Facile Solvothermal Synthesis and Gas Sensitivity of Graphene/WO3 Nanocomposites

Graphene has attracted enormous attention owing to its extraordinary properties, while graphene-based nanocomposites hold promise for many applications. In this paper, we present a two-step exploitation method for preparation of graphene oxides and a facile solvothermal route for preparation of few-layer graphene nanosheets and graphene/WO₃ nanocomposites in an ethanol-distilled water medium. The as-synthesized samples were characterized by using field emission scanning electron microscopy (FE-SEM), high-resolution transmission electron microscopy (HRTEM), ultraviolet-visible (UV-vis) spectroscopy, Raman spectroscopy, X-ray diffraction (XRD), thermogravimetric-differential thermal analysis (TG-DTA) and gas-sensing test. The resistivity of the thick-film gas sensors based on sandwich-like graphene/WO₃ nanocomposites can be controlled by varying the amount of graphene in the composites. Graphene/WO₃ nanocomposites with graphene content higher than 1% show fast response, high selectivity and fine sensitivity to NO_x.     

One-Step Microwave-Assisted Synthesis and Visible-Light Photocatalytic Activity Enhancement of BiOBr/RGO Nanocomposites for Degradation of Methylene Blue

In this study, bismuth oxybromide/reduced graphene oxide (BiOBr/RGO), i.e. BiOBr-G nanocomposites, were synthesized using a one-step microwave-assisted method. The structure of the synthesized nanocomposites was characterized using Raman spectroscopy, X-ray diffractometry (XRD), photoluminescence (PL) emission spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier-transform infrared spectroscopy (FTIR), and ultraviolet-visible diffuse reflection spectroscopy (DRS). In addition, the ability of the nanocomposite to degrade methylene blue (MB) under visible light irradiation was investigated. The synthesized nanocomposite achieved an MB degradation rate of above 96% within 75 min of continuous visible light irradiation. In addition, the synthesized BiOBr-G nanocomposite exhibited significantly enhanced photocatalytic activity for the degradation of MB. Furthermore, the results revealed that the separation of the photogenerated electron–hole pairs in the BiOBr-G nanocomposite enhanced the ability of the nanocomposite to absorb visible light, thus improving the photocatalytic properties of the nanocomposites. Lastly, the MB photo-degradation mechanism of BiOBr-G was investigated, and the results revealed that the BiOBr-G nanocomposites exhibited good photocatalytic activity.     

ZnO Semiconductor Nanoparticles and Their Application in Photocatalytic Degradation of Various Organic Dyes

The biosynthesis of oxide semiconductor nanoparticles (NPs) using materials found in nature opens a wide field of study focused on sustainability and environmental protection. Biosynthesized NPs have the capacity to eliminate organic dyes, which pollute water and cause severe damage to the environment. In the present work, the green synthesis of zinc oxide (ZnO) NPs was carried out using Capsicum annuum var. Anaheim extract. The photocatalytic elimination of methylene blue (MB), methyl orange (MO), and Rhodamine B (RhB) in UV radiation was evaluated. The materials were characterized by scanning and transmission electron microscopy (SEM and TEM) and SEM-coupled energy dispersive spectroscopy (EDS), attenuated total reflectance-infrared (ATR-IR), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), Photoluminescence (PL), and ultraviolet-visible spectroscopy (UV-Vis). The TEM analysis showed the NPs have an average size of 40 nm and quasi-spherical shape. ATR-IR showed the ZnO NPs contained functional groups from the extract. The analysis through XRD indicated that the NPs have a hexagonal zincite crystal structure with an average crystallite size of approximately 17 nm. The photoluminescence spectrum (PL) presented an emission band at 402 nm. From the UV-Vis spectra and TAUC model, the band-gap value was found to be 2.93 eV. Finally, the photocatalytic assessment proved the ZnO NPs achieved 100% elimination of MB at 60 min exposure, and 85 and 92% degradation of MO and RhB, respectively, at 180 min. This indicates that ZnO NPs, in addition to using a friendly method for their synthesis, manage to have excellent photocatalytic activity in the degradation of various organic pollutants.     

Surface Structure Analysis of Initial High-Temperature Oxidation of SS441 Stainless Steel

Chromia-forming ferritic stainless steel (FSS) is a highly promising interconnect material for application in solid oxide fuel cells. In this study, initial oxidation of chromium oxides was performed at 500–800 °C to understand the evolution of materials at an early stage. The structural variations in oxide scales were analyzed through scanning electron microscopy, energy dispersive spectroscopy (EDS), transmission electron microscopy (TEM), X-ray diffractometry (XRD), laser confocal microscopy (LSCM), X-ray photoelectron spectroscopy (XPS), and Raman spectroscopy. Surface electrochemical properties were investigated through electrochemical impedance spectroscopy to understand how the heat treatment temperature affected surface impedance. Treatment temperatures higher than 700 °C facilitate the diffusion of Cr and Mn, thus allowing ferritic spinels to form on the surface and leading to high electrical conductivity.     

Heterostructural Mixed Oxides Prepared via ZnAlLa LDH or ex-ZnAl LDH Precursors—Effect of La Content and Its Incorporation Route

The effect of La content and its incorporation route on physicochemical properties of ZnO/Zn(Al,La)₂O₄ or La₂O₃–ZnO/ZnAl₂O₄ mixed oxides with a spinel structure obtained from ZnAlLa Layered double hydroxides (LDHs) or ex-ZnAl LDH materials was investigated. The heterostructural nanocomposites with the similar Zn/Al molar ratio and varied La content were prepared by two techniques: via co-precipitation and thermal treatment of ZnAlLa LDHs at 500 °C or via incipient wetness impregnation of ex-ZnAl LDHs with aqueous solutions of lanthanum nitrate and subsequent thermal treatment. The obtained series of materials were characterized by the following techniques: X-ray fluorescence (XRF), N₂ adsorption (BET), X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), thermogravimetric analysis with evolved gas analysis (TG/DTG/EGA), scanning transmission electron microscopy (STEM) energy-dispersive X-ray spectroscopy (EDS), high-resolution transmission electron microscopy (HRTEM) and Fourier-transform infrared spectroscopy (FFT). The evaluation of activity toward the high-temperature water gas shift (HT-WGS) within the temperature range of 350–420 °C was carried out on the basis of rate constant measurements in the kinetic mode using a differential reactor. The co-precipitation technique allowed for a better distribution of La in bulk and on the spinel surface than in case of lanthanum incorporation via impregnation. ZnO/Zn(Al,La)₂O₄ or La₂O₃–ZnO/ZnAl₂O₄ mixed oxides were characterized by moderate activity in the HT-WGS reaction. The results reveal that introduction of lanthanum oxide over 2.4–2.8 wt% induces the phase separation of the ZnAl₂O₄ spinel, forming ZnO on the ZnAl₂O₄ spinel surface.     

Polypyrrole Decorated Flower-like and Rod-like ZnO Composites with Improved Microwave Absorption Performance

In this study, zinc oxide (ZnO)/polypyrrole (PPy) composites with flower- and rod-like structures were successfully fabricated by in situ polymerization and the hydrothermal method and used as microwave absorption (MWA) materials. The surface morphologies, crystal structures, and electromagnetic features of the as-prepared samples were measured by field-emission scanning electron microscopy (FE-SEM), energy dispersive spectroscopy (EDS), X-ray diffraction (XRD), and vector network analyzer (VNA). The results show that the conductive polymer PPy was successfully decorated on the surface of ZnO substrates. The MWA ability of flower- and rod-like ZnO/PPy composites is significantly enhanced after introduction of PPy. Rod-like ZnO/PPy composites exhibited superior MWA properties than those of flower-like ZnO/PPy. The former achieved a minimum reflection loss (RL_min) of −59.7 dB at 15.8 GHz with a thickness of 2.7 mm, and the effective absorption bandwidth (EAB, RL < −10 dB) covered 6.4 GHz. PPy addition and stacked structure of rod-like ZnO/PPy composites can effectively improve the dielectric properties, form multiple reflections of incident electromagnetic waves, and generate an interfacial polarization effect, resulting in improved MWA properties of composite materials.     

Near Infrared Investigation of Polypropylene–Clay Nanocomposites for Further Quality Control Purposes—Opportunities and Limitations

Polymer nanocomposites are usually characterized using various methods, such as small angle X-ray diffraction (XRD) or transmission electron microscopy, to gain insights into the morphology of the material. The disadvantages of these common characterization methods are that they are expensive and time consuming in terms of sample preparation and testing. In this work, near infrared spectroscopy (NIR) spectroscopy is used to characterize nanocomposites produced using a unique twin-screw mini-mixer, which is able to replicate, at ~25 g scale, the same mixing quality as in larger scale twin screw extruders. We correlated the results of X-ray diffraction, transmission electron microscopy, G′ and G″ from rotational rheology, Young’s modulus, and tensile strength with those of NIR spectroscopy. Our work has demonstrated that NIR-technology is suitable for quantitative characterization of such properties. Furthermore, the results are very promising regarding the fact that the NIR probe can be installed in a nanocomposite-processing twin screw extruder to measure inline and in real time, and could be used to help optimize the compounding process for increased quality, consistency, and enhanced product properties.     

Investigation on Variables Contributing to the Synthesis of C-S-H/PCE Nanocomposites by Co-Precipitation Method

The usage of nanoscale calcium silicate hydrate (nano C-S-H) proved to have an excellent promotion effect on the early performance of concrete as nano C-S-H with ultra-fine particle size can act as seeding for cement hydration. Therefore, it is of importance to tune the particle size during the synthesis process of nano C-S-H. In this paper, the influence of several variables of the particle size distribution (PSD) of nano C-S-H synthesized by chemical co-precipitation method with the aid of polycarboxylate (PCE) was studied by orthogonal experimental design. In addition, the composition, microstructure, and morphology of the C-S-H/PCE nanocomposites were analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Raman spectrum. The results showed that the concentration of reactants had a significant impact on the PSD of C-S-H/PCE nanocomposites, followed by the dosage of dispersant. Ultrasonic treatment was effective in breaking the C-S-H/PCE aggregates with unstable agglomeration structures. The change in synthetic variables had a negligible effect on the composition of the C-S-H/PCE nanocomposites but had a significant influence on the crystallinity and morphology of the composites.     

Synthesis of Nylon 6/Modified Carbon Black Nanocomposites for Application in Uric Acid Adsorption

High uric acid levels cause different clinic conditions. One of them is hyperuricemia, which leads to kidney damage. A solution for eliminating uric acid in the blood is by hemodialysis, which is performed using nanocomposite membranes. In this work, Nylon 6 nanocomposites were synthesized with modified carbon black (MCB), which were considered candidate materials for hemodialysis membranes. The modification of carbon black was made with citric acid using the variable-frequency ultrasound method. The new MCB was characterized by Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), X-ray diffraction (XRD), transmission electron microscopy (TEM), and dispersion tests. Nylon 6/MCB nanocomposites were processed using the ultrasound-assisted melt-extrusion method to improve the dispersion procedure of the nanoparticles. The Nylon 6/MCB nanocomposites were characterized by FTIR, TGA, and differential scanning calorimetry (DSC). These were assessed for the absorption of toxins and hemocompatibility. MBC and nanocomposites showed excellent uric acid removal (78–82%) and hemocompatibility (1.6–1.8%). These results suggest that Nylon 6/MCB nanocomposites with low loading percentages can be used on a large scale without compatibility problems with blood.     

Structural and Electrical Characterization of Pure and Al-Doped ZnO Nanorods

Pure and Al-doped (3 at.%) ZnO nanorods were prepared by two-step synthesis. In the first step, ZnO thin films were deposited on silicon wafers by spin coating; then, ZnO nanorods (NR) and Al-doped ZnO NR were grown using a chemical bath method. The structural properties of zincite nanorods were determined by X-ray diffraction (XRD) and corroborated well with the morphologic properties obtained by field-emission gun scanning electron microscopy (FEG SEM) with energy-dispersive X-ray spectroscopy (EDS). Morphology results revealed a minute change in the nanorod geometry upon doping, which was also visible by Kelvin probe force microscopy (KPFM). KPFM also showed preliminary electrical properties. Detailed electrical characterization of pure and Al-doped ZnO NR was conducted by temperature-dependent current–voltage (I–V) measurements on Au/(Al)ZnO NR/n-Si junctions. It was shown that Al doping increases the conductivity of ZnO NR by an order of magnitude. The I–V characteristics of pure and Al-doped ZnO NR followed the ohmic regime for lower voltages, whereas, for the higher voltages, significant changes in electric conduction mechanisms were detected and ascribed to Al-doping. In conclusion, for future applications, one should consider the possible influence of the geometry change of (Al)ZnO NRs on their overall electric transport properties.     

ZnO Films Incorporation Study on Macroporous Silicon Structure

In the present work, we developed hybrid nanostructures based on ZnO films deposited on macroporous silicon substrates using the sol–gel spin coating and ultrasonic spray pyrolysis (USP) techniques. The changes in the growth of ZnO films on macroporous silicon were studied using a UV-visible spectrometer, an X-ray diffractometer (XRD), scanning electron microscopy (SEM) and atomic force microscopy (AFM). XRD analysis revealed the beneficial influence of macroporous silicon on the structural properties of ZnO films. SEM micrographs showed the growth and coverage of ZnO granular and flake-like crystals inside the pores of the substrate. The root mean square roughness (RMS) measured by AFM in the ZnO grown on the macroporous silicon substrate was up to one order of magnitude higher than reference samples. These results prove that the methods used in this work are effective to cover porous and obtain nano-morphologies of ZnO. These morphologies could be useful for making highly sensitive gas sensors.     

Zinc Oxide Nanoparticles for Water Purification

In this study, zinc oxide nanoparticles were synthesized through a simple co-precipitation method starting from zinc acetate dihydrate and sodium hydroxide as reactants. The as-obtained ZnO nanoparticles were morphologically and structurally characterized by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), photocatalytic activity, and by determining the antimicrobial activity against Gram-negative and Gram-positive bacteria. The XRD pattern of the zinc oxide nanoparticles showed the wurtzite hexagonal structure, and its purity highlighted that the crystallinity correlated with the presence of a single product, zinc oxide. The ZnO nanoparticles have an average crystallite size of 19 ± 11 nm, which is in accordance with the microscopic data. ZnO nanoparticles were tested against methyl orange, used as a model pollutant, and it was found that they exhibit strong photocatalytic activity against this dye. The antibacterial activity of ZnO nanoparticles was tested against Gram-negative and Gram-positive strains (Escherichia coli, Staphylococcus aureus, and Candida albicans). The strongest activity was found against Gram-positive bacteria (S. aureus).     

Heat-Treated Ni-CNT Nanocomposites Produced by Powder Metallurgy Route

Nickel nanocomposites reinforced by carbon nanotubes (Ni-CNTs) are one of the possible candidates for applications in highly demanding industries such as the automotive and aerospace industries. As is well known, one of the limitations on the use of some materials in these applications is thermal stability. Some components in these industries are frequently subjected to high temperatures, which is crucial to understanding their microstructures and, consequently, their mechanical properties. For this reason, the main objective of this research is to understand the microstructural evolution of Ni-CNTs nanocomposites when subjected to heat treatment. The nanocomposites with varying levels of CNT content were produced by powder metallurgy, and unreinforced nickel was used for comparison purposes under the same conditions. The dispersion of CNTs, a critical aspect of nanocomposites production, was carried out by ultrasonication, which already proved its efficiency in previous research. The heat treatments were performed under high vacuum conditions at high temperatures (700 and 1100 °C for 30 and 120 min, respectively). Microhardness tests analyzed the mechanical properties while the extensive microstructural evaluation was conducted by combining advanced characterization techniques such as scanning electron microscopy (SEM) with electron backscatter diffraction (EBSD), transmission electron microscopy (TEM), and high-resolution TEM. The obtained results are promising and show that the presence of CNTs can contribute to the thermal stability of the Ni-CNT nanocomposites produced.     

Synthesis of Selected Mixed Oxide Materials with Tailored Photocatalytic Activity in the Degradation of Tetracycline

The elimination of antibiotics occurring in the natural environment has become a great challenge in recent years. Among other techniques, the photocatalytic degradation of this type of pollutant seems to be a promising approach. Thus, the search for new photoactive materials is currently of great importance. The present study concerns the sol–gel synthesis of mono, binary and ternary TiO₂-based materials, which are used as active photocatalysts. The main goal was to evaluate how the addition of selected components—zirconium dioxide (ZrO₂) and/or zinc oxide (ZnO)—during the synthesis of TiO₂-based materials and the temperature of thermal treatment affect the materials’ physicochemical and photocatalytic properties. The fabricated mixed oxide materials underwent detailed physicochemical analysis, utilizing scanning-electron microscopy (SEM), X-ray diffraction (XRD), diffuse reflectance spectroscopy (DRS), energy-dispersive X-ray spectroscopy (EDS), low-temperature N₂ sorption (BET model), X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared spectroscopy (FTIR). The synthesized mixed oxide materials were used as photocatalysts in the heterogeneous photodegradation of tetracycline (TC). The physicochemical properties of the fabricated photocatalysts, including morphology, crystalline and textural structure, as well as the pH of the reaction system in the photocatalytic tests, were taken into account in determining their photo-oxidation activity. LC–MS/MS analysis was used to identify the possible degradation products of the selected antibiotic.     

Acacia nilotica Pods’ Extract Assisted-Hydrothermal Synthesis and Characterization of ZnO-CuO Nanocomposites

This work represents a novel combination between Acacia nilotica pods’ extract and the hydrothermal method to prepare nanoparticles of pure zinc oxide and pure copper oxide and nanocomposites of both oxides in different ratios. Five samples were prepared with different ratios of zinc oxide and copper oxide; 100% ZnO (ZC0), 75% ZnO: 25% CuO (ZC25), 50% ZnO: 50% CuO (ZC50), 25% ZnO: 75% CuO (ZC75), and 100% CuO (ZC100). Several techniques have been applied to characterize the prepared powders as FTIR, XRD, SEM, and TEM. The XRD results confirm the formation of the hexagonal wurtzite phase of zinc oxide and the monoclinic tenorite phase of copper oxide. The microscopy results show the formation of a heterostructure of nanocomposites with an average particle size of 13–27 nm.     

Preparation of ZnO Nanoparticle/Acrylic Resin Superhydrophobic Coating via Blending Method and Its Wear Resistance and Antibacterial Properties

Herein, a facile method for the preparation of an acrylic resin-based superhydrophobic coating is provided. Firstly, ZnO nanoparticles were modified with silane to obtain hydrophobic ZnO, which was then homogeneously blended with acrylic resin. Subsequently, the mixture was sprayed on an aluminum sheet to form a cured coating. The surface composition and morphology of the coating were characterized using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM). The hydrophobicity, wear resistance, and antibacterial properties of the prepared samples were tested. The optimized hydrophobicity was achieved with 10 wt% modification agent and resin-to-ZnO mass ratio of 1:4, exhibiting contact and sliding angles of 168.11° and 7.2°, respectively. Wear resistance was insufficient with a low resin content, while it grew with the increase in the resin content. However, when the resin content was excessively high, the hydrophobicity was reduced because the resin could wrap the modified ZnO nanoparticles and decrease the number of hydrophobic groups on the surface. Compared with the pure acrylic resin coating, the ZnO nanoparticle/acrylic resin superhydrophobic coating demonstrated a significant enhancement in the antibacterial properties.     

Conductive Polyaniline Patterns on Electrospun Polycaprolactone/Hydroxyapatite Scaffolds for Bone Tissue Engineering

Currently, the challenge for bone tissue engineering is to design a scaffold that would mimic the structure and biological functions of the extracellular matrix and would be able to direct the appropriate response of cells through electrochemical signals, thus stimulate faster bone formation. The purpose of the presented research was to perform and evaluate PCL/n-HAp scaffolds locally modified with a conductive polymer-polyaniline. The material was obtained using electrospinning, and a simple ink-jet printing method was applied to receive the conductive polyaniline patterns on the surface of the electrospun materials. The samples of scaffolds were analyzed by scanning electron microscopy (SEM), X-ray diffraction (XRD), thermal analysis (DSC, TGA), and infrared spectroscopy (FTIR) before and after immersion of the material in Simulated Body Fluid. The effect of PANI patterns on changes in the SBF mineralization process and cell morphology was evaluated in order to prove that the presented material enables the growth and proliferation of bone cells.     

Study on Dissolution and Modification of Cotton Fiber in Different Growth Stages

Cotton fibers with ultra-high purity cellulose are ideal raw materials for producing nanocellulose. However, the strong hydrogen bond and high crystallinity of cotton fibers affect the dissociation of cotton fibers to prepare nanocellulose. The structures of two kinds of cotton fibers (CM and XM) in different growth stages from 10 to 50 days post-anthesis (dpa) were studied by Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD). In the process of cotton fiber growth, the deposition rate of cellulose macromolecules firstly increased and then stabilized. Then, the surface morphology, the chemical composition, and the crystal structure of the nanocellulose prepared from cotton fibers with different growth stages by deep eutectic solvent, a green solvent, were characterized by Transmission Electron Microscope (TEM), scanning electron microscopy (SEM) analysis, XRD, and Thermo Gravimetry (TG). The growth time of cotton fibers affected the properties of prepared nanocellulose, and nanocellulose obtained from cotton fibers at about 30 dpa had less energy consumption, higher yield, and milder reaction conditions.     

Visible-Light-Driven Photocatalytic Inactivation of Bacteria,Bacteriophages, and Their Mixtures Using ZnO-Coated HDPE Beads as Floating Photocatalyst

Semiconductor materials used as photocatalysts are considered among the most effective ways to treat biologically polluted water. Certainly, efficiency depends on the selection of photocatalyst and its substrate, as well as the possibility of its application in a broader spectrum of light. In this study, a reactive magnetron sputtering technique was applied for the immobilisation of ZnO photocatalyst on the surface of HDPE beads, which were selected as the buoyant substrates for enhanced photocatalytic performance and easier recovery from the treated water. Moreover, the study compared the effect on the inactivation of the microorganism between ZnO-coated HDPE beads without Ni and with Ni underlayer. Crystal structure, surface morphology, and chemical bonds of as-deposited ZnO films were investigated by X-ray diffraction, scanning electron microscopy, and X-ray photoelectron spectroscopy, respectively. Visible-light-induced photocatalytic treatment was performed on the Gram-negative and Gram-positive bacteria and bacteriophages PRD1, T4, and their mixture. Higher bacteria inactivation efficiency was obtained using the ZnO photocatalyst with Ni underlayer for the treatment of S. Typhimurium and M. Luteus mixtures. As for infectivity of bacteriophages, T4 alone and in the mixture with PRD1 were more affected by the produced photocatalyst, compared with PRD1.     

One Step In-Situ Synthesis of Zinc Oxide Nanoparticles for Multifunctional Cotton Fabrics

Zinc oxide nanoparticles (ZnO NPs) have acquired great significance in the textile sector due to their impressive efficiency and multifold utilization, such as antimicrobials, UV protection, photo catalytic activity, and self-cleaning. The aim of this work is in-situ growth of ZnO NPs on 100% cotton fabrics with the one-step hydrothermal method for preparation of multifunctional textile with UV protecting, antibacterial, and photo catalytic properties. Sodium hydroxide (NaOH) and Zinc nitrate hexahydrate [Zn(NO₃)₂·6H₂O] were used as reactants for the growth of zinc oxide on the 100% cotton fabrics. The loaded amount of Zn contents on the cotton fabric was determined by using induced coupled plasma atomic emission spectroscopy (ICP-AES). The surface morphological characterization of deposited ZnO NPs was examined, employing scanning electron microscopy (SEM), X-ray powder diffraction (XRD) and, Fourier- transform infrared spectroscopy (FTIR). The characterization results showed the presence of ZnO NPs on cotton fabrics having hexagonal wurtzite crystalline structure. The synthesized ZnO NPs on fabrics exhibited promising results for antibacterial, UV protection, and photo catalytic performance.