Microwave sintering of nano-sized ZnO synthesized by a liquid route

Zinc oxide is a widely used material in various applications in electronic, optic, and spintronic fields, in particular. The control of the final properties of ZnO requires the mastering of the final microstructure. To achieve this goal, the grain growth of ZnO has been examined as a function of the sintering conditions, in particular in using a specific microwave sintering method. In order to get nano-sized ZnO powder as a starting material, a liquid route was implemented. The latter is based on the direct precipitation of a zinc oxalate solution. After thermal treatment, pure ZnO powder was obtained with a very narrow grain size distribution, centered at around 20 nm. The sintering of this powder was then carried out in conventional and microwave furnaces. While an important grain growth occurs during the conventional sintering, it is shown that microwave sintering allows us to maintain the grain size at the nano-metric scale.     

Hot pressing of nanocrystalline zinc oxide compacts: Densification and grain growth during sintering

Sintering behavior of nanocrystalline zinc oxide (ZnO) powder compacts using hot pressing method was investigated. The sintering conditions (temperature and total time) and results (density and grain size) of two-step sintering (TSS), conventional sintering (CS) and hot pressing (HP) methods were compared. The HP technique versus CS was shown to be a superior method to obtain higher final density (99%), lower sintering temperature, shorter total sintering time and rather fine grain size. The maximum density achieved via HP, TSS and CS methods were 99%, 98.3% and 97%, respectively. The final grain size of samples obtained by HP was greater than that of TSS method. However, the ultra-prolonged sintering total time and the lower final density (88 ks and 98.3%) are the drawbacks of TSS in comparison with the faster HP (17 ks and 99%) method.     

Characteristics of Optimized Al:ZnO sputtering targets prepared by nanostructured powder

Optimized Al:ZnO sputtering target was prepared by cold isostatic pressing (CIP) using nanostructured zinc oxide powder and aluminum oxide powder as raw material. Compared with the target prepared by conventional raw materials, the performance of the optimized Al:ZnO sputtering target is greatly improved. The microstructure of the optimized Al:ZnO sputtering target is refined and its average grain size is less than 5 μm with 99.7% theoretical density. Al:ZnO thin films of both optimized and conventional targets were prepared by RF magnetron sputter and their properties were characterized, respectively. The Al:ZnO thin films obtained by optimized target feature better uniformity and compactness, and the internal stress is −378.8 MPa, which is nearly 2/3 lower than that of the conventional target. The film obtained by optimized targets also features a 97% IR transmittance, 1.71 nm Rq surface roughness and non-offset (002) XRD peak. It can be speculated that the optimized Al:ZnO target has great potential to prepare micrometer scale Al:ZnO films and employed in thin-film ZnO device industry.     

Electric and microstructural characteristics of bulk ZnO fabricated by underwater shock compaction

An underwater shock compaction of pure zinc oxide (ZnO) powder has been performed. This technique uses an underwater shock wave generated by detonation of an explosive. Shock pressure used in this work was about 10 GPa. The morphology and structure of shock-consolidated ZnO was investigated by X-ray diffraction (XRD) method and scanning electron microscopy (SEM). The density and impedance characteristics of shock-consolidated ZnO were measured by Archimedes method and Nyquist plot method, respectively. The shock-consolidated ZnO without visible cracks was successfully obtained. It was confirmed that the shock-consolidated ZnO had 99% of theoretical density without grain growth and high grain boundary resistivity in comparison with the commercial sintered ZnO.     

Performance enhancement of multiple-gate ZnO metal-oxide-semiconductor field-effect transistors fabricated using self-aligned and laser interference photolithography techniques

The simple self-aligned photolithography technique and laser interference photolithography technique were proposed and utilized to fabricate multiple-gate ZnO metal-oxide-semiconductor field-effect transistors (MOSFETs). Since the multiple-gate structure could improve the electrical field distribution along the ZnO channel, the performance of the ZnO MOSFETs could be enhanced. The performance of the multiple-gate ZnO MOSFETs was better than that of the conventional single-gate ZnO MOSFETs. The higher the drain-source saturation current (12.41 mA/mm), the higher the transconductance (5.35 mS/mm) and the lower the anomalous off-current (5.7 μA/mm) for the multiple-gate ZnO MOSFETs were obtained.     

Preparation and characterizations of highly transparent UV-curable ZnO-acrylic nanocomposites

A sol–gel chemical route was adopted to prepare the zinc oxide (ZnO) nanoparticles as small as 4 nm. UV-curable ZnO-acrylic nanocomposites were then prepared by employing 3-(trimethoxysilyl)propyl methacrylate (TPMA) as the surface modification agent of ZnO particles. UV–vis analysis revealed a high optical transparency (>95%) in visible light region for nanocomposite thin films with ZnO contents up to 20 wt.%. The addition of ZnO nanoparticles also enhanced the dielectric constants of nanocomposites and the dielectric constants greater than 4 in frequencies ranging from 1 to 600 MHz was obtained in the samples containing 10 wt.% of ZnO nanoparticles. A comparison of experimental results and theoretical calculation indicated that the interfacial polarizations in between ZnO nanoparticles and polymer matrix may play an important role in the enhancement of dielectric properties of nanocomposites.     

Structural and electrical properties of 0.56Pb(Ni1/3Nb2/3)O3-0.10Pb(Zn1/3Nb2/3)O3-0.34PbTiO3 ceramics prepared by different ceramic processings

The ternary system of 0.56Pb(Ni_1/3Nb_2/3)O₃-0.10Pb(Zn_1/3Nb_2/3)O₃-0.34PbTiO₃ (0.56PNN-0.10PZN-0.34PT) ceramics were prepared by conventional solid-state reaction method via straight mixed oxide method, columbite precursor method and B-site oxide mixing route. X-ray diffraction (XRD) measurement demonstrated that both the tetragonal and rhombohedral phases coexist in the B-site oxide mixing route prepared ceramics accompanied by the largest content of perovskite phase of 95.18%. The 0.56PNN-0.10PZN-0.34PT ceramics prepared by the straight mixed oxide method and the B-site oxide mixing route exhibit rather homogeneous microstructure. As a comparison, in the columbite precursor method prepared ceramics nebulous granules and octahedral or other polyhedral morphology grains are observed. All the sintered ceramics exhibit diffused ferroelectric phase transition where the dielectric response peaks are broad, diffused and strongly frequency dependent. However, the temperature of dielectric maximum (T_m) increases greatly from 398.0 K of the 0.56PNN-0.10PZN-0.34PT ceramics prepared by the B-site oxide mixing route to 423.3 K of the ones prepared by the straight mixed oxide method. Saturated and symmetric P-E hysteresis loops are observed in all the sintered ceramics, where the B-site oxide mixing route prepared ceramics exhibit large value of remanent polarization (P_r) of 17.13 μC/cm² and the least value of coercive field (E_c) of 11.99 kV/cm. Piezoelectric constant (d₃₃) exhibits the largest value of 449 pC/N for the ceramics prepared by the B-site oxide mixing route. Such results are related to the phase composition, density and porosity of the ceramics.     

Photocatalytic degradation of Rhodamine B dye under UV/solar light using ZnO nanopowder synthesized by solution combustion route

Nano-sized ZnO powder with crystallite size in the range 12 to 50 nm were prepared by solution combustion route. The product was characterized by powder X-ray diffraction (PXRD), scanning electron microscope (SEM) and Fourier transform infrared spectroscopy (FTIR). Photocatalytic degradation of rhodamine B (RB) dye was carried out with ZnO nanopowder. The effect of parameters such as the crystallite size, amount of catalyst, concentration of the dye, pH and irradiation on photocatalytic degradation of RB is studied. The results reveal that the maximum decolorization (more than 95%) of dye occurred with ZnO catalyst in 8 min of stirring at basic pH under solar light irradiation. It was also found that chemical oxygen demand (COD) reduction takes place at a faster rate under solar light as compared to that of UV light. The results suggest that, the ZnO solar photocatalytic irradiation is better than the calcined ZnO/solar and UV light irradiation.     

Lanthanum Strontium Manganite Powders Synthesized by Gel-Casting for Solid Oxide Fuel Cell Cathode Materials

Lanthanum strontium manganite ((La_0.8Sr_0.2)_0.9MnO₃; LSM) powder was successfully synthesized by an aqueous gel-casting technique, using carbonaceous precursors. Both thermal and X-ray diffraction analysis confirmed that the gel-casting LSM powder formed a single perovskite phase at 850°C, which is 100°–150°C lower than that of the LSM powder prepared by the conventional solid-state reaction route. The significantly reduced phase formation temperature of the gel-casting LSM powder is most likely due to the homogeneously distributed and immobilized precursor particles in a polymeric network, promoting the sintering and crystallization process. The LSM electrode prepared by the gel-cast LSM powder showed good electrocatalytic activity for the O₂ reduction reaction for solid oxide fuel cells.     

Preparation and electrochemical performances of ZnO nanowires as anode materials for Ni/Zn secondary battery

ZnO nanowires were synthesized by a hydrothermal route without any substrate or template. Structure analyses through XRD, SEM, TEM and HRTEM indicated that ZnO nanowires had high purity and perfect crystallinity, and grew along [0 0 0 1]. The diameter was 50-80 nm, the length was about several micrometers and length-diameter ratio was more than 100. As electrode materials of Ni/Zn batteries, ZnO nanowires showed the obviously improved cycle stability, average discharge capacity of 609 mAh g⁻¹, higher discharge voltage/lower charge voltage. Slow rate cyclic voltammetry showed that electrochemical activity of ZnO nanowires was superior to that of the conventional ZnO. The improvements of electrochemical performance were ascribed to the unique nanowire structure. During the charging/discharging cycles, nanowires were broke, grew in diameter, and changed into nanorods. Nanowires lying parallel to the anodes could suppress the growth of dendrite clusters perpendicular to the anodes.     

Fluorine doped zinc oxide nanowires: Enhanced photocatalysts degrade malachite green dye under visible light conditions

Enhanced visible-light absorption of 4 at% fluorine (F) doped zinc oxide (ZnO) nanowires (F:ZnO) produced via a hydrothermal method with 15 M sodium hydroxide (NaOH) is explored with various characterization techniques: XRD, TEM, UV–vis spectra, Pl spectra, XPS, and surface area analysis. Moreover, photocatalytic performance of as-prepared samples is studied via degradation of malachite green dye under visible light irradiation. Finally, the photocatalyst’s optimal amount to use is determined as well as its recyclability. Results show that band gaps of ZnO nanostructures depend on NaOH concentration, doping 15 M NaOH resultant ZnO nanowires with 4 at% F further narrows the band gap, F:ZnO nanowires perform 1.6 times better than the pure ZnO nanowires in malachite green dye (MG) degradation tests, overloading the solution with the photocatalyst actually hinders degradation performance, and the F:ZnO photocatalyst remains a robust performer even after five cycles.     

Effect of ZnO seed layers on the solution chemical growth of ZnO nanorod arrays

High density ZnO nanorod arrays were grown on Si substrates coated with ZnO seed layers via aqueous solution route. The ZnO seed layers were deposited on the substrate using DC reactive sputtering and RF magnetron sputtering. It was found that ZnO seed layer with (1 0 3) preferred orientation, prepared using DC reactive sputtering, did not facilitate the formation of ZnO nanorods in the solution grown process. Prior seeding of the surface by ZnO layer with (0 0 2) preferred orientation, deposited using RF magnetron sputtering, leads to nucleation sites on which ZnO nanorod arrays can grow in a highly aligned fashion. ZnO nanorods with well-defined hexagonal facets (0 0 2) were grown almost vertically over the entire substrate. The uniformity and alignment of the nanorod arrays are strongly related to the properties of underneath ZnO seed layers.     

Synthesis and Activity of Heterogeneous Pd/Al2O3 and Pd/ZnO Catalysts Prepared from Colloidal Palladium Nanoparticles

Heterogeneous catalysts composed of Pd nanoparticles on zinc oxide (ZnO) and aluminum oxide (Al₂O₃, alumina) were synthesized and tested for catalytic activity. Palladium nanoparticles were synthesized via solution-precipitation methods and deposited on aluminum oxide and zinc oxide supports. The particles were synthesized by decomposing a palladium precursor (Pd(Mes)₂) in a solution of trioctylphosphine [TOP route] or palladium acetate (Pd(OAc)₂) in a solution of octylamine [amine route] at 300 °C. The particles were washed and suspended in hexane, whereupon they were deposited on an oxide powder. Supported nanoparticle powders were subjected to CO oxidation tests to determine catalytic activity. Particle sizes ranged from 2.4 ± 0.4 nm average diameter when prepared using trioctylphosphine to 4 ± 1 nm using the amine route. No significant size change was observed after removal of the surfactant and catalytic testing by CO oxidation. The highest conversion of CO to CO₂ occurred with a calcined sample, indicating that the removal of surfactant increases activity.     

Hydrothermal synthesis of different colors and morphologies of ZnO nanostructures and comparison of their photocatalytic properties

Various zinc oxide nanostructures were synthesized using thermal decomposition of zinc acetate dihydrate in a single process. The characterization of samples using powder X-ray diffraction, scanning electron microscope and FT-IR measurements revealed that the pure phase of different morphologies such as nanoparticles, nanowires and nanodisks had been synthesized successfully. Surprisingly some synthesized ZnO nanostructures were dark gray. The results showed that the reason may have been related to the oxygen deficiency and strong asymmetric stretching mode of wurtzite ZnO nanostructure. Using such samples, the photodegradation of Methylene blue was performed by UV–vis absorption measurement and the effect of morphology on the photocatalytic properties of different ZnO nanostructures was examined. The results showed that the nanodisks had the best photocatalytic performance among the other morphologies. The reason was attributed to the presence of specific crystal planes such as (0001) facets in nanodisks which can improve their photocatalytic performance.     

Microstructural evolution and contact-mechanical properties of SiC ceramics prepared colloidally with low additive content

The microstructural evolution and contact-mechanical properties of liquid-phase sintered (LPS) SiC ceramics processed colloidally with low loads of sintering additives was investigated as a function of the sintering duration, and was compared with the case of their counterparts processed conventionally. The two processing routes differ in the preparation of the powder batch, which in the colloidal method is done by covering the SiC particles with an oxide nano-film synthesized by the sol–gel method, whereas in the conventional method it is done by mixing mechanically the SiC powder with the oxide powders. It was found that the colloidal processing route offers clear benefits in terms of densification and contact-mechanical properties (stiffness, hardness, and damage and wear resistances) over the conventional processing route when the sintering times are short, but not when the sintering times are moderate or prolonged. Furthermore, no differences were found in the microstructural evolution with the sintering duration between the two types of ceramics. Based on the results, it is proposed that the more sophisticated colloidal processing route is certainly the appropriate choice for short sintering times, whereas in other cases its use would be justified if the goal is to incorporate into the microstructure new homogeneous multi-component oxide additives with tailored stoichiometry.     

Enhancement of the interfacial polarization resistance of La0.6Sr0.4Co0.2Fe0.8O3-δ cathode by microwave-assisted combustion method

Thermogravimetry, phase formation, microstructural evolution, specific surface area, and electrical properties of La_0.6Sr_0.4Co_0.2Fe_0.8O_3−δ (LSCF) cathode were studied as functions of its preparation technique. The pure perovskite LSCF cathode powder was synthesized through glycine–nitrate process (GNP) using microwave heating technique. Compared with conventional heating technique, microwave heating allows the rapid combustion to occur simultaneously between the nitrates and glycine in a controllable manner. The resulting powder is a single-phase nanocrystallite with a mean particle size of 113 nm and a high specific surface area of 12.2 m²/g, after calcination at 800 °C. Impedance analysis indicates that microwave heating has significantly reduced the polarization resistance of LSCF cathode. The area specific resistance (ASR) value of 0.059 and 0.097 Ω cm² at 800 °C and 750 °C, respectively, were observed. These values were twofold lower than the corresponding ASR of the cathode (0.133 and 0.259 Ω cm² at 800 °C and 750 °C, respectively) prepared through conventional heating. Results suggest that the microwave heating GNP strongly contributes to the enhancement of the LSCF cathode performance for intermediate temperature solid oxide fuel cells.     

Processing of different alumina–zirconia composites by slip casting

Two Al₂O₃–ZrO₂ mixture preparation routes: classical powder mixing and addition of a Zr (IV) precursor solution to a well dispersed Al₂O₃ suspension, were used to produce alumina (Al₂O₃)–zirconia (ZrO₂) slip cast composites. For the conventional powder mixing route, two commercial 3 mol% yttria-partially stabilized zirconia powders, 0.3 wt% Al₂O₃-doped (Al-doped Y-PSZ) and without Al₂O₃ (Y-PSZ), were employed. The influence of the zirconia content and the solid loading on the rheological properties of concentrated aqueous Al₂O₃–ZrO₂ slips were investigated. The density of green samples was studied and related to the degree of slip dispersion. In addition, the influence of the processing conditions on the density and microstructure development of sintered samples were investigated. By using the Zr (IV) precursor route, nano-sized ZrO₂ (ZN) particles homogeneously distributed on the Al₂O₃ particle surfaces were obtained; however, it let to aggregates of some Al₂O₃ particles with very fine ZrO₂ uniformly distributed. The viscosity and yield stress values of Al₂O₃–ZN suspensions were markedly higher than those of Al₂O₃–Al-doped Y-PSZ and Al₂O₃–Y-PSZ ones, for all the compositions and solid loading studied and resulted in a less dense packing of cast samples. However, for the composite with 10.5 vol% ZN a high sintered density and a smaller ZrO₂ grain size distribution compared with the conventional powder mixing route could be obtained.     

Synthesis of multi-shelled ZnO hollow microspheres and their improved photocatalytic activity

Herein, we report an effective, facile, and low-cost route for preparing ZnO hollow microspheres with a controlled number of shells composed of small ZnO nanoparticles. The formation mechanism of multiple-shelled structures was investigated in detail. The number of shells is manipulated by using different diameters of carbonaceous microspheres. The products were characterized by X-ray powder diffraction, scanning electron microscopy, and transmission electron microscopy. The as-prepared ZnO hollow microspheres and ZnO nanoparticles were then used to study the degradation of methyl orange (MO) dye under ultraviolet (UV) light irradiation, and the triple-shelled ZnO hollow microspheres exhibit the best photocatalytic activity. This work is helpful to develop ZnO-based photocatalysts with high photocatalytic performance in addressing environmental protection issues, and it is also anticipated to other multiple-shelled metal oxide hollow microsphere structures.     

Influence of nanocrystalline diamond powder on the growth and photoluminescence of open-ended ZnO nanorods

This paper reports the influence of introducing nanocrystalline diamond powder on the growth and photoluminescence of ZnO nanorods fabricated by hydrothermal technique. The majority of ZnO nanorods show an open-ended feature due to the addition of nano-diamond powder in the reaction solution. It is speculated that the diamond nanocrystallines dropped on the top of the growing ZnO nanorods would suppress the further growth at the localized positions to form the open-ended nanorods. The photoluminescence spectra of the ZnO products show the band-edge-related UV emission of ZnO nanorods at ~ 380 nm, in addition to a broad visible band centered at about 650 nm, which may originate from the emissions related to defects in the open-ended ZnO nanorods. The open-ended ZnO nanorods and/or combined with diamond nanocrystallines would be favorable for potential applications including UV sensors, electron field emitter, and various photoelectric nanodevices.     

A comparative study on UV light activated porous TiO2 and ZnO film sensors for gas sensing at room temperature

In order to find a new approach for screening the photoactivated gas sensing materials with high sensitivity, a comparative study was carried out. With the simple technique of screen printing, TiO₂ and ZnO were used to fabricate the UV light activated gas sensors which were applied at room temperature. To facilitate the simultaneous measurements of the current transients of the two materials, they were printed on the same alumina substrate. Compared with ZnO, TiO₂ exhibited a superior performance to ethanol and formaldehyde gases. It was found that the responses of TiO₂ increased with the concentration of test gas and amounted to 224 and 1700 to 100 ppm ethanol and formaldehyde gases, respectively, while the responses of ZnO to 100 ppm ethanol and formaldehyde gases were 0.14 and 1.5, respectively. The mechanism of such a huge difference between TiO₂ and ZnO was discussed in detail. Furthermore, it is suggested that metal oxide semiconductor with lower photo-to-dark current ratio can achieve higher photoactivated gas sensitivity.