Effect of processing parameter on structural,optical and electrical properties of photovoltaic chalcogenide nanostructured RF magnetron sputtered thin absorbing films

The aim of this work was to develop high quality of CuIn_1−xGa_xSe₂ thin absorbing films with x (Ga/In+Ga)<0.3 by sputtering without selenization process. CuIn_0.8Ga_0.2Se₂ (CIGS) thin absorbing films were deposited on soda lime glass substrate by RF magnetron sputtering using single quaternary chalcogenide (CIGS) target. The effect of substrate temperature, sputtering power & working pressure on structural, morphological, optical and electrical properties of deposited films were studied. CIGS thin films were characterised by X-ray diffraction (XRD), Field emission scanning electron microscope (FE-SEM), Energy dispersive X-ray spectroscopy (EDAX), Atomic force microscopy (AFM), UV–vis–NIR spectroscopy and four probe methods. It was observed that microstructure, surface morphology, elemental composition, transmittance as well as conductivity of thin films were strongly dependent on deposition parameters. The optimum parameters for CIGS thin films were obtained at a power 100 W, pressure 5 mT and substrate temperature 500 °C. XRD revealed that thin film deposited at above said parameters was polycrystalline in nature with larger crystallite size (32 nm) and low dislocation density (0.97×10¹⁵ lines m⁻²). The deposited film also showed preferred orientation along (112) plane. The morphology of the film depicted by FE-SEM was compact and uniform without any micro cracks and pits. The deposited film exhibited good stoichiometry (Ga/In+Ga=0.19 and In/In+Ga=0.8) with desired Cu/In+Ga ratio (0.92), which is essential for high efficiency solar cells. Transmittance of deposited film was found to be very low (1.09%). The absorption coefficient of film was ~10⁵ cm⁻¹ for high energy photon. The band gap of CIGS thin film evaluated from transmission data was found to be 1.13 eV which is optimum for solar cell application. The electrical conductivity (7.87 Ω⁻¹ cm⁻¹) of deposited CIGS thin film at optimum parameters was also high enough for practical purpose.     

Effects of process parameters on the synthesis and characterization of CuIn1−xGaxSe2 nanopowders produced by new modified solvothermal method

In this research, CuIn_1?xGa_xSe₂ (CIGS) nanopowders were synthesized by a new modified solvothermal process which utilized a controllable internal pressure and a stirring system during the process. The effects of process parameters on the synthesis and characterization of CIGS nanopowders were studied including reaction temperature, process time, applying internal imposed pressure, and Ga substitution with In. Chloride sources of copper, indium, and selenium powders along with gallium nitrate powder were used as precursor materials which were dissolved in triethylenetetramine as a solvent at various synthesis conditions to prepare final products in a specific autoclave. Crystal structure, morphology, and optical properties of prepared nanopowders were characterized using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), field emission scanning electron microscopy (FESEM), energy dispersive X-ray analysis (EDX), high-resolution transmission electron microscopy (HRTEM), and diffuse-reflectance UV/vis spectroscopy (DRS). The results indicate that using both a stirring system and internal imposed pressure of 400 kPa have significant effects on the synthesis of single phase CIGS nanopowders and their crystallinity in short process time. It is also showed that samples synthesized under conditions of internal imposed pressure and long process time could form the rosette-like particles. Furthermore, optical measurements revealed that the band gap energies for prepared particles (1.05–1.38 eV) are close to those of bulk materials.     

Synthesis and characterization of TiO2-doped Polyaniline nanocomposites by chemical oxidation method

Polyaniline (PANI)/TiO₂ nanocomposite samples with various dopant percentages of TiO₂ were synthesized at room temperature using a chemical oxidative method. The samples were characterized by ultraviolet-visible spectrometer, Fourier transform infrared (FTIR) spectrometer, X-ray diffraction (XRD), scanning electron microscopy (SEM), EDAX and conductivity measurements. Incorporation of TiO₂ nanoparticles caused a slight red shift at 310 nm in the absorption spectra due to the interactions between the conjugated polymer chains and TiO₂ nanoparticles with π–π^? transition. FTIR confirmed the presence of TiO₂ in the molecular structure. In PANI/TiO₂ composites, two additional bands at 1623 cm^?1 and 1105 cm^?1 assigned to Ti–O and Ti–O^–C stretching modes were present. It can be concluded that Ti organic compounds are formed with an alignment structure of TiO₂ particles. XRD patterns revealed that, as the TiO₂ percentage was increased, the amorphous nature disappeared and the composites became more strongly oriented along the (1 1 0) direction, which showed the tetragonal structure of nanocrystalline TiO₂. SEM studies revealed the formation of uniform granular morphology with average grain size of 200 nm for (50%) PANI/TiO₂ nanocomposite samples.     

Optical properties of ZnS nanoparticles prepared by high energy ball milling

In this work, we synthesized zinc sulfide (ZnS) nanoparticles by the mechanochemical route using zinc acetate and sodium sulfide as source materials in a high energy planetary ball mill at rotation speed of 300 rpm with ball to powder ratio 5:1 for 30–120 min. Powder samples were collected at duration of 30 min for different analyses. The milled powders were washed with methanol to remove impurity and dried at 50 °C for 2 h. ZnS nanoparticles are characterized by X-ray diffraction, transmission electron microscopy, field-emission scanning electron microscopy, UV–vis–NIR spectrophotometry and fluorescence spectrophotometry. The crystallite size of synthesized ZnS nanoparticles is found to be approximately 2 nm. The optical band gap of the ZnS nanoparticles is found to be in the range of 4.71–5.17 eV. Room temperature photoluminescence (PL) spectra of the samples exhibit blue-light emission using UV excitation wavelength of 280 nm.     

Structural,optical and antibacterial properties of nanocrystalline Zn1–xLaxO compound semiconductor

The Zn_1–xLa_xO powders were synthesized by the planetary ball milling method. An accumulated milling time of 15 h with a milling speed of 400 rpm were found to be the optimum milling conditions. The crystal structure, morphology, selected area electron diffraction, and elemental analysis were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and energy dispersive spectroscopy. The solubility limit of La that could substitute at the Zn sites was only 5 mol% or x=0.05. The dependence of the crystallite size on the La doping content can be explained by the Zener pinning effect. The particle size of the milled ZnO powder was about 34.03 nm and the particle size was reduced to 30.90 nm when doped with 10 mol% La. The particles of all milled samples could agglomerate as a cluster. The largest E_g value of 3.14 eV was obtained from the Zn_0.97La_0.03O powder due to this sample having the smallest crystallite size. The Zn_1–xLa_xO powders can inhibit Staphylococcus aureus better than Escherichia coli due to the presence of an extra lipopolysaccharide layer on the outer surface of the latter.     

Electrodeposition of CuIn1−xGaxSe2 solar cells with a periodically-textured surface for efficient light collection

The photoresponse of CuIn_1?xGa_xSe₂ (CIGS) solar cells is improved using a periodically-textured structure as an antireflection layer. The CIGS absorber layers were prepared by one-step electrodeposition from an aqueous solution containing 12 mM CuSO₄, 25 mM In₂(SO₄)₃, 28 mM Ga₂(SO₄)₃, and 25 mM SeO₂. The electrodeposited CIGS films exhibit the (112)-preferred orientation of the chalcopyrite structures and feature improved film stoichiometry after the selenization process. In addition, the lower bandgap value of 0.97 eV is caused by the discrepancy of the reduction potentials for each constituent, resulting in insufficient Ga content in the deposited films. Using self-assembled silica nanoparticles as the etching mask, periodically-textured structures can be easily formed on an indium tin oxide (ITO)-coated soda lime glass to achieve a low average reflection (<10.5%) in a wide wavelength and incident angle range. With the periodic textured structures suppressing light reflections from the front surface, the photogenerated current in the semi-transparent CIGS solar cells made with transparent conducting electrodes is 1.82 times higher than they otherwise would be.     

Nanostructured CuO/PANI composite as supercapacitor electrode material

An in-situ polymerization method has been employed to prepare CuO/PANI nanocomposite. The prepared samples have been characterized by X-ray diffraction (XRD), FTIR spectroscopy, field emission scanning electron microscopy (FESEM), and BET analysis. Application of the prepared samples has been evaluated as supercapacitor material in 1 M Na₂SO₄ solution using cyclic voltammetry (CV) in different potential scan rates, ranging from 5 to 100 mV s⁻¹, and electrochemical impedance spectroscopy (EIS). The specific capacitance of CuO/PANI has been calculated to be as high as 185 F g⁻¹, much higher than that obtained for pure CuO nanoparticles (76 F g⁻¹). Moreover, the composite material has shown better rate capability (75% capacitance retention) in various scan rates in comparison with the pure oxide (30% retention). EIS results show that the composite material benefits from much lower charge transfer resistance, compared to CuO nanoparticles. Moreover, much better cyclic performance has been achieved for the composite material.     

Cu(In,Ga)Se<Subscript>2</Subscript> Thin Film Preparation from a Cu(In,Ga) Metallic Alloy and Se Nanoparticles by an Intense Pulsed Light Technique

The main contribution of this paper is the development of a novel process for the formation of copper indium gallium diselenide (CIGS) films. CIGS films with a thickness of 4 μm and grain size from 0.3 μm to 1 μm were prepared from a Cu(In_0.7Ga_0.3) (CIG) metallic alloy and Se nanoparticles by the intense pulsed light (IPL) technique. The melting of the CIG and Se nanoparticles and nucleation of CIGS occurred in a very short reaction time of 2 ms. It is believed that the Se diffuses into the CIG lattice to form the CIGS chalcopyrite crystal structure. The tetragonal chalcopyrite crystal structure was confirmed by x-ray powder diffraction (XRD), while the microstructure and composition were determined by field-emission scanning electron microscopy (FESEM), energy-dispersive x-ray spectroscopy (EDAX), and x-ray fluorescence (XRF) spectroscopy.     

Growth of Zn doped Cu(In, Ga)Se2 thin films by RF sputtering for solar cell applications

Cu(In, Ga)Se₂ (CIGS) surface was modified with Zn doping using a magnetron sputtering method. CuInGa:Zn precursor films targeting a CuIn_0.7Ga_0.3Se₂ stoichiometry with increasing Zn content from 0 to 0.8 at% were prepared onto Mo-coated glass substrates via co-sputtering of Cu–Ga alloy, In and Zn targets. The CuInGa:Zn precursors were then selenized with solid Se pellets. The structures and morphologies of grown Zn doped CIGS films were found to depend on the Zn content. At zinc doping level ranging between 0.2 and 0.6 at%, the Zn doping improved the crystallinity and surface morphology of CIGS films. Compared with the performance of the non-doped CIGS cell, the fabricated CIGS solar cell displayed a relative efficiency enhancement of 9–22% and the maximum enhancement was obtained at a Zn content of 0.4 at%.     

Studies on structural,morphological, magnetic and optical properties of chromium sesquioxide (Cr2O3) nanoparticles: Synthesized via facile solvothermal process by different solvents

Chromium sesquioxide (Cr₂O₃) nanoparticles have been successfully synthesized via the facile solvothermal process, by using CrO₃ in different solvents. The as-synthesized nanoparticle sizes are calculated and confirmed to be 25–45 nm, by using X-ray diffraction (XRD) and transmission electron microscopy (TEM). The functional groups of the samples were tested by the Fourier transform infrared (FTIR) spectroscopy. Fine and spherical-like morphologies and compositional elements of the products were observed by the scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) spectroscopy. A weak ferromagnetic (WFM) property was observed for sample by the vibrating sample magnetometer (VSM). The observed band gap values (E_g=4.33–3.54 eV) higher than that of bulk Cr₂O₃ (~3.4 eV) indicated that the particles had been successfully synthesized in the nano region, and measured by ultra-violet visible (UV–vis) absorption spectroscopy. The broad visible emission at ~399 nm, in the photoluminescence spectroscopy revealed the high purity and perfect crystallinity of the samples.     

Photocatalytic degradation of methyl orange and gas-sensing performance of nanosized ZnO

ZnO nanoparticles were synthesized by calcining composites of zinc nitrate and poly(vinyl pyrrolidone) (PVP, molecular weight 30 000) at a mass ratio of 1:2 at 500 °C for 2 h. X-Ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) techniques were used to characterize the as-synthesized ZnO nanoparticles. The particles ranged in size from 30 to 50 nm. Infrared spectra of PVP and the PVP+Zn(NO₃)₂·6H₂O composite revealed coordination between the carbonyl (C=O) of PVP and Zn²⁺ of zinc nitrate, which led to a uniform nanoparticle morphology. The gas-sensing properties and photocatalytic performance of the final product were systematically investigated. The results show that the ZnO nanoparticles exhibit both a high response for ethanol detection and excellent photocatalytic activity for degradation of methyl orange under UV irradiation for 30 min.     

Tunable morphological evolution of in situ gold catalysts mediated silicon nanoneedles

Achieving tunable growth of high quality Silicon (Si) nanoneedles (NNs) is challenging. We report the optimized morphology of in situ gold (Au) catalysts assisted SiNNs grown via very high frequency plasma enhanced chemical vapor deposition (VHF-PECVD) method. The vapor-liquid-solid (VLS) mechanism mediated morphological evolution is tuned using hydrogen (H₂) and silane (SiH₄) gas flow. Au-coated Si(100) substrates are treated using H₂ plasma to create in situ Au nanoparticles (NPs) with high catalytic activity. FESEM images manifested the existence of mono-dispersed Au NPs and high yield of SiNNs having diameter ranging from 80 to 140 nm and lengths up to 2.31±0.3 µm. Furthermore, these NNs gradually became thinner to form sharp tips of diameter as small as 4 nm. XRD pattern confirmed the diamond (cubic) crystalline phases of SiNNs. HRTEM images revealed the occurrence of Au NPs at the crystalline SiNNs tips. Raman spectrum of as-grown SiNNs exhibited the TO phonon mode accompanied by a red-shift (~23.59 cm⁻¹). Synthesized SiNNs displayed extremely low reflectance (~8%) at short wavelengths (λ<700 nm), indicating excellent antireflection properties. Our controllable and optimized growth method may constitute a basis to achieve high quality SiNN arrays, which are beneficial for various applications.     

Synthesis and electrocatalytic properties of manganese dioxide for non-enzymatic hydrogen peroxide sensing

Manganese dioxide nanoparticles were synthesized by chemical reduction route at different growth temperatures of 40 °C, 80 °C, 100 °C and were characterized using X-ray Diffraction (XRD), Field emission scanning electron microscopy (FESEM), X-ray photoelectron spectroscopy (XPS), Cyclic Voltammetry (CV) and chronoamperometry (CA) analysis. FESEM results show that on increasing growth temperature the morphology changes from clusters into mixture of rods and flakes. XPS analysis reveals the formation of MnO₂. Then these particles were immobilized on Pt electrode. A platinum (Pt) electrode modified with low dimensional MnO₂ was investigated as a chronoamperometric (CA) sensor for hydrogen peroxide sensing (H₂O₂). The sample prepared at 100 °C shows good electrocatalytic ability for H₂O₂ sensing when compared with the samples prepared at 40 °C and 80 °C. At an operating potential of 0.3 V vs. Ag/AgCl catalytic oxidation of the analyte is measured for chronoamperometric (CA) monitoring. The CA signals are linearly proportional to the concentration of H₂O₂. It is also found that the morphology of the nanostructure plays a vital role in the detection of H₂O₂.     

Effects of Ga concentration on structural and electrical properties of screen printed-CIGS absorber layers on polyethylene terephthalate

Copper indium gallium diselenide (CIGS) films were deposited as an absorber layer on polyethylene terephthalate (PET) substrates by a screen printing technique using CIGS ink with a Ga content ranging from 0.3 to 0.6. The melting point of PET substrate is 254.9 °C; the average transmission in the visible (400 nm–800 nm) for PET substrates is greater than 85%. Effects of Ga content of the CIGS absorber layer on structural and electrical properties of the CIGS films were studied. The lattice parameters, a and c for all CIGS films were decreased with increasing Ga content. At room temperature, Hall mobility and charge-carrier concentration of the CIGS films varies from 97.2 to 2.69 cm² V⁻¹ s⁻¹ and 9.98×10¹⁶ to 3.23×10¹⁸ cm⁻³, respectively.     

Synthesis,growth and physical properties of silver gallium sulfide single crystals

The temperature oscillation method was used to synthesize dense single-phase polycrystalline AgGaS₂ from high purity elements. AgGaS₂ single crystal of 8 mm diameter and 45 mm length, free of voids and crack was obtained by the descending ampoule with steady ampoule rotation method using the synthesized polycrystalline charge. The grown crystal was subjected to powder X-ray diffraction and single crystal X-ray diffraction. The AgGaS₂ has been studied using differential scanning calorimetry (DSC) technique. The single crystal has high transmission of 75% in the Mid IR region. The band gap energy was calculated using absorption spectrum. The stoichiometric composition of AgGaS₂ was measured using energy dispersive spectrometry (EDAX). The structural and compositional uniformities of AgGaS₂ were studied using micro-Raman scattering spectroscopy at room temperature. The photoluminescence behavior of AgGaS₂ has been analyzed. It shows the maximum emission at 538 nm. The resistivity of the grown single crystal has been measured.     

Synthesis of tungsten disulphide nanoparticles by the chemical vapor condensation method

Crystalline tungsten disulphide nanoparticles were successfully synthesized by the chemical vapor condensation (CVC) method. The process performed as decomposition of tungsten hexacarbonyl over sulphur vapor in inert gas flow, where WS₂ nanoparticles were synthesized by direct reaction between as formed pure tungsten nanoclusters and sulphur vapor. Influence of experimental parameters on shape, size distribution, structure and phase composition of nanoparticles were evaluated by transmission and scanning electron microscopy and X-ray diffraction analysis. The produced nanoparticles have closely spherical shape with the mean size in the range 20–70 nm in diameter dependently of process parameters. Nested “onion-like” structure of nanoparticles was observed. The mean value of interlayer distance in the {0 0 0 1} direction, is about 0.6358±0.031 nm. Due to nanodimensional size, physical properties and layered structure tungsten disulphide nanoparticles have great potential as a solid lubricant material.     

Direct thermal decomposition synthesis and characterization of hematite (α-Fe2O3) nanoparticles

Hematite (α-Fe₂O₃₎ nanoparticles were prepared via direct thermal decomposition method using γ-Fe₂O₃ as a wet chemically synthesized precursor. The precursor was calcinated in air at 500 °C. Samples were characterized by Thermogravimetric analysis (TGA), X-ray diffraction, Infrared, Scanning electron microscopy, Transmission electron microscopy (TEM) and Photon correlation spectroscopy (PCS). TEM and PCS analyses revealed that the average particle size of the α-Fe₂O₃ nanoparticles synthesized at 500 °C are about 18±2 nm and 50±3 nm for 1 h and 24±2 nm and 82±3 nm for 2 h, respectively. The difference in average particle size determined by PCS and TEM analysis is due to the electrostatic forces between particles, and their agglomeration in PCS analysis. Magnetic properties have been detected by a Vibrating sample magnetometry at room temperature. The α-Fe₂O₃ nanoparticles exhibited a weak ferromagnetic behavior at room temperature.     

Promising methane gas sensor synthesized by microwave-assisted Co3O4 nanoparticles

The morphology and gas sensing characteristics of Co₃O₄ nanoparticles prepared using the microwave irradiation were investigated. XRD and TEM are used to analyze the structural and the morphological properties of the prepared nanoparticles. XRD results confirmed the formation of pure phase of these nanoparticles. The gas sensor based on the synthesis Co₃O₄ nanoparticles reveals faster response and recovery time at low temperature detection toward methane gas. Specifically, for methane concentration of 1%, the response and the recovery times at 200 °C are 100 s and 50 s, respectively. Furthermore, the sensing characteristics of Co₃O₄ nanoparticles were improved by increasing the operating temperatures and gas concentrations as well. The experimental results clearly demonstrate the potential use of Co₃O₄ nanoparticles as a sensing material in the fabrication of CH₄ sensors.     

Defects in Zn1−x−yCoxMgyO nanoparticles: Probed by XRD,RAMAN and PAS techniques

Wurtzite Zn_1?x?yMg_xCo_yO nanoparticles of size 14–20 nm are synthesized by the conventional coprecipitation route and are analyzed using XRD, FESEM, UV–visible, Raman, and Positron annihilation spectroscopic techniques. XRD patterns reveal formation of a single wurtzite phase of ZnO on adding Mg, Co or both. In addition to six Raman active modes corresponding to the wurtzite structure of space group C_6ν⁴, we also observe additional Raman modes at 519, 544 and 673 cm^?1 irrespective of the dopant type and concentration. These modes exactly match with the silent vibrational modes of ZnO lattice as calculated by the ab initio calculations. From positron life time measurements, we observe that while the shortest lifetime τ₁, the lifetime of positrons that annihilate in the grain boundary regions match well with the lifetime of positrons in a defect free ZnO (τ₁～158 ps), the intermediate lifetime, τ₂ of all three samples match with the life time of positron annihilating at the cluster of (Zn+O) di-vacancies. We conclude that the origin of additional Raman modes is not due to impurities as reported in the literature rather is due to host lattice defects.     

Effects of graphite on the synthesis of 1-D single crystal In2O3 nanostructures at high temperature

This study investigated the effects of graphite powder on the growth mechanisms of one-dimensional (1-D) single-crystal indium oxide (In₂O₃) nanostructures. The study was conducted using a chemical vapor deposition (CVD) method at 1000 °C; In₂O₃ and graphite powder mixed with In₂O₃, with a weight ratio of 1:1, were used as the source material, while 2 nm-thick n-type silicon (100), coated with a gold catalyst, was used as a substrate. It was observed that nanostructures grew via a Vapor-Liquid-Solid (VLS) growth mechanism when only In₂O₃ was used, but grew via both VLS and Vapor-Solid (VS) growth mechanisms when graphite powder was used with the In₂O₃. The morphology and crystal structures of the nanostructures grown were investigated using X-Ray Diffraction (XRD), High Resolution Transmission Electron Microscopy (HR-TEM), Field Emission Scanning Electron Microscopy (FESEM) and Energy Dispersion X-Ray Spectroscopy (EDS). At room temperature (RT), all the nanostructures showed photoluminescence (PL) spectra at a wavelength of 367 nm in the UV-emission region and at wavelengths of 470 and 630 nm in the visible region.