Mechanical Properties of Cu2O Thin Films by Nanoindentation

In this study, the structural and nanomechanical properties of Cu₂O thin films are investigated by X-ray diffraction (XRD), atomic force microscopy (AFM), scanning electron microscopy (SEM) and nanoindentation techniques. The Cu₂O thin films are deposited on the glass substrates with the various growth temperatures of 150, 250 and 350 °C by using radio frequency magnetron sputtering. The XRD results show that Cu₂O thin films are predominant (111)-oriented, indicating a well ordered microstructure. In addition, the hardness and Young’s modulus of Cu₂O thin films are measured by using a Berkovich nanoindenter operated with the continuous contact stiffness measurements (CSM) option. Results indicated that the hardness and Young’s modulus of Cu₂O thin films decreased as the growth temperature increased from 150 to 350 °C. Furthermore, the relationship between the hardness and films grain size appears to closely follow the Hall-Petch equation.     

Aqueous Sol-Gel Synthesis of Different Iron Ferrites: From 3D to 2D

In this study, an aqueous sol-gel synthesis method and subsequent dip-coating technique were applied for the preparation of yttrium iron garnet (YIG), yttrium iron perovskite (YIP), and terbium iron perovskite (TIP) bulk and thin films. The monophasic highly crystalline different iron ferrite powders have been synthesized using this simple aqueous sol-gel process displaying the suitability of the method. In the next step, the same sol-gel solution was used for the fabrication of coatings on monocrystalline silicon (100) using a dip-coating procedure. This resulted, likely due to substrate surface influence, in all coatings having mixed phases of both garnet and perovskite. Thermogravimetric (TG) analysis of the precursor gels was carried out. All the samples were investigated by X-ray powder diffraction (XRD) analysis. The coatings were also investigated by scanning electron microscopy (SEM), atomic force microscopy (AFM) and Mössbauer spectroscopy. Magnetic measurements were also carried out.     

Effect of Annealing Temperature and Oxygen Flow in the Properties of Ion Beam Sputtered SnO2?x Thin Films

Tin oxide (SnO_2−x) thin films were prepared under various flow ratios of O₂/(O₂ + Ar) on unheated glass substrate using the ion beam sputtering (IBS) deposition technique. This work studied the effects of the flow ratio of O₂/(O₂ + Ar), chamber pressures and post-annealing treatment on the physical properties of SnO₂ thin films. It was found that annealing affects the crystal quality of the films as seen from both X-ray diffraction (XRD) and transmission electron microscopy (TEM) analysis. In addition, the surface RMS roughness was measured with atomic force microscopy (AFM). Auger electron spectroscopy (AES) analysis was used to obtain the changes of elemental distribution between tin and oxygen atomic concentration. The electrical property is discussed with attention to the structure factor.     

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.     

Hydrothermal Growth of Vertically Aligned ZnO Nanorods Using a Biocomposite Seed Layer of ZnO Nanoparticles

Well aligned ZnO nanorods have been prepared by a low temperature aqueous chemical growth method, using a biocomposite seed layer of ZnO nanoparticles prepared in starch and cellulose bio polymers. The effect of different concentrations of biocomposite seed layer on the alignment of ZnO nanorods has been investigated. ZnO nanorods grown on a gold-coated glass substrate have been characterized by X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM) techniques. These techniques have shown that the ZnO nanorods are well aligned and perpendicular to the substrate, and grown with a high density and uniformity on the substrate. Moreover, ZnO nanorods can be grown with an orientation along the c-axis of the substrate and exhibit a wurtzite crystal structure with a dominant (002) peak in an XRD spectrum and possessed a high crystal quality. A photoluminescence (PL) spectroscopy study of the ZnO nanorods has revealed a conventional near band edge ultraviolet emission, along with emission in the visible part of the electromagnetic spectrum due to defect emission. This study provides an alternative method for the fabrication of well aligned ZnO nanorods. This method can be helpful in improving the performance of devices where alignment plays a significant role.     

Controlling the Wettability of ZnO Thin Films by Spray Pyrolysis for Photocatalytic Applications

Herein, we synthesized the zinc oxide (ZnO) thin films (TFs) deposited on glass substrates via spray pyrolysis (SP) to prepare self-cleaning glass. Various process parameters were used to optimize photocatalytic performance. Substrates were coated at room temperature (RT) and 250 °C with a 1 mL or 2 mL ZnO solution while maintaining a distance from the spray gun to the substrate of 20 cm or 30 cm. Several characterization techniques, i.e., XRD, SEM, AFM, and UV–Vis were used to determine the structural, morphological, and optical characteristics of the prepared samples. The wettability of the samples was evaluated using contact angle measurements. As ZnO is hydrophilic in nature, the RT deposited samples showed a hydrophilic character, whereas the ZnO TFs deposited at 250 °C demonstrated a hydrophobic character. The XRD results showed a higher degree of crystallinity for samples deposited on heated substrates. Because of this higher crystallinity, the surface energy decreased, and the contact angle increased. Moreover, by using 2 mL solution, better surface coverage and roughness were obtained for the ZnO TFs. However, by exploiting the distance of the spray to the samples size distribution and surface coverage can be controlled, the samples deposited at 30 mL showed a uniform particle size distribution from 30–40 nm. In addition, the photoactivity of the samples was tested by the degradation of rhodamine B dye. Substrates prepared with a 2 mL solution sprayed at 20 cm showed higher dye degradation than other samples, which can play a vital role in self-cleaning. Hence, by changing the said parameters, the ZnO thin film properties on glass substrates were optimized for self-cleaning diversity.     

The Performance of Graphene-Enhanced THz Grating: Impact of the Gold Layer Imperfectness

We report the performance of a graphene-enhanced THz grating fabricated by depositing a gold layer on the femtosecond micromachined SiO₂ substrate. The morphology of the gold plated patterned substrate was studied by scanning electron microscopy (SEM) and atomic force microscopy (AFM), while the quality of the chemical vapor deposition (CVD) graphene was evaluated by Raman spectroscopy. The electromagnetic (EM) response of the metasurface comprising the graphene sheet and the gold plated substrate was studied by THz time domain spectroscopy in the 100 GHz–1 THz frequency range. We employed the finite elements method (FEM) to model the metasurface EM response by adjusting the ac conductivity of the gold layer covering the patterned SiO₂ substrate to reproduce the measured transmission/reflection spectra. The results of the numerical simulation reveal the impact of the imperfectness of the gold layer on the performance of the THz metasurface. The experimental results are well described in terms of the Drude–Smith model of metal conductivity that takes into account the anisotropic scattering of the carriers in thin metal films.     

Preparation of the Heterogeneous Saponified Poly(Vinyl Alcohol)/Poly(Methyl Methacrylate–Methallyl Alcohol) Blend Film

For the first time, poly(vinyl alcohol) (PVA)/poly(methyl methacrylate–methallyl alcohol) (P(MMA-MAA)) (9:1, 7:3, 5:5) blend films were made simultaneously using the saponification method in a heterogeneous medium from poly(vinyl acetate) (PVAc)/poly(methyl methacrylate) (PMMA) (9:1, 7:3, 5:5) blend films, respectively. The surface morphology and characteristics of the films were investigated using optical microscopy (OM), atomic force microscopy (AFM), X-ray diffractometer (XRD), Fourier transform infrared (FTIR) spectroscopy, thermogravimetric analysis (TGA), and differential scanning calorimetry (DSC). Moreover, the effect of the PVAc content on the degree of saponification (DS) of the PVAc/PMMA films were evaluated and revealed that the obtained DS value increased with the increase in PVAc content in the PVAc/PMMA blend films. According to the OM results, the saponified films demonstrated increased surface roughness compared with the unsaponified films. The AFM images revealed morphological variation among the saponified PVAc/PMMA blend films with different mass ratios of 9:1, 7:3, and 5:5. According to the DSC and TGA results, all blend film types exhibited higher thermal property after the saponification treatment. The XRD and FTIR results confirmed the conversion of the PVAc/PMMA into PVA/P(MMA-MAA) films. Thus, our present work may give a new idea for making blend film as promising medical material with significant surface properties based on hydrophilic/hydrophobic strategy.     

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.     

Ellipsometry Study of CdSe Thin Films Deposited by PLD on ITO Coated Glass Substrates

Cadmium selenide (CdSe) thin films were deposited on indium tin oxide (ITO) coated glass substrates using pulsed laser deposition (PLD) technique under different growth temperatures. Samples were investigated for their structural, morphological, and optical properties through X-ray diffraction (XRD), atomic force microscopy (AFM), and UV-Vis-NIR spectroscopy. AFM analysis revealed that the surface roughness of the as-grown CdSe thin films increased with the increase in deposition temperature. The optical constants and film thickness were obtained from spectroscopic ellipsometry analysis and are discussed in detail. The optical band gap of the as-grown CdSe thin films, calculated from the Tauc plot analysis, matched with the ellipsometry measurements, with a band gap of ~1.71 eV for a growth temperature range of 150 °C to 400 °C. The CdSe thin films were found to have a refractive index of ~3.0 and extinction coefficient of ~1.0, making it a suitable candidate for photovoltaics.     

The Effect of Polyethylene Glycol Addition on Wettability and Optical Properties of GO/TiO2 Thin Film

Modification has been made to TiO₂ thin film to improve the wettability and the absorption of light. The sol-gel spin coating method was successfully used to synthesize GO/TiO₂ thin films using a titanium (IV) isopropoxide (TTIP) as a precursor. Different amounts of polyethylene glycol (PEG) (20 to 100 mg) were added into the parent sol solution to improve the optical properties and wettability of the GO/TiO₂ thin film. The effect of different amounts of PEG was characterized using X-ray diffraction (XRD) for the phase composition, scanning electron microscopy (SEM) for microstructure observation, atomic force microscopy (AFM) for the surface topography, ultraviolet–visible spectrophotometry (UV-VIS) for the optical properties and wettability of the thin films by measuring the water contact angle. The XRD analysis showed the amorphous phase. The SEM and AFM images revealed that the particles were less agglomerated and surface roughness increases from 1.21 × 10² to 2.63 × 10² nm when the amount of PEG increased. The wettability analysis results show that the water contact angle of the thin film decreased to 27.52° with the increase of PEG to 80 mg which indicated that the thin film has hydrophilic properties. The optical properties also improved significantly, where the light absorbance wavelength became wider and the band gap was reduced from 3.31 to 2.82 eV with the presence of PEG.     

Fabrication of Cellulose Film with Enhanced Mechanical Properties in Ionic Liquid 1-Allyl-3-methylimidaxolium Chloride (AmimCl)

More and more attention has been paid to environmentally friendly bio-based renewable materials as the substitution of fossil-based materials, due to the increasing environmental concerns. In this study, regenerated cellulose films with enhanced mechanical property were prepared via incorporating different plasticizers using ionic liquid 1-allyl-3-methylimidazolium chloride (AmimCl) as the solvent. The characteristics of the cellulose films were investigated by scanning electron microscopy (SEM), atomic force microscopy (AFM), thermal analysis (TG), X-ray diffraction (XRD), ¹³C Solid-state cross-polarization/magic angle spinning nuclear magnetic resonance (CP/MAS NMR) and tensile testing. The results showed that the cellulose films exhibited a homogeneous and smooth surface structure. It was noted that the thermal stability of the regenerated cellulose film plasticized with glycerol was increased compared with other regenerated cellulose films. Furthermore, the incorporation of plasticizers dramatically strengthened the tensile strength and improved the hydrophobicity of cellulose films, as compared to the control sample. Therefore, these notable results exhibited the potential utilization in producing environmentally friendly cellulose films with high performance properties.     

Structural Properties of Thin ZnO Films Deposited by ALD under O-Rich and Zn-Rich Growth Conditions and Their Relationship with Electrical Parameters

The structural, optical, and electrical properties of ZnO are intimately intertwined. In the present work, the structural and transport properties of 100 nm thick polycrystalline ZnO films obtained by atomic layer deposition (ALD) at a growth temperature (T_g) of 100–300 °C were investigated. The electrical properties of the films showed a dependence on the substrate (a-Al₂O₃ or Si (100)) and a high sensitivity to T_g, related to the deviation of the film stoichiometry as demonstrated by the RT-Hall effect. The average crystallite size increased from 20–30 nm for as grown samples to 80–100 nm after rapid thermal annealing, which affects carrier scattering. The ZnO layers deposited on silicon showed lower strain and dislocation density than on sapphire at the same T_g. The calculated half crystallite size (D/2) was higher than the Debye length (L_D) for all as grown and annealed ZnO films, except for annealed ZnO/Si films grown within the ALD window (100–200 °C), indicating different homogeneity of charge carrier distribution for annealed ZnO/Si and ZnO/a-Al₂O₃ layers. For as grown films the hydrogen impurity concentration detected via secondary ion mass spectrometry (SIMS) was 10²¹ cm⁻³ and was decreased by two orders of magnitude after annealing, accompanied by a decrease in Urbach energy in the ZnO/a-Al₂O₃ layers.     

Influence of Thin Film Deposition on AFM Cantilever Tips in Adhesion and Young’s Modulus of MEMS Surfaces

Adhesion is a critical factor in microelectromechanical systems (MEMSs) and is influenced by many parameters. In important fields, such as microassembly, an improved understanding of adhesion can result in higher precision. This study examines the influence of deposition of gold and titanium onto the atomic force microscope (AFM) tips in adhesion forces and Young’s modulus, between a few MEMS substrates (silicon, gold, and silver) and the AFM tips. It was found that, except for gold substrate, an AFM tip coated with gold has the highest adhesion force of 42.67 nN for silicon substrates, whereas the titanium-coated AFM tip decreases the force for all the samples. This study suggests that such changes must be taken into account while studying the adhesion force. The final results indicate that utilizing gold substrate with titanium AFM tip led to the lowest adhesion force, which could be useful in adhesion force measurement during microassembly.     

Biocompatibility and Surface Properties of TiO2 Thin Films Deposited by DC Magnetron Sputtering

We present the study of the biocompatibility and surface properties of titanium dioxide (TiO₂) thin films deposited by direct current magnetron sputtering. These films are deposited on a quartz substrate at room temperature and annealed with different temperatures (100, 300, 500, 800 and 1100 °C). The biocompatibility of the TiO₂ thin films is analyzed using primary cultures of dorsal root ganglion (DRG) of Wistar rats, whose neurons are incubated on the TiO₂ thin films and on a control substrate during 18 to 24 h. These neurons are activated by electrical stimuli and its ionic currents and action potential activity recorded. Through X-ray diffraction (XRD), the surface of TiO₂ thin films showed a good quality, homogeneity and roughness. The XRD results showed the anatase to rutile phase transition in TiO₂ thin films at temperatures between 500 and 1100 °C. This phase had a grain size from 15 to 38 nm, which allowed a suitable structural and crystal phase stability of the TiO₂ thin films for low and high temperature. The biocompatibility experiments of these films indicated that they were appropriated for culture of living neurons which displayed normal electrical behavior.     

Fabrication of Graphene/Zinc Oxide Nano-Heterostructure for Hydrogen Sensing

In this study, hydrogen (H₂) and methane (CH₄) were used as reactive gases, and chemical vapor deposition (CVD) was used to grow single-layer graphene on a copper foil substrate. The single-layer graphene obtained was transferred to a single-crystal silicon substrate by PMMA transfer technology for the subsequent growth of nano zinc oxide. The characteristics of CVD-deposited graphene were analyzed by a Raman spectrometer, an optical microscope, a four-point probe, and an ultraviolet/visible spectrometer. The sol–gel method was applied to prepare the zinc oxide seed layer film with the spin-coating method, with methanol, zinc acetate, and sodium hydroxide as the precursors for growing ZnO nanostructures. On top of the ZnO seed layer, a one-dimensional zinc oxide nanostructure was grown by a hydrothermal method at 95 °C, using a zinc nitrate and hexamethylenetetramine mixture solution. The characteristics of the nano zinc oxide were analyzed by scanning electron microscope(SEM),x-ray diffractometer(XRD), and Raman spectrometer. The obtained graphene/zinc oxide nano-heterostructure sensor has a sensitivity of 1.06 at a sensing temperature of 205 °C and a concentration of hydrogen as low as 5 ppm, with excellent sensing repeatability. The main reason for this is that the zinc oxide nanostructure has a large specific surface area, and many oxygen vacancy defects exist on its surface. In addition, the P–N heterojunction formed between the n-type zinc oxide and the p-type graphene also contributes to hydrogen sensing.     

In Situ Monitoring of Pulsed Laser Annealing of Eu-Doped Oxide Thin Films

Eu³⁺-doped oxide thin films possess a great potential for several emerging applications in optics, optoelectronics, and sensors. The applications demand maximizing Eu³⁺ photoluminescence response. Eu-doped ZnO, TiO_2, and Lu₂O₃ thin films were deposited by Pulsed Laser Deposition (PLD). Pulsed UV Laser Annealing (PLA) was utilized to modify the properties of the films. In situ monitoring of the evolution of optical properties (photoluminescence and transmittance) at PLA was realized to optimize efficiently PLA conditions. The changes in optical properties were related to structural, microstructural, and surface properties characterized by X-ray diffraction (XRD) and atomic force microscopy (AFM). The substantial increase of Eu³⁺ emission was observed for all annealed materials. PLA induces crystallization of TiO₂ and Lu₂O₃ amorphous matrix, while in the case of already nanocrystalline ZnO, rather surface smoothening0related grains’ coalescence was observed.     

Microstructure and Optical Properties of Nanostructural Thin Films Fabricated through Oxidation of Au–Sn Intermetallic Compounds

AuSn and AuSn₂ thin films (5 nm) were used as precursors during the formation of semiconducting metal oxide nanostructures on a silicon substrate. The nanoparticles were produced in the processes of annealing and oxidation of gold–tin intermetallic compounds under ultra-high vacuum conditions. The formation process and morphology of a mixture of SnO₂ and Au@SnO_x (the core–shell structure) nanoparticles or Au nanocrystalites were carefully examined by means of spectroscopic ellipsometry (SE), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) combined with energy-dispersive X-ray spectroscopy (EDX). The annealing and oxidation of the thin film of the AuSn intermetallic compound led to the formation of uniformly distributed structures with a size of ∼20–30 nm. All of the synthesized nanoparticles exhibited a strong absorption band at 520–530 nm, which is typical for pure metallic or metal oxide systems.     

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.     

Study of ZnO-CNT Nanocomposites in High-Pressure Conditions

Recently, carbon nanotubes (CNTs) have been used extensively to develop new materials and devices due to their specific morphology and properties. The reinforcement of different metal oxides such as zinc oxide (ZnO) with CNT develops advanced multifunctional materials with improved properties. Our aim is to obtain ZnO-CNT nanocomposites by in situ hydrothermal method in high-pressure conditions. Various compositions were tested. The structure and morphology of ZnO-CNT nanocomposites were analyzed by Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry—thermogravimetry (DSC-TG), X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), and transmission electron microscopy (TEM). These analyses showed the formation of complex ZnO-CNT structures. FT-IR spectra suggest possible interactions between CNT and ZnO. DSC-TG analysis also reveals the formation of some physical bonds between ZnO and CNT, through the appearance of endothermic peaks which could be assigned to the decomposition of functional groups of the CNT chain and breaking of the ZnO-CNT bonds. XRD characterization demonstrated the existence of ZnO nanocrystallites with size around 60 nm. The best ZnO:CNT composition was further selected for preliminary investigations of the potential of these nanocomposite powders to be processed as pastes for extrusion-based 3D printing.