Effect of Ce doping on microstructural,morphological and optical properties of ZrO2 nanoparticles

Pure and Ce doped ZrO₂ nanostructures have been synthesized by the microwave irradiation method. The prepared nanoparticles were characterized by various analytical techniques like Thermogravimetric and Differential Thermal Analysis (TG–DTA), X-Ray Diffraction (XRD), Fourier Transform Infra-Red Spectroscopy (FTIR), Scanning Electron Microscopy (SEM), Energy Dispersive Spectrum (EDS) and Transmission Electron Microscopy (TEM). The XRD pattern of Ce doped ZrO₂ nanoparticles have been confirms that the tetragonal structure. TEM observations indicated that the average particle size of the pure ZrO₂ some particles spherical shaped and some particles agglomeration in the range of 16–44 nm. Whereas on addition of Ce agglomeration in the range of 32–56 nm. The pure ZrO₂ and Ce doped ZrO₂ nanoparticles were further characterized for their optical properties by UV–vis reflectance spectra (DRS) and Photoluminescence (PL) spectroscopy.     

Nitrogen dioxide (NO2) sensing performance of p-polypyrrole/n-tungsten oxide hybrid nanocomposites at room temperature

Polypyrrole (PPy)–tungsten oxide (WO₃) hybrid nanocomposite have been successfully synthesized using different weight percentages of tungsten oxide (10–50%) dispersed in polypyrrole matrix by solid state synthesis method. The sensor based on PPy–WO₃ was fabricated on glass substrate using cost effective spin coating method for detection of NO₂ gas in the low concentration range of 5–100 ppm. The gas sensing performance of hybrid material was studied and compared with those of pure PPy and WO₃. It was found that PPy–WO₃ hybrid nanocomposite sensor can complement the drawbacks of pure PPy and WO₃. The structure, morphology and surface composition properties of PPy–WO₃ hybrid nanocomposites were employed by X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, field emission scanning electron microscopy (FESEM), Transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). The presence of WO₃ in PPy matrix and their interaction was confirmed using XRD, FTIR techniques. The porous surface morphology was observed with addition of WO₃ in PPy matrix which is useful morphology for gas sensing applications. TEM image of PPy–WO₃ hybrid nanocomposites shows the average diameter of 80–90 nm. X-ray photoelectron spectroscopy (XPS) was used to characterize the chemical composition of nanocomposites. It was observed that 50% WO₃ loaded PPy sensor operating at room temperature exhibit maximum response of 61% towards 100 ppm of NO₂ gas and able to detect low concentration of 5 ppm NO₂ gas with reasonable response of 8%. The hybrid sensor shows better sensitivity, selectivity, reproducibility and stability compared to pure PPy and WO₃. The proposed sensing mechanism of hybrid nanocomposite in presence of air and NO₂ atmosphere was discussed with the help of energy band diagram. Furthermore, the interaction of NO₂ gas with PPy–WO₃ hybrid nanocomposites sensor was studied by cole–cole plot using impedance spectroscopy.     

Investigation of structural,optical and morphological properties of copper doped zinc sulphide nanoparticles

Semiconductor nanoparticles doped with transition metal ions can influence the transition probabilities and electronic structure. The undoped and copper doped zinc sulphide nanoparticles with various concentrations are synthesized by wet chemical co-precipitation method. These nanoparticles are characterized by using X-ray powder diffraction (XRD), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), Selected Area Electron Diffraction (SAED), UV–visible (UV–vis) absorption spectroscopy, Fourier Transform Infrared (FT-IR) Spectroscopy, conductivity measurement and time-resolved photoluminescence studies. X-ray powder diffraction analysis reveals that the synthesized samples have cubic zinc blende structure. The Scanning Electron Microscope shows the synthesized nanoparticles are agglomerated. The UV–visible spectra reveal the absorption edge is red shifted. The FT-IR spectra show vibrational peaks around 617 cm⁻¹ which indicate the presence of Cu–S stretching modes. The AC conductivity measurement confirms the semiconducting nature and shows a marked increase in conductivity as the doping concentration of copper increases. The photoluminescence shows that the emission at 426 nm may be due to transition from the conduction band to the zinc vacancies. These transition metal ions doped semiconductor nanoparticles have important applications in solid state lighting, imaging, and other photonic devices.     

Biologically synthesized copper sulfide nanoparticles: Production and characterization

In the present research, copper sulfide nanoparticles were synthesized through a low-cost and environmentally friendly method using the fungus Fusarium oxysporum for the first time. The extracellularly generated nanoparticles were characterized by UV–vis, Florescence Spectroscopy, Fourier Transform Infrared Spectroscopy (FTIR), and Transmission Electron Microscopy (TEM). According to the UV–vis, Florescence and FTIR analysis, it was confirmed that the biosynthesized nanoparticles were created of copper sulfide composition. Moreover, from the morphological point of view, TEM images demonstrated that spherical particles having the size of 2–5 nm were entangled in spherical peptide shells which were about 20 nm in diameter.     

Effect of ethyl cellulose on thermal resistivity of thixotropic ZnO nano-particle paste for thermal interface material in light emitting diode application

A large amount of heat trapped inside Light Emitting Diode (LED) is the consequence of large thermal resistance between the heat source and the heat sink. Zinc oxide (ZnO) thick film was screen-printed from thixotropic paste that consisted of binder, filler and solvent to act as thermal interface material. Structural, surface morphology, vibrational and thermal properties of the samples were studied by means of Field Emission Scanning Electron Microscopy (FESEM), Atomic Force Measurement (AFM), Fourier Transform Infrared Spectroscopy (FTIR) and Thermal Transient Tester (T3ster). XRD analysis revealed that the formation of hexagonal wurtzite ZnO powder, which is free of hydroxide. FESEM results indicated that 50 wt% of filler loading in the thick film had created longer thermal transportation chain. The surface roughness of thick film displays variation in the range of from 64.8 to 218 nm. The presence of ZnO and binder were confirmed by FTIR spectrum at 518 cm⁻¹ and 668 cm⁻¹ to 2974 cm⁻¹, respectively. Thermal characterization reveals a drop in film’s resistivity with the higher content of filler loading of 50 wt% and 55 wt%. The lowest rise in junction temperature of tested LED is reported to be 14.7 °C of 50 wt% of filler loading.     

Discrete phase method particle simulation of ultra-fine package assembly with SAC305-TiO2 nano-reinforced lead free solder at different weighted percentages

This paper presents a 3D numerical simulation of nano-reinforced lead (Pb)-free solder at the ultra-fine joint component for 01005 capacitor with dimension of 0.2 × 0.2 × 0.4 mm³. The nano-reinforced particles introduced in the Sn-3.0Ag-0.5Cu (SAC305) solder is titanium oxide (TiO₂) nanoparticles with approximate diameter of ≈ 20 nm at different weight percentages of 0.01, 0.05 and 0.15 wt% respectively. The 3D model developed is based on the reflow thermal profile of nano-reinforced Pb-free solder in the wetting zone temperature of 217 °C–239 °C. A two way interactions utilizing both volume of fluid method (VOF) and discrete phase method (DPM) are introduced in the current study. The study effectively shows the distribution of the nanoparticles as it is being doped in the molten solder after undergoing soldering process. Based on the findings, it was shown that good agreement can be seen between experimental data obtained using High Resolution Transmission Electron Microscope (HRTEM) system as compared to multiphase DPM based simulation. At weight percentage of SAC305 + 0.05% TiO₂ nanoparticles, the nanoparticles are well distributed. The fillet height of nano-reinforced solder also meets the minimum requirement for 01005 capacitor. Additionally, as the weight percentage of the doped nanoparticles increases, the time required for the formation of wetted solder also increases. In terms of the velocity and pressure distribution of the nano-reinforced lead (Pb)-free solder, higher weight percentage of doped nanoparticles have higher velocity distribution and lower pressure distributions.     

Room temperature NO2 gas sensing properties of DBSA doped PPy–WO3 hybrid nanocomposite sensor

We demonstrate the chemiresistive NO₂ gas sensor based on DBSA doped PPy–WO₃ hybrid nanocomposites operating at room temperature. The sensor was fabricated on glass substrate using simple and cost effective drop casting method. The gas sensing performance of sensor was studied for various toxic/flammable analytes like NO₂, C₂H₅OH, CH₃OH, H₂S and NH₃. The sensor shows higher selectivity towards NO₂ gas with 72% response at 100 ppm. Also the sensor can successfully detect low concentration of NO₂ gas upto 5 ppm with reasonable response of 12%. Structural, morphological and compositional analyses evidenced the successful formation of DBSA doped PPy–WO₃ hybrid nanocomposite with uniform dispersion of DBSA into PPy–WO₃ hybrid nanocomposite and enhance the gas sensing behavior. We demonstrated that DBSA doped PPy–WO₃ hybrid nanocomposite sensor films shows excellent reproducibility, high stability, moderate response and recovery time for NO₂ gas in the concentration range of 5–100 ppm. A gas sensing mechanism based on the formation of random nano p–n junctions distributed over the surface of the sensor film has been proposed. In addition modulation of depletion width takes place in sensor on interaction with the target NO₂ gas has been depicted on the basis of schematic energy band diagram. Impedance spectroscopy was employed to study bulk, grain boundary resistance and capacitance before and after exposure of NO₂ gas. The structural and intermolecular interaction within the hybrid nanocomposites were explored by Raman and X-ray photoelectron spectroscopy (XPS), while field emission scanning electron microscopy (FESEM) was used to characterize surface morphology. The present method can be extended to fabricate other organic dopent-conducting polymer–metal oxide hybrid nanocomposite materials and could find better application in the gas sensing.     

Effect of oxygen vacancy in tungsten oxide on the photocatalytic activity for decomposition of organic materials in the gas phase

The relationship between the oxygen vacancy of tungsten oxide and its ability to decompose organic materials under visible-light irradiation was investigated experimentally. In the field of rechargeable batteries, the highest charge-discharge rate is obtained when tungsten oxide is used as a negative electrode with an O/W ratio of 2.72. This result suggested that the number of oxygen vacancies in tungsten oxide affects the photocatalytic decomposition behavior of organic materials. Therefore, with the aim of increasing the photocatalytic activity of tungsten oxide to decompose organic materials, we attempted to clarify the role of the oxygen vacancy. WO_3 − x nanoparticles, including WO_2.83 and WO_2.72 nanoparticles, were fabricated by changing the annealing temperature in a 10% H₂, 90% N₂ atmosphere to generate different densities of oxygen vacancies. Tungsten oxide with O/W ratios of 2.83 and 2.72 exhibited no photocatalytic activity for the photodecomposition of organic materials. The maximum decomposition rate was obtained for stoichiometric WO₃ (O/W = 3). The reason for the decrease or disappearance of the photodecomposition ability should originate in the increase in the number of electrons generated by the oxygen vacancies. These excess electrons promote the recombination reaction between electrons and holes in WO_3 − x, and hence reduce the lifetime of electron-hole pairs.     

Effect of fluorine doping on the structural,optical and electrical properties of spray deposited cadmium stannate thin films

Cadmium stannate (Cd₂SnO₄) thin films were coated on Corning 1737 glass substrates at 540 °C by spray pyrolysis technique, from the aqueous solution of cadmium acetate and tin (II) chloride precursors. Fluorine doped Cd₂SnO₄ (F: Cd₂SnO₄) thin films were prepared by adding ammonium fluoride in the range of 0–5 wt% of the total weight of cadmium acetate and tin (II) chloride in the spray solution. Thickness of the prepared films is about 300 nm. X-ray diffraction analysis of the Cd₂SnO₄ and 3 wt% F: Cd₂SnO₄ films shows the signature for the growth along (222) direction. Scanning electron micrographs showed that fluorine doping effectively modifies the surface morphology of Cd₂SnO₄ films. Average optical transmittance in the visible region (500–850 nm) for Cd₂SnO₄ is ~79% and it is increased to ~83% for 1 wt% doping concentration of the NH₄F in the solution. Fluorescence spectra of F: Cd₂SnO₄ (1 wt% and 3 wt%) exhibit peak at 601 nm. F: Cd₂SnO₄ film (1 wt%) shows mobility of ~42 cm²/V s, carrier concentration of ~9.5×10¹⁹ cm^?3 and resistivity of ~1.5×10^?3 Ω cm.     

Structure,cation valence states and electrochemical properties of nanostructured Mn3O4

Nanostructured Mn₃O₄ with an average crystallite of ~10 nm is synthesized by the controlled reduction of potassium permanganate using hydrazine. The phase purity, average crystallite/particle size, morphology and state of agglomeration were studied using X-ray diffraction (XRD), Transmission Electron microscopy (TEM) and Scanning Electron Microscopy (SEM) analyses. Nitrogen sorption studies give a specific surface area of 62 m²/g and also reveal the mesoporous nature. The presence of Mn⁴⁺ ions is inferred from the Fourier Transform Infra-Red (FTIR) spectroscopy and X-ray Photoelectron Spectroscopy (XPS) studies. The decrease in the c/a ratio obtained from XRD analysis also indicates the presence of Mn⁴⁺ ions. Electrochemical analysis was done on a symmetric capacitor with nanostructured Mn₃O₄ as the active material and 6 M KOH solution as the electrolyte. Cyclic voltammograms revealed pseudocapcitive behavior with specific capacitance values falling sharply with scan rate. The power density and energy density values obtained from chornopotentiograms are fairly large and indicate the potential application in the field of supercapacitors.     

Simplified phosphorescent organic light-emitting diodes with a WO3-doped wide bandgap organic charge transport layer

The effects of p-type doping of wide bandgap ambipolar 4,4′-N,N′-dicarbazolebiphenyl (CBP) with WO₃ were investigated through detailed electrical device characterization. It was found that, to achieve effective doping for improved hole injection and transport, the doping level should be greater than 20 mol% and the doped layer should be at least 10 nm thick. A large downward shift of the Fermi level in WO₃-doped CBP causes band bending and depletion at the doped/undoped CBP interface, resulting in an additional energy barrier which hampers hole transport. Simplified green phosphorescent organic light-emitting diodes (PhOLEDs) with CBP as the hole transport and host material were fabricated. With a WO₃-doped hole transport layer, the PhOLEDs attained brightness of 11,163 cd/m² at 20 mA/cm², and exhibited an improved reliability under constant-current stressing as compared to undoped PhOLEDs.     

Growth and characterization of silicon oxide films formed in the presence of Si,SiC, and Si3N4

In order to comparatively study the growth and characterization of silicon oxide films on Si-based substrates, top-cut solar grade silicon (SOG-Si) containing Si₃N₄ rods and SiC lumps were used as raw materials and respectively heated at 1773 K and 1873 K under Ar gas. The samples were investigated by Focus Ion Beam/Scanning Electron Microscope (FIB/SEM) and Energy Dispersive Spectroscopy (EDS). Results indicated that silicon oxides with different morphologies successfully grew on the substrates via various mechanisms. Passive oxidation was evident in the formation of a dense SiO₂ surface layer on the base material at 1773 K, while active oxidation was evident in the formation of SiO₂ with particle, rod, and nanowire-like morphologies, which was the re-oxidation product of SiO at 1873 K under the active-to-passive transition. Si, SiC, and Si₃N₄ have the similar oxidation tendency to form silicon oxides under either passive or active regimes.     

Hydrothermal synthesis of WO3 films on the TiO2 substrates and their photochromic properties

Tungsten oxide (WO₃) films have been prepared on the synthesized TiO₂ substrates from a sodium tungsten precursor via a hydrothermal method. X-ray diffraction, scanning electron microscopy and transmission electron microscopy analyses were used to investigate the effect of precursor concentrations on the structures and morphologies of the films. Ordered WO₃ films were successfully synthesized on the as-grown TiO₂ substrates. With the concentrations increasing from 0.001 M to 0.024 M, the morphologies of the films changed from multi-layer laminated structure to ladder-shaped lamellar structure finally columnar structure. The results also showed that with an increase in precursor concentration, the observed absorptions at 365 nm of the films increased until precursor concentration of 0.016 M, and then decreased with higher concentration. The film obtained with precursor concentration of 0.016 M on the TiO₂ substrate had the best photochromic properties.     

Rapid thermal annealing of cerium dioxide thin films sputtered onto silicon (111) substrates: Influence of heating rate on microstructure and electrical properties

The impact of the heating rate (HR) of a Rapid Thermal Annealing (RTA) on the crystallinity and on the morphology of CeO₂ thin films has been investigated by Raman Spectroscopy (RS), Photoluminescence (PL), Scanning Electron Microscopy (SEM), Energy Dispersive Spectroscopy (EDS), and tapping mode Atomic Force Microscopy (AFM). The electrical properties of CeO₂ thin films have also been studied with the Conductive AFM mode. This paper highlights the importance of the heating rate value used during an RTA on crystalline quality, morphology and on the electrical properties of the CeO₂ layer. In fact, the best crystallinity with a good morphology and a high resistivity has been obtained for a CeO₂ layer sputtered on (111) Si substrate and post-annealed at 1000 °C for 30 s with an HR of 25 °C/s.     

High thermal annealing effect on structural and optical properties of ZnO–SiO2 nanocomposite

The effect of annealing temperature on photoluminescence (PL) of ZnO–SiO₂ nanocomposite was investigated. The ZnO–SiO₂ nanocomposite was annealed at different temperatures from 600 °C to 1000 °C with a step of 100 °C. High Resolution Transmission Electron Microscope (HR-TEM) pictures showed ZnO nanoparticles of 5 nm are capped with amorphous SiO₂ matrix. Field Emission Scanning Electron Microscope (FE-SEM) pictures showed that samples exhibit spherical morphology up to 800 °C and dumbbell morphology above 800 °C. The absorption spectrum of ZnO–SiO₂ nanocomposite suffers a blue-shift from 369 nm to 365 nm with increase of temperature from 800 °C to 1000 °C. The PL spectrum of ZnO–SiO₂ nanocomposite exhibited an UV emission positioned at 396 nm. The UV emission intensity increased as the temperature increased from 600 °C to 700 °C and then decreased for samples annealed at and above 800^°C. The XRD results showed that formation of willemite phase starts at 800 °C and pure willemite phase formed at 1000 °C. The decrease of the intensity of 396 nm emission peak at 900 °C and 1000 °C is due to the collapse of the ZnO hexagonal structure. This is due to the dominant diffusion of Zn into SiO₂ at these temperatures. At 1000 °C, an emission peak at 388 nm is observed in addition to UV emission of ZnO at 396 nm and is believed to be originated from the willemite.     

Detection of H2S,SO2, and NO2 using electrostatic sprayed tungsten oxide films

This paper presents the electrostatic spray deposition of tungsten oxide (WO₃) films for the detection of different pollutant gases. The influence of several types of precursors on the structure and morphology of the films was studied by means of X-ray diffraction (XRD) and scanning electron microscopy (SEM) techniques. This preliminary study allowed to select the proper precursor for the preparation of pure and porous WO₃ films which offer high gas response (R_air/R_gas=1200) to low concentrations of H₂S (10 ppm) at low operating temperature (200 °C). The gas response to NO₂ and SO₂ is low at this temperature suggesting no possible interference with these two gases during the H₂S detection. Furthermore, the films are able to detect very low concentrations of NO₂ (less than 1 ppm) at 150 °C.     

Fabrication and performance evaluation of symmetrical supercapacitor based on manganese oxide nanorods–PANI composite

Manganese oxide nanorods distributed over polyaniline (PANI) network was prepared by one step facile synthesis condition. pH of the reactant solution was tuned using sulfuric acid. Effect of pH on the morphology, chemical composition, structure and electrochemical performance of the prepared materials were studied. Thermal investigation reveals the decomposition of PANI at temperatures below 600 °C. Structural details and chemical composition of the compound was obtained from XRD, FTIR and XPS studies. α type MnO₂ was found to be crystallized in the prepared MnO₂–PANI composite. Single crystal manganese oxide nanorods distributed over the PANI network was cognizant from the FESEM and HRTEM investigations. Nanorods of average diameter 82 nm and length 482 nm were obtained without deploying any surfactants or templates. Electrochemical techniques like Cyclic Voltammetry (CV), Chronopotentiometry (CP) and Electrochemical Impedance Spectroscopy (EIS) were utilized. Study results indicate that the composites prepared shows excellent electrochemical performance. Among the prepared materials, MnP-46 exhibits a maximum specific capacitance of 687 Fg⁻¹ at 5 mV s⁻¹ scan rate and a capacitance retention of 95% over 2000 cycling. Promising performance of MnP-46 was further tested in a symmetrical two cell configuration. The cell was operative upto 1 V potential window. MnP-46 in a symmetrical arrangement demonstrates 179 Fg⁻¹ at 5 mV/s scan rate. High conductivity of the electrode material was confirmed from the Nyquist plot.     

Synthesis of highly selective and sensitive Cu-doped ZnO thin film sensor for detection of H2S gas

Copper (Cu) doped zinc oxide (ZnO) thin films were successfully prepared by a simple sol-gel spin coating technique. The effect of Cu doping on the structural, morphology, compositional, microstructural, optical, electrical and H₂S gas sensing properties of the films were investigated by using XRD, FESEM, EDS, FTIR, XPS, Raman, HRTEM, and UV–vis techniques. XRD analysis shows that the films are nanocrystalline zinc oxide with the hexagonal wurtzite structure and FESEM result shows a porous structured morphology. The gas response of Cu-doped ZnO thin films was measured by the variation in the electrical resistance of the film, in the absence and presence of H₂S gas. The gas response in relation to operating temperature, Cu doping concentration, and the H₂S gas concentration has been systematically investigated. The maximum H₂S gas response was achieved for 3 at% Cu-doped ZnO thin film for 50 ppm gas concentration, at 250 °C operating temperature.     

WO3/TiO2 nanocomposites: Salt–ultrasonic assisted hydrothermal synthesis and enhanced photocatalytic activity

A series of WO₃/TiO₂ composite photocatalysts were fabricated via a facile salt–ultrasonic assisted hydrothermal process. The obtained samples were characterized by X-ray diffraction, scanning eletron microscopy, energy dispersive X-ray spectroscopy and UV–vis diffused reflectance spectroscopy. It was confirmed that anatase TiO₂ and monoclinic WO₃ coexisted in the composites. The photocatalytic activity of as-prepared WO₃/TiO₂ composites for degradation of Rhodamin B (RhB) under visible light irradiation was investigated. The results showed that WO₃/TiO₂ composites have a higher photocatalytic activity than those of pure TiO₂ and pure WO₃. First-principle calculations based on density functional theory were performed to explore the electronic structure and illustrate the photocatalytic mechanism of WO₃/TiO₂. The calculated energy gap was 2.53 eV, which was close to the experimental observation (2.58 eV). Due to the combination of WO₃/TiO₂, the photoinduced electrons and holes transfer between the WO₃ and TiO₂ in opposite directions, thus providing sufficient charge separation, which contributed to the photocatalytic activity enhancement.     

Effect of calcination temperature on Cu doped NiO nanoparticles prepared via wet-chemical method: Structural,optical and morphological studies

In the present study, NiO and Cu-doped NiO nanoparticles were successfully synthesized by wet chemical method at room temperature using sodium hydroxide (NaOH) as precipitating agent. The as-prepared Cu-doped NiO powder samples were subjected to three different calcination temperatures such as, 350 °C, 450 °C and 550 °C in order to investigate the impact of calcined temperatures on the phase formation, particle size and band gap evolution. The phase formation and crystal structure information of the prepared nanomaterials were examined by X-ray powder diffraction (XRD). XRD revealed the face-centered cubic (FCC) structure. Average crystalline size of pure and doped samples estimated using Scherer formula was found to be 15 nm and 9 nm respectively. With increase in the calcination temperature from 350 °C to 550 °C for the Cu doped NiO samples the particle size of the nanoparticles was found to increase from 4 nm to 9 nm respectively. The optical study for both pure and doped NiO nanoparticles was performed using an UV–Vis spectrophotometer in the wavelength range of 200–800 nm. The strong absorption in the UV region confirms the band gap absorption in NiO and was estimated from the UV–Vis diffuse reflectance spectra via Tauc plot. Systematic studies were also carried out to study the effect of calcination on the optical transmittance. Samples were also investigated using Raman and Fourier Transform Infrared Spectroscopy (FTIR). Furthermore, morphology of the pure NiO and Cu-doped NiO Nanoparticles were examined by scanning electron microscope (SEM).