Surface structural features and optical analysis of nanostructured Cu-oxide thin film coatings coated via the sol-gel dip coating method

Nanostructured thin film coatings of copper oxide (Cu-oxide) were investigated to determine their physical structure, surface morphology, surface electronic bonding states, and optical properties. The Cu-oxide had been coated onto reflective aluminum substrates via a facile one-step sol–gel dip-coating route using a copper nitrate precursor. Characterizations were conducted using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), field emission scanning electron microscopy (FESEM), and ultra-violet visible (UV–Vis) spectroscopic methods, and representative sol-gel reactions using copper nitrate precursor were proposed. The XPS spectra confirmed the presence of copper oxide elements. Further exploration of the Cu2p3/2 peak in XPS spectra revealed that the electronic structure of the copper component consisted of tetrahedral Cu(I) and octahedral Cu(II) with the presence of octahedral Cu(II) enabling coatings to have high absorption levels across the solar spectrum. The deconvolution of the O1s spectra exhibited three curve-fitting components: the lattice O²⁻, surface oxygen, and subsurface O⁻ species. FESEM results showed that the coating surface was an agglomerated copper oxide nanoparticles structure forming a porous structure. The optical band-gap of Cu-oxide thin film coatings, via the Tauc plot, was 2.7 eV.     

Engineering of morphological,optical, structural,photocatalytic and catalytic properties of nanostructured CuO thin films fabricated by reactive DC magnetron sputtering

Nanostructured thin films of CuO were deposited on silica glass substrates using reactive DC magnetron sputtering technique. Microstructural, morphological, optical, catalytic and photocatalytic properties of the prepared CuO thin films were examined using FESEM, AFM, Rutherford backscattering spectrometry, XRD, XPS, UV–Vis absorption and PL spectroscopy. FESEM showed nanostructures in the thin films, which were confirmed to be of monoclinic CuO by XRD analysis. Substrate temperature variation (40 °C, 100 °C and 300 °C) was found to significantly alter the optical, morphological, photocatalytic and structural properties of the CuO nanostructured thin film coatings. FESEM and AFM analyses showed decrease in size of nanostructures and surface roughness increase with increase in substrate temperature. Increase in UV–Vis absorbance and PL intensity of CuO thin films with decrease in crystallite size were noticed as the substrate temperature was increased. The prepared nanostructured CuO thin films exhibited highly enhanced photocatalytic activities and degraded dyes (MB and MO) in water in just 40 min under solar exposure and catalytic transformation of 4-nitrophenol (4-NP) took place in just 15 min. The developed CuO nanostructured thin film coatings are very promising for large scale, practical and advanced catalytic reduction of toxic 4-NP and photocatalytic applications in solar driven water purification.     

Investigation of the microstructure,cation distribution and optical properties of nanoscale NixMg1-xAl2O4 spinel pigments

Nanoscale Ni_xMg_1-xAl₂O₄ spinel pigments were synthesized by a citric acid precursor combined with the gel-casting method. The microstructure, cation distribution and optical properties as a function of calcining temperature and nickel content were investigated by the X-ray diffraction (XRD) Rietveld refinement, transmission/field emission scanning electron microscopy (TEM/FESEM), X-ray photoelectron spectroscopy (XPS), colour measurement and UV–vis–NIR spectrophotometry. Upon increasing the calcining temperature, both Ni²⁺ and Mg²⁺ hindered the migration of Al³⁺ to octahedral sites. When the Ni content increased, the cation site percentage of Ni²⁺ in the tetrahedral and octahedral sites varied slightly while that of Al³⁺ and Mg²⁺ change substantially. The cation exchange resulted in an increase in the inversion parameters and a decrease in the lattice parameters with increasing temperature or Ni content. Furthermore, Rietveld refinement also showed a shrinkage of the tetrahedra and an expansion of the distorted octahedra in the spinel structure. Short-range information based on optical spectra suggests that variation in the splitting energy of tetrahedra and octahedra caused the change in the spectral absorption. This study may deepen the understanding of the structural-optical property relationship of Ni_xMg_1-xAl₂O₄ spinel, which is vital to the further colour modification of ceramics and glazes.     

Battery-like behavior of Ni-ceria based systems: Synthesis,surface defects and electrochemical assessment

NiO, CeO₂ and respective composites are extensively used in energy storage devices due to mostly their high electrochemical activity. However, the assessment of battery-like behavior of Ni-ceria based systems comprising (Ni or Gd)-doped ceria combined with NiO seems to be neglected in the literature. In this work, NiO and ceria-based solid solutions composite powders were obtained by a co-precipitation synthesis method. The structure and particle size of the calcined powders were investigated by X-ray diffractometry (XRD) and field emission scanning electron microscopy (FESEM), respectively. Oxidative states of composites were inspected by X-ray photoelectron spectroscopy (XPS). The electrochemical performance of powders was evaluated by cyclic voltammetry, galvanostatic charge-discharge and impedance spectroscopy. Refinement of the XRD patterns showed that powders have nanosized crystallites and mean size of particles within 20 – 70?nm were revealed by FESEM. The improved specific capacity of the NiO-CeO₂ electrode material (about 2.5 times higher than that of NiO-CGO at 5?mV?s^?1) is due to an increase in Faradic reactions taken place on its surface with a higher fraction of defects (namely Ni³⁺, Ce³⁺ and oxygen vacancies), as determined by XPS. The superior electrochemical performance of the NiO-CeO₂ electrode is also confirmed by electrochemical impedance spectroscopy.     

S–N Co-Doped TiO2 Photocatalysts with Visible-Light Activity Prepared by Sol–Gel Method

S–N co-doped anatase nanosized TiO₂ photocatalyst was successfully prepared by simple sol–gel method. The samples were characterized by XRD, XPS, UV–Vis. From the results of UV–Vis, a red shift of the absorption edge was brought out owing to the S and N codoping. XPS and UV–Vis studies revealed that N and S were in situ codoped in the lattice of TiO₂ and the absorbance in visible light region decreased with the calcination temperature increased. The photocatalytic activity was evaluated by the photocatalytic oxidation of penicillin solution under visible light irradiation. The results show that visible-light induced photocatalytic activities of the as-prepared TiO₂ powders were improved by S–N copoing. The high activity of S–N co-doped TiO₂ can be related to the results of the synergetic effects of strong absorption in the UV–Vis region, red shift in adsorption edge.     

Study of the changes in the structure and optical properties of MgxCo1-xCr2-yAlyO4 spinel caused by A/B site ion substitution

In this work, nanosubmicron blue-green pigment powder based on the composition of Mg_xCo_1-xCr_2-yAl_yO₄（0 = x ≤ 1, 0 = y ≤ 2）was prepared by a gel casting method. X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), Rietveld refinement with GSAS (General Structure Analysis System), and UV–Vis absorption spectroscopy were used to study the phase composition, grain size, morphology, cation distribution in the crystal structure and spectral absorption of the samples. Colour parameters were also studied by using a colour measurement spectrophotometer. The studies demonstrate that the distribution of cations in the crystal structure is disordered and that divalent and trivalent cations are mixed to occupy tetrahedral and octahedral sites. Furthermore, the substitution of ions at the A/B site leads to a change in the cation distribution ratio at the tetrahedral and octahedral sites. With increasing Mg²⁺ doping concentration, the inversion parameter of the spinel increases, while with increasing Al³⁺ doping concentration, the inversion parameter of the spinel decreases. In addition, changes in the calcining atmosphere lead to a change in the oxygen vacancy content in the structure. Under the condition of a reductive atmosphere, the oxygen vacancy content significantly increases, and the inversion parameter also increases. The colour difference for the synthesized Mg_xCo_1-xCr_2-yAl_yO₄ spinel powder is related to the proportion of chromophore ions occupying tetrahedral and octahedral sites and the number of oxygen vacancies.     

Synthesis,characterization, and performance assessment of a perovskite-type nano photocatalyst for degradation of thiamethoxam

It is essential to remove thiamethoxam (THMX) from surface water as it negatively impacts the ecology and neurological systems of insects. Hence, a study was conducted to degrade THMX with different compositions of LaFeO₃/g-C₃N₄ (LFCN) composites. Several methods, including X-ray powder diffraction (XRD), ultraviolet–visible spectroscopy (UV–Vis), X-ray photoelectron spectroscopy (XPS), Brunauer–Emmett–Teller (BET), and field emission scanning electron microscopy (FESEM), were applied to characterize the synthesized photocatalyst. The influence of many parameters on degradation, for example, THMX concentration, dosage of catalyst, and pH were studied experimentally. The degradation was highest under both UV-C and sunlight for the synthesized catalyst, 1% LaFeO₃/g-C₃N₄ (LFCN1), in comparison to graphitic carbon nitride (g-CN), and bare lanthanum ferrite (LF). The degradation was around 95% for LFCN1 under UV-C light having an intensity of 15 W/m² whereas degradation was 71.8% with LFCN1 photocatalyst under sunlight at neutral pH in 120 min of reaction time. The increased activity of LFCN1 was attributable to an improved surface area and a lower band gap. The study of reaction kinetics indicated second-order behaviour. Additionally, a probable mechanism for degradation was put forth.     

The Stability Study of Au/La-Co–O Catalysts for CO Oxidation

Perovskite oxide LaCoO₃ and the mixture oxides of La₂O₃ + Co₃O₄ were prepared by sol–gel method. Then Au/La–Co–O catalysts were prepared by deposition- precipitation (DP) method and characterized by means of XRD, BET, XPS, TEM and IR. The catalytic performance for CO low-temperature oxidation and stability over these catalysts were compared. The results of experiment showed gold catalysts supported on perovskite oxides have higher catalytic activity and stability than that of supported on the simple oxides.     

Microstructural and Optoelectronic Studies on Polyaniline: TiO2 Nanocomposites

Thin films of polyaniline (PANi) and PANi: titanium oxide (TiO₂) composites have been synthesized by sol–gel spin coating technique. The TiO₂ powder of particle size 50–60 nm was synthesized by the sol–gel technique and the polyaniline was synthesized by the chemical oxidative polymerization of aniline. The composite films were characterized by X-ray diffraction (XRD), atomic force microscopy (AFM), scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy, UV-vis spectroscopy and the four-probe method. The results were compared with corresponding data on pure polyaniline films. The intensity of diffraction peaks for PANi:TiO₂ composites is lower than that for TiO₂. The characteristic FTIR peaks of pure PANi are observed to shift to a higher wavenumber in PANi:TiO₂ composite, which is attributed to the interaction of TiO₂ particles with PANi molecular chains. The resistivity measurement shows that the molecular chain constitution of polyaniline is the most important carrier in the polyaniline: nano-TiO₂ composite.     

The role of Pb and annealing temperature on the structural,magnetic, optical and dielectric properties of W-type hexaferrite nanostructures

In this paper, W-type Sr_1-xPb_xCo₂Fe₁₆O₂₇ nanostructures were synthesized by auto-combustion sol-gel method. Then, the effects of annealing temperature and Pb contents on the structural, magnetic, optical, and dielectric properties of Sr_1-xPb_xCo₂Fe₁₆O₂₇ nanostructure were investigated. First, a gel of metal nitrates with a specific molar ratio with x different was prepared and then the gel was annealed at different temperatures for 4?h. To determine the annealing temperature of the samples, the prepared gel was examined by thermogravimetric analysis and differential thermal analysis. The morphology and crystal structure of the prepared samples were characterized by field emission scanning electron microscopy (FESEM) and X-ray diffraction pattern (XRD). The results of XRD patterns indicated that the annealing temperature of synthesized Sr_1-xPb_xCo₂Fe₁₆O₂₇ was reduced by increasing Pb contents. In addition, FESEM images showed that the microstructure of the samples was homogeneous and uniform, but since the samples have a magnetic property, the particles were aggregated. Fourier transform infrared analysis (FT-IR) was used to confirm the phase formation. The FT-IR results of the samples indicated that the tetrahedral and octahedral sites, which are the important attributes of hexaferrites, were formed. The magnetic properties of the samples were measured by vibrating sample magnetometer (VSM). The VSM results of the samples showed that because of increasing Pb content, the amount of saturation magnetization and that of magnetic coercivity decreased from 81.29 to 10.23?emu/g and 2285–477?Oe, respectively. The optical properties of the samples were investigated by ultraviolet–visible spectroscopy, which revealed that the energy gap decreases and the absorption peaks move towards longer wavelengths by increasing Pb content. The dielectric properties of the samples were investigated by the LCR meter. It was found that by increasing frequency, the dielectric constant (ε^′) and the dielectric loss (?) of the samples were decreased.     

Down-conversion from Er3+-Yb3+ codoped CaMoO4 phosphor: A spectral conversion to improve solar cell efficiency

The present paper focuses on near infrared (NIR) down-conversion photoluminescence (PL) properties by studying the energy transfer mechanism between Er³⁺ and Yb³⁺ in CaMoO₄:Er³⁺, Yb³⁺ phosphors. We have successfully synthesized a series of Er³⁺ doped and Yb³⁺ codoped CaMoO₄ phosphors by hydrothermal method. The down-conversion of Er³⁺-Yb³⁺ combination with CaMoO₄ phosphor is designed to overcome the energy losses due to spectral mismatch when a high energy photon is incident on the Si-solar cell. The XRD, FESEM, EDX, PL, UV–Vis, Lifetime measurements were carried out to characterize the prepared down-converting phosphors. The crystallinity and surface morphology were studied by X-ray diffraction (XRD) and Field Emission Scanning Electron Microscopy (FESEM) techniques. The down-conversion PL spectra have been studied using 380 nm excitation wavelength. The Er³⁺ doped phosphors exhibit hypersensitive emission at 555 nm in the visible region due to ⁴S_3/2→⁴I_15/2 transition. The addition of Yb³⁺ into Er³⁺ doped CaMoO₄ attribute an emission at 980 nm due to ²F_5/2→²F_7/2 transition. The decrease in emission intensity in visible region and increase in NIR region reveals the energy transfer from Er³⁺ to Yb³⁺ through cross relaxation. The UV–Vis–NIR spectra shows the strong absorption peak around 1000 nm due to Yb³⁺ ion. The lifetime measurement also reveals the energy transfer from Er³⁺ to Yb³⁺ ions. The maximum value of energy transfer efficiency (ETE) and corresponding theoretical internal quantum efficiency are estimated as 74% and 174% respectively.     

LDPE/Bi2O3 nanocomposites: Enhanced mechanical,dielectric, and optical properties

This study is focused on investigating the role of bismuth oxide (Bi₂O₃) nanoparticles to improve structural, optical, electrical, and mechanical properties of low-density polyethylene (LDPE). For this purpose, Bi₂O₃ nanoparticles were synthesized by using the solvothermal method and examined by transmission electron microscopes (TEM), x-ray diffraction (XRD), Fourier transformed infrared (FTIR) spectroscopy, and ultraviolet–visible (UV–Vis) light absorption methods. LDPE-based nanocomposites were prepared by changing the nanoparticle additive ratio in the composite from 0% to 2% by weight. The composites were analyzed in the context of their FTIR spectra, atomic force microscope (AFM) images, UV–Vis light absorption spectra, stress–strain curves, and energy storage abilities. While the AFM findings indicate a smoother surface for the composites, the optical band gap analysis reveals a slightly decreased direct optical band gap energy. The analyses based on dielectric spectroscopy also highlight the LDPE/0.5% n-Bi₂O₃ composite in terms of the best energy storage capability. Additionally, the highest Young's modulus, toughness, stress at break, and percentage of strain at break were also recorded for the LDPE/0.5% n-Bi₂O₃ composite. In this context, the LDPE/0.5% n-Bi₂O₃ composite with improved dielectric and mechanical properties can be suggested as a new promising LDPE-based nanocomposite with better properties for industrial purposes.     

Novel method of fabrication of polyaniline–CdS nanocomposites: Structural,morphological and optoelectronic properties

Polyaniline–CdS nanocomposites have been synthesized by spin coating technique. The nanocrystalline CdS powder of particle size 40–50 nm was synthesized by sol–gel technique and the polyaniline was synthesized by chemical oxidative polymerization of aniline. The composite films were characterized by X-ray diffraction (XRD), field effect scanning electron microscopy (FESEM), Fourier transform infrared spectroscopy (FTIR), UV–Vis spectroscopy and Four probe method. The results were compared with corresponding data on pure polyaniline films. The intensity of diffraction peaks for PANi–CdS composites is lower than that for CdS. The conductivity measurement shows that molecular chain constitution of polyaniline is the most important carrier in polyaniline–CdS nano composite. The optical studies showed that variation in band gap of polyaniline (3.40 eV) to 2.54 eV CdS which is attributed to the interaction of CdS nanoparticles with PANi molecular chains.     

Room temperature deposition of XRD-amorphous TiO2 thin films: Investigation of device performance as a function of temperature

In this study, TiO₂ thin films were fabricated by radio frequency sputtering at room temperature in pure Ar atmosphere starting from a 6?in. TiO₂ target. The thickness of the films was controlled by deposition time and the effect of Ar sputtering pressure on the characteristics of TiO₂ thin films was evaluated. Surface morphology and optical properties of TiO₂ films were investigated using X-ray diffraction (XRD), Atomic Force Microscopy (AFM), Scanning Electron Microscopy (SEM) and UV–Vis spectrophotometry. Also, the refractive index and extinction coefficient of films were inferred by fitting spectrophotometric data. Schottky diode were fabricated by evaporation of Ni on TiO₂ films. Current-voltage (I-V) measurements of Ni/TiO₂ films showed that the rectifying properties of the device improves with the increasing of TiO₂ film density and thickness. Therefore, the best I-V characteristic of the device was investigated depending on the temperature. Also, Ni/n-TiO₂/p-Si/Al devices were fabricated to understand their transport mechanism.     

Eggplant as an appreciable bio-template for green synthesis of NiO nanoparticles: Study of physical and photocatalytic properties

In this study, we described a green, sustainable, and feasible method for synthesizing 5 nm NiO nanoparticles. Eggplant skin was chosen as an appropriate bio-template with a high potential to induce its structure into the desired metal oxide. Two approaches were used and compared to synthesize NiO bio-template: hydrothermal and sol-gel. The morphology and physical properties of the obtained NiO nanoparticles were evaluated using FESEM, TEM, XRD, BET, FT-IR, TGA, and UV–Vis analyses. All these methods confirm that the hydrothermal method is a better approach for synthesizing NiO bio-template nanoparticles than the sol-gel method. UV–Vis analysis revealed that the NiO nanoparticles produced by the hydrothermal method have a low bandgap of 2.88 eV, which is a key factor for photocatalytic applications.     

Sm mediated structural properties for MO dye degradation on the titania surface

In the present investigation, titania thin films doped with varying concentrations of Samarium (Sm) were synthesized by spin coating method on glass substrate. The obtained films were annealed at two different temperatures (350 and 450 ?C) to induce crystallinity. The structural property of these samples was characterized by using X-ray Diffraction (XRD) and Raman spectrometer. The surface morphology of the films was analysed by Field Emission Scanning Electron Microscopy (FESEM) and Atomic Force Microscopy (AFM). The presence of pure anatase phase with enhanced polycrystalline nature was evident for the films annealed at 350 and 450 ?C. Due to the addition of Sm, the titania thin films exhibited increased crystallinity. The Raman analysis also support the presence of crystalline anatase phase and the existence of defects in the deposited films. The prepared samples were also subjected to photocatalytic activity studies by using methyl orange (MO) dye and the results are discussed herein. The rate constant increased and half life time decreased considerably for 0.4 at% doped samples. The current work provides new ideas for monitoring the structural properties by adding low concentration rare earth dopant into metal oxides (titania) suitable for various applications.     

Synthesis and characterization of polythiophene/titanium dioxide composites

Polythiophene/titanium dioxide (PT/TiO₂) composites were prepared by the in situ chemical oxidative polymerization method. The resulting PT/TiO₂ composites were characterized by Fourier transform infrared (FT-IR) spectroscopy, ultraviolet–visible (UV–Vis) diffuse reflectance spectroscopy, X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and field emission scanning electron microscopy (SEM). UV–Vis diffuse reflectance spectra measurements show that the PT/TiO₂ composites can adsorb light of wavelengths ranging from 200 nm to 800 nm. The PT/TiO₂ composites showed good adsorption properties and were more efficient in removing dye from solution than pure PT and pure TiO₂. The PT/TiO₂ composites exhibited photocatalytic activities to some extent under UV light illumination.     

钇掺杂有序多孔TiO2薄膜的制备与可见光催化性能

采用胶体晶体薄膜为模板,利用溶胶–凝胶法制备了钇掺杂有序多孔TiO2薄膜,通过Fourier变换红外光谱、扫描电子显微镜、X射线衍射、X射线光电子能谱、紫外–可见光谱表征样品的结构和形貌,并以甲基橙为模型化合物研究了钇掺杂有序多孔TiO2薄膜材料可见光催化性能。结果表明：钇掺杂有序多孔TiO2薄膜规整致密,晶型为锐钛矿型,样品中钇元素含量约为1.2%。钇掺杂使得TiO2吸收光红移至可见光区,钇掺杂有序多孔TiO2薄膜可见光催化性能好于未掺杂有序多孔TiO2薄膜。     

Polymer-assisted freeze-drying synthesis of Ag-doped ZnO nanoparticles with enhanced photocatalytic activity

Ag-doped ZnO nanoparticles with high and stable photocatalytic activity were prepared by polymer-assisted freeze-drying method with simple process and without organic solvents used. The structural morphology and optical properties of Ag-doped ZnO nanoparticles were characterized by X-ray Diffraction (XRD), Inductive Coupled Plasma Optical Emission Spectrometry (ICP-OES), Field Emission Scanning Electron Microscopy (FESEM), Transmission Electron Microscopy (TEM) and high resolution TEM (HRTEM) with energy dispersive X-ray spectroscopy, Ultraviolet-visible Diffuse Reflectance Spectroscopy (UV–vis DRS), X-ray Photoelectron Spectroscopy (XPS) and Fourier Transmission Infrared Spectroscopy (FTIR). Moreover, the thermoanalytical measurements (TGA–DTG) analysis is carried out for proper calcination temperature. XRD results show that Ag nanoparticles were successfully doped into ZnO lattice, and UV–vis DRS results indicate that the doped Ag nanoparticles result in ZnO exhibiting enhanced light trapping capability in the 400?nm and 600?nm range. The photocatalytic activity of Ag-doped ZnO was examined by analyzing the degradation of methyl orange (MO) and methylene blue (MB) dyes under UV light and solar light irradiation, and the results show that all Ag-doped ZnO nanoparticles exhibit better photocatalytic activity than those of pure ZnO nanoparticles at the same degradation conditions; especially the synthesized Ag-ZnO nanoparticles are easy to be recycled and have high photocatalytic stability. Based on the experimental results, the photocatalytic electron transfer path and the photocatalytic mechanism of Ag-ZnO nanoparticles under UV and solar irradiation conditions are explained and clarified.     

溶胶–凝胶法制备太阳光谱选择性吸收薄膜的研究进展

从太阳光谱选择性吸收薄膜的作用原理、吸收材料和膜系结构特点出发,结合实际工作,综述近年来溶胶–凝胶法制备的纳米颗粒–电介质复合材料型和尖晶石结构过渡金属氧化物型两类太阳光谱选择性吸收薄膜的研究进展,并探讨目前存在的问题及今后研究的方向。与以溅射为代表的现代气相沉积技术制备薄膜相比,溶胶–凝胶法制备的这两类薄膜具有与之相当的光学性能(吸收率α>0.90,发射率ε<0.10)和优异的湿热稳定性,同时还具有工艺简便、设备要求低以及易于大面积制膜等优点;但是溶胶–凝胶法引入了溶液中的化学反应,组分间的兼容性以及化学反应的特异性使得难以通过简单变换化学组分获得种类繁多的薄膜,因而目前溶胶–凝胶法制备的太阳光谱选择性吸收薄膜还局限在少数材料上。