indicate minimal contribution from the Drude term due to the dielectric nature of the films. However as doping levels increase, the rise in the concentration of free electrons favors the use of Drude model. Brendel model was confirmed to work well with dielectric films - the undoped titanium Oxide films in our case.

Keywords: modeling, Brendel model, optical constants, titanium oxide, Drude Model

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Authors: Luciana P. Mazur, Tatiana A. Pozdniakova, Rui A. R. Boaventura, Vitor J. P. Vilar

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The electroplating industry requires a lot of process water, which generates a large volume of wastewater loaded with heavy metals. Two different wastewaters were collected in a company’s wastewater treatment plant, one after the use of zinc in the metal plating process and the other after the use of chromium. The main characteristics of the Zn(II) and Cr(VI) wastewaters are: pH = 6.7/5.9; chemical oxygen demand = 55/<5 mg/L; sodium, potassium, magnesium and calcium ions concentrations of 326/28, 4/28, 11/7 and 46/37 mg/L, respectively; zinc(II) = 11 mg/L and Cr(VI) = 39 mg/L. Batch studies showed that L. hyperborea can be established as a natural cation exchanger for heavy metals uptake mainly due to the presence of negatively charged functional groups in the surface of the biomass. Beyond that, L. hyperborea can be used as a natural electron donor for hexavalent chromium reduction to trivalent chromium at acidic medium through the oxidation of the biomass, and Cr(III) can be further bound to the negatively charged functional groups. The uptake capacity of Cr(III) by the oxidized biomass after Cr(VI) reduction was higher than by the algae in its original form. This can be attributed to the oxidation of the biomass during Cr(VI) reduction, turning other active sites available for Cr(III) binding. The brown macroalgae Laminaria hyperborea was packed in a fixed-bed column in order to evaluate the feasibility of the system for the continuous treatment of the two galvanization wastewaters. The column, with an internal diameter of 4.8 cm, was packed with 59 g of algae up to a bed height of 27 cm. The operation strategy adopted for the treatment of the two wastewaters consisted in: i) treatment of the Zn(II) wastewater in the first sorption cycle; ii) desorption of pre-loaded Zn(II) using an 1.0 M HCl solution; iii) treatment of the Cr(VI) wastewater, taking advantage of the acidic conditions of the column after the desorption cycle, for the reduction of the Cr(VI) to Cr(III), in the presence of the electrons resulting from the biomass oxidation. This cycle ends when all the oxidizing groups are used.

Keywords: biosorption, brown marine macroalgae, zinc, chromium

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Authors: Adnan I. O. Zaid

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Zinc aluminum alloys are versatile materials which are widely used in manufacturing several parts in the automobile and aircraft industries. The effect of grain refinement of these alloys by rare earth elements on their mechanical characteristics is scarce. The equal channel angular pressing is relatively recent method for producing severe plastic deformation in materials subjected to it resulting in refinement of their structure and enhancement of their mechanical characteristics. The phase diagram of these alloys indicates that large dendrites of large grain size can be formed during their solidification of the cast which tends to deteriorate their mechanical strength and surface quality. To overcome this problem they are normally grain refined by either titanium or titanium + boron to their melt prior to solidification. In this paper, comparison between the effect of adding either titanium, (Ti), titanium+boron, (Ti+B), or Molybdenum, Mo, to zinc-aluminum22, alloy, (ZA22) on its metallurgical and mechanical characteristics in the cast condition and after pressing by the ECAP process is investigated. It was found that addition of either Ti, Ti+B, or Mo to the ZA22 alloy in the cast condition resulted in refining of their structure being more refined by the addition of Mo, then .Ti+B and less refining by Ti addition. Furthermore, the ECAP process resulted in further refinement of the alloy micro structure except in case of Ti+B addition where poisoning i.e. coarsening of the grains has occurred. Regarding the addition of these element on the mechanical behavior; it was found that addition of Ti Or Ti+B resulted in little enhancement of the alloy strength factor and its flow stress at 20% true strain; whereas, the addition of resulted in deteriorating of its mechanical behavior as % decrease in the strength factor and % in its flow stress of 20%. As for the strain hardening index; addition of any of these elements resulted in decreasing the strain hardening index.

Keywords: addition, grain refinement, mechanical characteristics, microstructure, rare earth elements, ZA-22, Zinc- aluminum alloy

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Authors: Chiau Yuan Lim, Hayyiratul Fatimah Mohd Zaid, Fai Kait Chong

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Deep Eutectic Solvent (DES) is used in various applications due to its simplicity in synthesis procedure, biodegradable, inexpensive and easily available chemical ingredients. Graphene Oxide is a popular catalyst that being used in various processes due to its stacking carbon sheets in layer which theoretically rapid up the catalytic processes. In this study, choline chloride based DESs were synthesized and ChCl-PEG(1:4) was found to be the most effective DES in performing desulfurization, which it is able to remove up to 47.4% of the sulfur content in the model oil in just 10 minutes, and up to 95% of sulfur content after repeat the process for six times. ChCl-PEG(1:4) able to perform up to 32.7% desulfurization on real diesel after 6 multiple stages. Thus, future research works should focus on removing the impurities on real diesel before utilising DESs in petroleum field.

Keywords: choline chloride, deep eutectic solvent, fuel desulfurization, graphene oxide

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Authors: L. Khalfa, M. Bagane, M. L. Cervera, S. Najjar

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The aim of this work is to present a low cost adsorbent for removing toxic heavy metals from aqueous solutions. Therefore, we are interested to investigate the efficiency of natural clay minerals collected from south Tunisia and their modified form using sulfuric acid in the removal of toxic metal ions: Zn(II) and Pb(II) from synthetic waste water solutions. The obtained results indicate that metal uptake is pH-dependent and maximum removal was detected to occur at pH 6. Adsorption equilibrium is very rapid and it was achieved after 90 min for both metal ions studied. The kinetics results show that the pseudo-second-order model describes the adsorption and the intraparticle diffusion models are the limiting step. The treatment of natural clay with sulfuric acid creates more active sites and increases the surface area, so it showed an increase of the adsorbed quantities of lead and zinc in single and binary systems. The competitive adsorption study showed that the uptake of lead was inhibited in the presence of 10 mg/L of zinc. An antagonistic binary adsorption mechanism was observed. These results revealed that clay is an effective natural material for removing lead and zinc in single and binary systems from aqueous solution.

Keywords: heavy metal, activated clay, kinetic study, competitive adsorption, modeling

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Authors: Farida Kaouah, Chahida Oussalah, Wassila Hachi, Salim Boumaza, Mohamed Trari

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A catalyst of ZnO nanoparticles was used in the photocatalytic process of treatment for potential use towards bisphenol A (BPA) degradation in an aqueous solution. To achieve this study, the effect of parameters such as the catalyst dose, initial concentration of BPA and pH on the photocatalytic degradation of BPA was studied. The results reveal that the maximum degradation (more than 93%) of BPA occurred with ZnO catalyst in 120 min of stirring at natural pH (7.1) under solar light irradiation. It was found that chemical oxygen demand (COD) reduction takes place at a faster rate under solar light as compared to that of UV light. The kinetic studies were achieved and revealed that the photocatalytic degradation process obeyed a Langmuir–Hinshelwood model and followed a pseudo-first order rate expression. This work envisages the great potential that sunlight mediated photocatalysis has in the removal of bisphenol A from wastewater.

Keywords: bisphenol A, photocatalytic degradation, sunlight, zinc oxide, Langmuir–Hinshelwood model, chemical oxygen demand

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Authors: Qifei Jing, Vadim V. Silberschmidt, Lin Li, ZhiLi Dong

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Graphene oxide (GO) was chemically functionalized to prepare polyurethane (PU) composites with improved mechanical and thermal properties. In order to achieve a well exfoliated and stable GO suspension in an organic solvent (dimethylformamide, DMF), 4, 4′- methylenebis(phenyl isocyanate) and polycaprolactone diol, which were the two monomers for synthesizing PU, were selectively used to functionalize GO. The obtained functionalized GO (FGO) could form homogeneous dispersions in DMF solvent and the PU matrix, as well as provide a good compatibility with the PU matrix. The most efficient improvement of mechanical properties was achieved when 0.4 wt% FGO was added into the PU matrix, showing increases in the tensile stress, elongation at break and toughness by 34.2%, 27.6% and 64.5%, respectively, compared with those of PU. Regarding the thermal stability, PU filled with 1 wt% FGO showed the largest extent of improvement with T2% and T50% (the temperatures at which 2% and 50% weight-loss happened) 16 °C and 21 °C higher than those of PU, respectively. The significant improvement in both mechanical properties and thermal stability of FGO/PU composites should be attributed to the homogeneous dispersion of FGO in the PU matrix and strong interfacial interaction between them.

Keywords: composite, dispersion, graphene oxide, polyurethane

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Authors: Pavel Baroch, Jiri Rezek, Michal Prochazka, Tomas Kozak, Jiri Houska

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Transparent semiconducting amorphous IGZO films have attracted great attention due to their excellent electrical properties and possible utilization in thin film transistors or in photovoltaic applications as they show 20-50 times higher mobility than that of amorphous silicon. It is also known that the properties of IGZO films are highly sensitive to process parameters, especially to oxygen partial pressure. In this study we have focused on the comparison of properties of transparent semiconducting amorphous indium gallium zinc oxide (IGZO) thin films prepared by conventional sputtering methods and those prepared by high power impulse magnetron sputtering (HiPIMS) method. Furthermore we tried to optimize electrical and optical properties of the IGZO thin films and to investigate possibility to apply these coatings on thermally sensitive flexible substrates. We employed dc, pulsed dc, mid frequency sine wave and HiPIMS power supplies for magnetron deposition. Magnetrons were equipped with sintered ceramic InGaZnO targets. As oxygen vacancies are considered to be the main source of the carriers in IGZO films, it is expected that with the increase of oxygen partial pressure number of oxygen vacancies decreases which results in the increase of film resistivity. Therefore in all experiments we focused on the effect of oxygen partial pressure, discharge power and pulsed power mode on the electrical, optical and mechanical properties of IGZO thin films and also on the thermal load deposited to the substrate. As expected, we have observed a very fast transition between low- and high-resistivity films depending on oxygen partial pressure when deposition using conventional sputtering methods/power supplies have been utilized. Therefore we established and utilized HiPIMS sputtering system for enlargement of operation window for better control of IGZO thin film properties. It is shown that with this system we are able to effectively eliminate steep transition between low and high resistivity films exhibited by DC mode of sputtering and the electrical resistivity can be effectively controlled in the wide resistivity range of 10-² to 10⁵ Ω.cm. The highest mobility of charge carriers (up to 50 cm2/V.s) was obtained at very low oxygen partial pressures. Utilization of HiPIMS also led to significant decrease in thermal load deposited to the substrate which is beneficial for deposition on the thermally sensitive and flexible polymer substrates. Deposition rate as a function of discharge power and oxygen partial pressure was also systematically investigated and the results from optical, electrical and structure analysis will be discussed in detail. Most important result which we have obtained demonstrates almost linear control of IGZO thin films resistivity with increasing of oxygen partial pressure utilizing HiPIMS mode of sputtering and highly transparent films with low resistivity were prepared already at low pO2. It was also found that utilization of HiPIMS technique resulted in significant improvement of surface smoothness in reactive mode of sputtering (with increasing of oxygen partial pressure).

Keywords: charge carrier mobility, HiPIMS, IGZO, resistivity

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Authors: S. F. H. Tasfy, N. A. M. Zabidi, M. S. Shaharun

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Carbon dioxide is highly thermochemical stable molecules where it is very difficult to activate the molecule and achieve higher catalytic conversion into alcohols or other hydrocarbon compounds. In this paper, series of the bimetallic Cu/ZnO-based catalyst supported by SBA-15 were systematically prepared via impregnation technique with different Cu: Zn ratio for hydrogenation of CO₂ to methanol. The synthesized catalysts were characterized by transmission electron microscopy (TEM), temperature programmed desorption, reduction, oxidation and pulse chemisorption (TPDRO), and surface area determination was also performed. All catalysts were tested with respect to the hydrogenation of CO₂ to methanol in microactivity fixed-bed reactor at 250^oC, 2.25 MPa, and H₂/CO₂ ratio of 3. The results demonstrate that the catalytic structure, activity, and methanol selectivity was strongly affected by the ratio between Cu: Zn, Where higher catalytic activity of 14 % and methanol selectivity of 92 % was obtained over Cu/ZnO-SBA-15 catalyst with Cu:Zn ratio of 7:3 wt. %. Comparing with the single catalyst, the synergetic between Cu and Zn provides additional active sites to adsorb more H₂ and CO₂ and accelerate the CO₂ conversion, resulting in higher methanol production under mild reaction conditions.

Keywords: hydrogenation of carbon dioxide, methanol synthesis, Cu/ZnO-based catalyst, mesoporous silica (SBA-15), metal ratio

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Authors: Martin Juckel

Abstract:

Probably no other field of inorganic chemistry has undergone such a rapid development in the past two decades than the low oxidation state chemistry of main group elements. This rapid development has only been possible by the development of new bulky ligands. In case of our research group, super-bulky monodentate amido ligands and β-diketiminate ligands have been used to a great success. We first synthesized the unprecedented magnesium(I) dimer [ᴹᵉˢNacnacMg]₂ (ᴹᵉˢNacnac = [(ᴹᵉˢNCMe)₂CH]-; Mes = mesityl, which has since been used both as reducing agent and also for the synthesis of new metal-magnesium bonds. In case of the zinc bromide precursor [L*ZnBr] (L*=(N(Ar*)(SiPri₃); (Ar* = C₆H₂{C(H)Ph₂}₂Me-2,6,4, the reduction with [ᴹᵉˢNacnacMg]₂ led to such a metal-magnesium bond. This [L*ZnMg(ᴹᵉˢNacnac)] compound can be seen as an ‘inorganic Grignard reagent’, which can be used to transfer the metal fragment onto other functional groups or other metal centers; just like the conventional Grignard reagent. By simple addition of (TBoN)GeCl (TBoN = N(SiMe₃){B(DipNCH)₂) to the aforesaid compound, we were able to transfer the amido-zinc fragment to the Ge center of the germylene starting material and to synthesize the first example of a germanium(II)-zinc bond: [:Ge(TBoN)(ZnL*)]. While these reactions typically led to complex product mixture, [:Ge(TBoN)(ZnL*)] could be isolated as dark blue crystals in a good yield. This new compound shows interesting reactivity towards small molecules, especially dihydrogen gas. This is of special interest as dihydrogen is one of the more difficult small molecules to activate, due to its strong (BDE = 108 kcal/mol) and non-polar bond. In this context, the interaction between H₂ σ-bond with the tetrelylene p-Orbital (LUMO), with concomitant donation of the tetrelylene lone pair (HOMO) into the H₂ σ* orbital are responsible for the activation of dihydrogen gas. Accordingly, the narrower the HOMO-LUMO gap of tertelylene, the more reactivity towards H₂ it typically is. The aim of a narrow HOMO-LUMO gap was reached by transferring electropositive substituents respectively metal substituents with relatively low Pauling electronegativity (zinc: 1.65) onto the Ge center (here: the zinc-amido fragment). In consideration of the unprecedented reactivity of [:Ge(TBoN)(ZnL*)], a computational examination of its frontier orbital energies was undertaken. The energy separation between the HOMO, which has significant Ge lone pair character, and the LUMO, which has predominantly Ge p-orbital character, is narrow (40.8 kcal/mol; cf.∆S-T= 24.8 kcal/mol), and comparable to the HOMO-LUMO gaps calculated for other literature known complexes). The calculated very narrow HOMO-LUMO gap for the [:Ge(TBoN)(ZnL*)] complex is consistent with its high reactivity, and is remarkable considering that it incorporates a π-basic amide ligand, which are known to raise the LUMO of germylenes considerably.

Keywords: activation of dihydrogen gas, narrow HOMO-LUMO gap, first germanium(II)-zinc bond, inorganic Grignard reagent

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Authors: Arjun Dakuri, J. Hayavadana

Abstract:

The study includes selection of 100 % bamboo fabric and cotton fabric for the study. The 100% bamboo fabrics were of 127 g/m², and 112 g/m² and 100% cotton grey fabric were of 104 g/m². The cotton fabric was desized, scoured, bleached and then treated with ZnO (as antimicrobial agent) with 1%, 2% and 3% using pad-dry cure method, whereas the bamboo fabrics were only desized. The antimicrobial activity of bamboo and ZnO treated cotton fabrics were evaluated and compared against E. coli and S. aureus as per the standard AATCC - 147. Moisture management properties of selected fabrics were also analyzed. Further, the selected fabric samples were tested for comfort properties like bending length, tearing strength, drape-ability, and specific handle force and air permeability. It was observed that bamboo fabrics show significant antibacterial activity and the same was shown by 3% ZnO treated cotton fabric. Both cotton and bamboo fabrics show improved moisture management properties than the cotton fabric. The comfort properties of bamboo fabrics are found to be superior to cotton fabrics making it more suitable for applications in place of cotton.

Keywords: antimicrobial activity, bamboo, cotton, comfort properties, moisture management, zinc oxide

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Authors: Piyaporn Buaklang, Narisa Kengtrong Bordeerat

Abstract:

The use of nanoparticles is increasing worldwide and there are many nanotech-based daily products available in the market. The toxicity of nanoparticles results from their extremely small size which can be transported easily into the blood stream and other organs. We aimed to study the genotoxicity of two nanoparticles, Titanium dioxide (TiO2-NPs) and Zinc oxide (ZnO-NPs), in TK6 cells by micronucleus assay. The cells were tested at 8, 24, and 48 hours after exposed to 0.10, 0.25, 0.50 and 1.00 µg/mL of TiO2-NPs particles size < 25 nm and < 100 nm and to ZnO-NPs at 1, 10, 50, and 100 µg/mL, particles size < 50 nm and < 100 nm. At 24 hours of incubation transmission electron microscope (TEM) revealed that the nanoparticles TiO2-NPs at 1.00 µg/mL and ZnO-NPs at 10 µg/mL were able to be taken into the cells and induced the production of increasing amount of micronucleus in dose-dependent manner. The effect of the two nanoparticles on chromosome aberration indicated that TiO2-NPs and ZnO-NPs are genotoxic. In addition, the toxicity of TiO2-NPs was found to be 10 times more toxic than ZnO-NPs after 24 hours exposure. Analysis showed that the TiO2-NPs induced formation of micronucleus was both time and dose dependent, whereas the genotoxicity of ZnO-NPs was only dose dependent. In conclusion, TiO2-NPs and ZnO-NPs were able to transport through the cells membrane and directly genotoxic to TK6 cells in dose-dependent manner.

Keywords: nanoparticles, genotoxicity, human lymphoblast cells (TK6), micronucleus

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Authors: Tripti Singhal, C. Tara Satyavathi, S. P. Singh, Aruna Kumar, Mukesh Sankar S., C. Bhardwaj, Mallik M., Jayant Bhat, N. Anuradha, Nirupma Singh

Abstract:

Pearl millet is a climate-resilient nutritious crop. We report iron and zinc content QTLs from 3 divergent locations. The content of grain Fe in the RILs ranged between 36 and 114 mg/kg, and that of Zn from 20 to 106 mg/kg across the three years at over 3 locations (Delhi, Dharwad, and Jodhpur). We used SSRs to generate a linkage map using 210 F₆ RIL derived from the (PPMI 683 × PPMI 627) cross. The linkage map of 151 loci was 3403.6 cM in length. QTL analysis revealed a total of 22 QTLs for both traits at all locations. Inside QTLs, candidate genes were identified using bioinformatics approaches.

Keywords: yield, pearl millet, QTL mapping, multi-environment, RILs

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Authors: Juiwen Liang, Choliang Chung

Abstract:

In this study, the silicon-base oxide nanofibers with hollow structure were prepared using single-nozzle electrospinning and heat treatment. Firstly, precursor solution was prepared: the Polyvinylpyrrolidone (PVP) and Tetraethyl orthosilicate (TEOS) dissolved in ethanol and to make sure the concentration of solution in appropriate using single-nozzle electrospinning to produce the nanofibers. Secondly, control morphology of the electrostatic spinning nanofibers was conducted, and design the temperature profile to created hollow nanofibers, exploring the morphology and properties of nanofibers. The characterized of nanofibers, following instruments were used: Atomic force microscopy (AFM), Field Emission Scanning Electron Microscope (FE-SEM), Transmission electron microscopy (TEM), Photoluminescence (PL), X-ray Diffraction (XRD). The AFM was used to scan the nanofibers, and 3D Graphics were applied to explore the surface morphology of fibers. FE-SEM and TEM were used to explore the morphology and diameter of nanofibers and hollow nanofiber. The excitation and emission spectra explored by PL. Finally, XRD was used for identified crystallization of ceramic nanofibers. Using electrospinning technique followed by subsequent heat treatment, we have successfully prepared silicon-base oxide nanofibers with hollow structure. Thus, the microstructure and morphology of electrostatic spinning silicon-base oxide hollow nanofibers were explored. Major characteristics of the nanofiber in terms of crystalline, optical properties and crystal structure were identified.

Keywords: electrospinning, single-nozzle, hollow, nanofibers

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Authors: Abderrahmane Hamdi, Julie Chalon, Benoit Dodin, Philippe Champagne

Abstract:

This research work concerns the synthesis of hydrophobic and self-cleaning coatings as an alternative to fluorine-based coatings used on glass. The developed, highly transparent coatings are produced by a chemical route (sol-gel method) using two silica-based precursors, hexamethyldisilazane and tetraethoxysilane (HMDS/TEOS). The addition of zinc oxide nanoparticles (ZnO NPs) within the gel provides a photocatalytic property to the final coating. The prepared gels were deposited on glass slides using different methods. The properties of the coatings were characterized by optical microscopy, scanning electron microscopy, UV-VIS-NIR spectrophotometer, and water contact angle method. The results show that the obtained coatings are homogeneous and have a hydrophobic character. In particular, after thermal treatment, the HMDS/TEOS@ZnO charged gel deposited on glass constitutes a coating capable of degrading methylene blue (MB) under UV irradiation. Optical transmission reaches more than 90% in most of the visible light spectrum. Synthetized coatings have also demonstrated their mechanical durability and self-cleaning ability.

Keywords: coating, durability, hydrophobicity, sol-gel, self-cleaning, transparence

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Authors: Ould Mohamed Cheikh, Mounir Chaik, Hind El Aakib, Mohamed Aggour, Abdelkader Outzourhit

Abstract:

Zinc sulfide [ZnS] and oxygenated zinc sulfide Zn(O,S) thin films were deposited on glass substrates, by reactive cathodic radio-frequency (RF) sputtering. The substrates power and percentage of oxygen were varied in the range of 100W to 250W and from 5% to 20% respectively. The structural, morphological and optical properties of these thin films were investigated. The optical properties (mainly the refractive index, absorption coefficient and optical band gap) were examined by optical transmission measurements in the ultraviolet-visible-near Infrared wavelength range. XRD analysis indicated that all sputtered ZnS films were a single phase with a preferential orientation along the (111) plane of zinc blend (ZB). The crystallite size was in the range of 19.5 nm to 48.5 nm, the crystallite size varied with RF power reaching a maximum at 200 W. The Zn(O,S) films, on the other hand, were amorphous. UV-Visible, measurements showed that the ZnS film had more than 80% transmittance in the visible wavelength region while that of Zn(O,S is 85%. Moreover, it was observed that the band gap energy of the ZnS films increases slightly from 3.4 to 3.52 eV as the RF power was increased. The optical band gap of Zn(O,S), on the other hand, decreased from 4.2 to 3.89 eV as the oxygen partial pressure is increased in the sputtering atmosphere at a fixed RF-power. Scanning electron microscopy observations revealed smooth surfaces for both type of films. The X-ray reflectometry measurements on the ZnS films showed that the density of the films (3.9 g/cm3) is close that of bulk ZnS.

Keywords: thin films Zn(O, S) properties, Zn(O, S) by Rf-sputtering, ZnS for solar cells, thin films for renewable energy

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Authors: Farida Kaouah, Wassila Hachi, Lamia Brahmi, Chahida Ousselah, Salim Boumaza, Mohamed Trari

Abstract:

The feasibility of using solar irradiation instead of UV light in photocatalysis is a promising approach for water treatment. In this study, photocatalytic degradation of a widely used textile dye, Acid Blue 25 (AB25), with noble metal loaded ZnO photocatalyst (Ag/ZnO), was investigated in aqueous suspension under solar light. The results showed that the deposition of Ag as a noble metal onto the ZnO surface, improved the photodegradation of AB25. . The effect of different parameters such as catalyst dose, initial dye concentration, and contact time was optimized and the optimal degradation of AB25 (97%) was achieved for initial AB25 concentration of 24 mg L−1 an catalyst dose of 1 g L−1 at natural pH (5.42) after 180 min. The kinetic studies were achieved and revealed that the photocatalytic degradation process obeyed to Langmuir–Hinshelwood model and followed a pseudo-first order rate expression. This work envisages the great potential that sunlight photocatalysis has in the degradation of dyes from wastewater

Keywords: acid dye, photocatalytic degradation, sunlight, zinc oxide, noble metal, Langmuir–Hinshelwood model

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Authors: Uc-Cayetano E. G., Ake-Uh O. E., Villanueva-Mena I. E., Ordonez L. C.

Abstract:

Carbon nanotubes (CNTs) and other graphitic nanostructures are materials with extraordinary physical, physicochemical and electrochemical properties which are being aggressively investigated for a variety of sensing applications. Thus, sensing of biological molecules such as proteins, DNA, glucose and other enzymes using either single wall or multiwall carbon nanotubes (MWCNTs) has been widely reported. Despite the current progress in this area, the electrochemical response of CNTs used in a variety of sensing arrangements still needs to be improved. An alternative towards the enhancement of this CNTs' electrochemical response is to chemically (or physically) modify its surface. The influence of the decoration with iron oxide nanoparticles in different types of MWCNTs on the amperometric sensing of glucose, urea, and cholesterol in solution is investigated. Commercial MWCNTs were oxidized in acid media and subsequently decorated with iron oxide nanoparticles; finally, the enzymes glucose oxidase, urease, and cholesterol oxidase are chemically immobilized to oxidized and decorated MWCNTs for glucose, urease, and cholesterol electrochemical sensing. The results of the electrochemical characterizations consistently show that the presence of iron oxide nanoparticles decorating the surface of MWCNTs enhance the amperometric response and the sensitivity to increments in glucose, urease, and cholesterol concentration when compared to non-decorated MWCNTs.

Keywords: WCNTs, enzymes, oxidation, decoration

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Authors: Benjamin Kaufmann, Michael Hofstätter, Nadine Raidl, Peter Supancic

Abstract:

ZnO varistors are the leading overvoltage protection elements in today’s electronic industry. Their highly non-linear current-voltage characteristics, very fast response times, good reliability and attractive cost of production are unique in this field. There are challenges and questions unsolved. Especially, the urge to create even smaller, versatile and reliable parts, that fit industry’s demands, brings manufacturers to the limits of their abilities. Although, the varistor effect of sintered ZnO is known since the 1960’s, and a lot of work was done on this field to explain the sudden exponential increase of conductivity, the strict dependency on sinter parameters, as well as the influence of the complex microstructure, is not sufficiently understood. For further enhancement and down-scaling of varistors, a better understanding of the microscopic processes is needed. This work attempts a microscopic approach to investigate ZnO varistor performance. In order to cope with the polycrystalline varistor ceramic and in order to account for all possible current paths through the material, a preferably realistic model of the microstructure was set up in the form of three-dimensional networks where every grain has a constant electric potential, and voltage drop occurs only at the grain boundaries. The electro-thermal workload, depending on different grain size distributions, was investigated as well as the influence of the metal-semiconductor contact between the electrodes and the ZnO grains. A number of experimental methods are used, firstly, to feed the simulations with realistic parameters and, secondly, to verify the obtained results. These methods are: a micro 4-point probes method system (M4PPS) to investigate the current-voltage characteristics between single ZnO grains and between ZnO grains and the metal electrode inside the varistor, micro lock-in infrared thermography (MLIRT) to detect current paths, electron back scattering diffraction and piezoresponse force microscopy to determine grain orientations, atom probe to determine atomic substituents, Kelvin probe force microscopy for investigating grain surface potentials. The simulations showed that, within a critical voltage range, the current flow is localized along paths which represent only a tiny part of the available volume. This effect could be observed via MLIRT. Furthermore, the simulations exhibit that the electric power density, which is inversely proportional to the number of active current paths, since this number determines the electrical active volume, is dependent on the grain size distribution. M4PPS measurements showed that the electrode-grain contacts behave like Schottky diodes and are crucial for asymmetric current path development. Furthermore, evaluation of actual data suggests that current flow is influenced by grain orientations. The present results deepen the knowledge of influencing microscopic factors on ZnO varistor performance and can give some recommendations on fabrication for obtaining more reliable ZnO varistors.

Keywords: metal-semiconductor contact, Schottky diode, varistor, zinc oxide

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