A study of size dependent structure, morphology and luminescence behavior of CdS films on Si substrate

Size tunable cadmium sulfide (CdS) films deposited by a dip coating technique on silicon (100) and indium tin oxide/glass substrates have been characterized using X-ray diffraction, X-ray reflectivity, transmission electron microscopy, atomic force microscopy and photoluminescence spectroscopy. The structural characterization indicated growth of an oriented phase of cadmium sulfide. Transmission electron microscopy used to calculate the particle size indicated narrow size dispersion. The tendency of nanocrystalline CdS films to form ordered clusters of CdS quantum dots on silicon (100) substrate has been revealed by morphological studies using atomic force microscopy. The photoluminescence emission spectroscopy of the cadmium sulfide films has also been investigated. It is shown that the nanocrystalline CdS exhibit intense photoluminescence as compared to the large grained polycrystalline CdS films. The effect of quantum confinement also manifested as a blue shift of photoluminescence emission. It is shown that the observed photoluminescence behavior of CdS is substantially enhanced when the nanocrystallites are assembled on silicon (100) substrate.     

Synthesis and optical properties of ZnS hollow spheres from single source precursor

A facile one-pot synthesis of ZnS hollow spheres has been carried out via a chemical transformation induced inside-out Ostwald ripening process from a single source precursor. The size and shell thickness of the ZnS hollow spheres can be controlled by adjusting the reaction temperature and reaction time, respectively. Photoluminescence spectra show a dominant emission peak at 470 nm accompanied by several weaker peaks. UV-vis measurement reveals that the obtained ZnS hollow spheres exhibit “hollow effect”. The formation process of ZnS hollow spheres has been discussed.     

Zinc oxide micro- and nanoparticles: Synthesis, structure and optical properties

Zinc oxide (ZnO) spherical nanoparticles (SNPs) and bitter-melon-like (BML) microparticles were synthesized by a hydrothermal route using a zinc (Zn) plate as a source and substrate at various synthesis conditions. The structural analysis confirmed the formation of ZnO with hexagonal wurtzite phase on the hexagonal Zn substrate with growth of the ZnO microparticles along the [1 0 1] direction. The UV-vis absorption spectra of the ZnO microparticles indicated absorption peaks in the UV region which can be attributed to the band gap of ZnO. The room temperature photoluminescence (PL) of the ZnO microparticles exhibited a broad emission band, which is fitted with four Gaussian peaks and were assigned to transitions involving free excitons and various defect centers. The growth model for the formation of ZnO micro- and nanoparticles is presented.     

Silver nanoparticles: Large scale solvothermal synthesis and optical properties

Silver nanoparticles have been successfully synthesized by a simple and modified solvothermal method at large scale using ethanol as the refluxing solvent and NaBH₄ as reducing agent. The nanopowder was investigated by means of X-ray diffraction (XRD), transmission electron microscopy (TEM), dynamic light scattering (DLS), UV-visible and BET surface area studies. XRD studies reveal the monophasic nature of these highly crystalline silver nanoparticles. Transmission electron microscopic studies show the monodisperse and highly uniform nanoparticles of silver of the particle size of 5 nm, however, the size is found to be 7 nm using dynamic light scattering which is in good agreement with the TEM and X-ray line broadening studies. The surface area was found to be 34.5 m²/g. UV-visible studies show the absorption band at ∼425 nm due to surface plasmon resonance. The percentage yield of silver nanoparticles was found to be as high as 98.5%.     

Surfactant controlled synthesis of crystalline phosphovanadate nanorods

Phosphovanadate nanorods were obtained in a reaction of vanadium (V) oxide as a precursor and a cationic surfactant, dodecylpyridinium chloride, as structure directing template at pH ∼3 at room temperature. The composition and morphology of the nanorods was established by powder X-ray diffraction (XRD), energy dispersive X-ray analysis (EDAX), fourier transform infra-red spectroscopy (FTIR), thermogravimetric analysis (TGA), transmission electron microscopy (TEM) and atomic force microscopy (AFM). The obtained nanorods have diameters of 40-60 nm with lengths up to 1 μm. The effect of reaction parameters such as concentration of surfactant and pH of the solution on the growth of nanorods has been investigated. A plausible mechanism involving the coalescence of nanoparticle ‘seeds’ leading to one-dimensional nanorods is also discussed. The same reaction when performed under hydrothermal condition, keeping other reaction parameters unchanged, resulted in the formation of phosphovanadate nanospheres of diameter 10-15 nm.     

Dopant induced variations in microstructure and optical properties of CeO2 nanoparticles

Nanocrystalline CeO₂ particles doped in the range of 0-20% of Ca²⁺, La³⁺, and Zr⁴⁺ have been prepared from hydrothermal synthesis of nitrate solutions at 200 °C and the influences of the dopants on microstructure and optical properties of the nanoparticles have been investigated. The unit cell parameter is found to be modified by −0.39, +0.83 and +0.16% for doping of 20% Zr⁴⁺, La³⁺, and Ca²⁺, respectively. For each batch prepared, nanoparticles with a narrow size distribution of 5-15 nm have been obtained. A high-resolution transmission electron microscopy investigation reveals that these particles are single crystals mostly having hexagonal, square or circular two-dimensional projections. UV-visible spectra of doped powders exhibit shift of the absorption edge and absorption peak with respect to those of the undoped CeO₂ particles and has been attributed to compensation of Ce³⁺ and decreasing crystallite size as result of doping.     

Investigation on one-pot hydrothermal synthesis,structural and optical properties of ZnS quantum dots

The advantage of hydrothermal synthesis of semiconductor quantum dots (QDs) over the control of particles size, morphology and stability is reported here. In a typical synthesis procedure, the zinc and sulfur precursor molar ratio of 1:3 was used in an aqueous solution at 150 °C. The cubic phase of ZnS with average particles size of 5 nm was confirmed and estimated from the X-ray diffraction (XRD) analysis. The composition and purity of the sample were analyzed from (energy dispersive-ray analysis) EDAX and (X-ray photoelectron spectroscopy analysis) XPS spectra. The absorption spectrum shows the large shift in the absorption band over 90 nm due to the quantum confinement of carriers. The emission spectrum of quantum dots carry more evidence on the presence of shallow trap, deep trap in the band gap of the material responsible for weak emission in the spectral region of 450–500 nm. High resolution transmission electron microscope and scanning electron microscope studies reveal the structural and morphological features of ZnS with slightly distorted spherical morphology. We found that the coordinating ability of solvent strongly influences the reaction process and morphology of the products.     

Thermal-treatment effect on the photoluminescence and gas-sensing properties of tungsten oxide nanowires

Single-crystalline non-stoichiometric tungsten oxide nanowires were initially prepared using a simple solvothermal method. High resolution transmission electron microscopy (HRTEM) investigations indicate that the tungsten oxide nanowires exhibit various crystal defects, including stacking faults, dislocations, and vacancies. A possible defect-induced mechanism was proposed to account for the temperature-dependent morphological evolution of the tungsten oxide nanowires under thermal processing. Due to the high specific surface areas and non-stoichiometric crystal structure, the original tungsten oxide nanowires were highly sensitive to ppm level ethanol at room temperature. Thermal treatment under dry air condition was found to deteriorate the selectivity of room-temperature tungsten oxide sensors, and 400 °C may be considered as the top temperature limit in sensor applications for the solvothermally-prepared nanowires. The photoluminescence (PL) characteristics of tungsten oxide nanowires were also strongly influenced by thermal treatment.     

Growth of PbS nanopyramidal particulate films for potential applications in quantum-dot photovoltaics and nanoantennas

We report a simple interfacial process called the liquid-liquid interface reaction technique (LLIRT) that leads to the formation of nanosized PbS particulate films with hitherto unreported pyramidal morphology. The resultant PbS films were characterized by transmission electron microscopy (TEM) with selected area electron diffraction (SAED), X-ray diffractometery (XRD), atomic force microscopy (AFM), near field scanning optical microscopy (NSOM) and UV-vis spectroscopy. The pyramidal morphology is speculated to originate from the preferred orientation of the 2 2 0 plane of cubic PbS. Our nanopyramidal PbS particulate films display remarkably sharp excitonic peak centered around 656 nm that accounts for a band gap of 1.8 eV suggesting, in turn, their potential application in QD photovoltaics. Interestingly, the feasibility of such nanopyramids to potentially act as nanoantennas (as revealed by the NSOM) is also suggested.     

A study on the structural and mechanical properties of nanocrystalline CuS thin films grown by chemical bath deposition technique

We report a chemical route for the deposition of nanocrystalline thin films of CuS, using aqueous solutions of Cu(CH₃COO)₂, SC(NH₂)₂ and N(CH₂CH₂OH)₃ [triethanolamine, i.e. TEA] in proper concentrations and ratios. The films were structurally characterized using X-ray diffraction technique (XRD), field emission scanning electron microscopy (FESEM) and optical analysis [both photo luminescence (PL) and ultraviolet-visible (UV-vis)]. Optical studies showed a large blue shift in the band gap energy of the films due to quantum confinement effect exerted by the nanocrystals. From both XRD and FESEM analyses, formation of CuS nanocrystals with sizes within 10-15 nm was evident. A study on the mechanical properties was carried out using nanoindentation and nanoscratch techniques, which showed good mechanical stability and high adherence of the films with the bottom substrate. Such study on the mechanical properties of the CuS thin films is being reported here for the first time. Current-voltage (I-V) measurements were also carried out for the films, which showed p-type conductivity.     

Preparation and characterization of indium doped CdS0.2Se0.8 thin films by spray pyrolysis

The CdS_0.2Se_0.8 and indium doped CdS_0.2Se_0.8 thin films have been deposited onto the amorphous glass and fluorine doped tin oxide coated glass substrates by spray pyrolysis. The doping concentration of indium has been optimized by photoelectrochemical characterization technique. The structural, surface morphological, optical and electrical properties of CdS_0.2Se_0.8 and indium doped CdS_0.2Se_0.8 thin films have been studied. X-ray diffraction studies reveal that the films are polycrystalline in nature with hexagonal crystal structure. Scanning electron microscopy studies reveal that the grains are uniform with uneven spherically shaped, distributed over the entire substrate surface. The complete surface morphology has been changed after doping. In optical studies, the transition of the deposited films is found to be direct allowed with optical energy gaps decreasing from 1.91 to 1.67 eV with indium doping. Semiconducting behavior has been observed from resistivity measurements. The thermoelectric power measurements reveal that the films exhibit n-type conductivity.     

Size tuning of MAA capped CdSe and CdSe/CdS quantum dots and their stability in different pH environments

The present work reports synthesis of mercaptoacetic acid capped CdSe nanoparticles soluble in water at different temperatures and with different precursor ratios. This enabled to tune the particle size of QDs from 2.7 to 5.8 nm. The particles consist of nanocrystals; with mixed phase, hexagonal wurtzite as well as sphalerite cubic and are luminescent with quantum yield 10%. The quantum yield up to 20% has been obtained by growing a shell of CdS over the CdSe. HR-TEM images, XRD patterns and the photoluminescence excitation spectra shows epitaxial growth of CdS shell over CdSe and with average size 3.2 ± 1.2 and 4.7 ± 1.2 nm for CdSe and CdSe/CdS quantum dots respectively. FT-IR spectrum and the negative zeta potential value together confirms the attachment of mercaptoacetic acid to the QD surface, where the carboxylic acid group is facing towards solvent and provides stability due to electrostatic hindrance. Further, the QDs are checked for their stability and the luminescence in environments of different pH (4–11 pH). Both CdSe and CdSe/CdS agglomerate with total elimination of fluorescence for 4 pH medium, and no shift in the fluorescence emission peak observed for the 6–9 pH, therefore QDs can be applicable as the fluorescence tags in this specific range of pH.     

Size-dependent optical and dielectric properties of nanocrystalline ZnS thin films synthesized via rf-magnetron sputtering technique

Nanocrystalline ZnS thin films have been synthesized by radio frequency magnetron sputtering technique on glass and Si substrates at a substrate temperature 300 K. X-ray diffraction and selected area electron diffraction studies confirmed the formation of nanocrystalline cubic phase of ZnS in the films, although the target material was hexagonal ZnS. The particle size, calculated from the XRD patterns of the thin films was found in the range 2.06-4.86 nm. TEM micrographs of the thin films revealed the manifestation of ZnS nanoparticles with sizes in the range 3.00-5.83 nm. UV-vis-NIR spectrophotometric measurements showed that the films were highly transparent (∼90%) in the wavelength range 400-2600 nm with a blue shift of the absorption edge. The direct allowed bandgaps have been calculated and they lie in the range 3.89-4.44 eV. The particle size, calculated from the shift of direct bandgap, due to quantum confinement effect lying in the range 3.23-5.60 nm, well support the TEM results. The room temperature photoluminescence spectra of the films showed two peaks centered around 315 and 450 nm. We assigned the first peak due to bandgap transitions while the latter was due to sulfur vacancy in the films. The composition analysis by energy dispersive X-rays also supported the existence of sulfur deficiency in the films. The dielectric property study showed high dielectric constant (85-100) at a higher frequency (>5 kHz).     

Synthesis of nanocrystalline iron oxide ultrathin films by thermal decomposition of iron nitropruside: Structural and optical properties

Ultrathin films of nanocrystalline α-Fe₂O₃ have been deposited on glass substrates from an inorganic precursor, iron nitropruside. This is a novel route of synthesis for iron oxide thin films on glass substrates, by annealing the precursor thin film in air at 650 °C for 15 min. The films were characterized using TG-DTA analysis, X-ray diffraction, UV-visible, FESEM, AFM and Raman measurements. X-ray diffraction and Raman analyses revealed that the deposited films contain α-phase of Fe₂O₃ (hematite). The synthetic route described here provides a very simple and cost-effective method to deposit α-Fe₂O₃ thin films on glass substrates with band gap energy of about 2.75 eV. The deposited films were found to show catalytic effect for the photo-degradation of phenol.     

Sonochemical synthesis of ZnO nanoparticles: The effect of temperature and sonication power

ZnO nanoparticles were synthesized by drop-wise addition of ZnCl₂ solution to KOH, in different temperatures and sonication output powers. The morphologies and structure of resulting materials were characterized by means of X-ray diffraction (XRD) and scanning electron microscopy (SEM). The morphology of the products was determined to be a mixture of nano rods as well as nanoparticles depending to sonication output power and temperature. A reduction in nanoparticles and aggregates sizes as well as amount of byproducts was observed by increasing the sonication output power. A combination of sonication output power and temperature was also studied on the properties of the product. At 70 °C and 45 W sonication output power, the smallest nanoparticles as well as narrower range of sizes in addition to minimum amount of byproducts was obtained in this work.     

Phase stabilization and microstructural studies of lead lanthanum titanate thin films

Thin ferroelectric films of PLTx (Pb_1−xLa_xTi_1−x/4O₃) have been prepared by a sol-gel spin coating process. As deposited films were thermally treated for crystallization and formation of perovskite structure. Characterization of these films by X-ray diffraction (XRD) have been carried out for various concentrations of La (x = 0.04, 0.08 and 0.12) on ITO coated corning glass substrates. For a better understanding of the crystallization mechanism, the investigations were carried out on films annealed at temperatures (350, 450, 550 and 650 °C). Characterization of these films by X-ray diffraction shows that the films annealed at 650 °C exhibit tetragonal phase with perovskite structure. Atomic force microscope (AFM) images are characterized by slight surface roughness with a uniform crack free, densely packed structure. Fourier transform infrared spectra (FTIR) studies of PLTx thin films (x = 0.08) deposited on Si substrates have been carried out to get more information about the phase stabilization.     

Hydrothermal routes to various controllable morphologies of nanostructural lithium aluminate

The α-LiAlO₂ powders have been successfully prepared by a hydrothermal route based on using the surfactant of heax-adecyltrimethyl ammonium bromide (CTAB) as the template. One-dimensional (1D) nanorods with higher and lower aspect ratio, 2D mesoporous microsheets were respectively observed with different concentration of the surfactants. A high specific surface area up to 151 m²/g was obtained by this method. The formation mechanism of the nanostructural lithium aluminate was proposed.     

Synthesis and characterization of Fe(III)-silicate precipitation tubes

Fe(III)-silicate precipitation tubes synthesized through “silica garden” route have been characterized using a number of analytical techniques including X-ray diffraction, infrared spectroscopy, atomic force microscopy, scanning and transmission electron microscopy. These tubes are brittle and amorphous and are hierarchically built from smaller tubes of 5-10 nm diameters. They remain amorphous at least up to 650 °C. Crystobalite and hematite are the major phases present in Fe(III)-silicate tubes heated at 850 °C. Morphology and chemical compositions at the external and internal walls of these tubes are remarkably different. These tubes are porous with high BET surface area of 291.2 m²/g. Fe(III)-silicate tubes contain significant amount of physically and chemically bound moisture. They show promise as an adsorbent for Pb(II), Zn(II), and Cr(III) in aqueous medium.     

Structural and optical characterizations of chemically deposited cadmium selenide thin films

Synthesis of cadmium selenide thin films by CBD method has been presented. The deposited film samples were subjected to XRD, SEM, UV-vis-NIR and TEP characterization. X-ray diffraction analysis showed that CdSe film sample crystallized in zinc blende or cubic phase structure. SEM studies reveal that the grains are spherical in shape and uniformly distributed all over the surface of the substrates. The optical band gap energy of as deposited film sample was found to be in the order of 1.8 eV. The electrical conductivity of the film sample was found to be 10⁻⁶ (Ω cm)⁻¹ with n-type of conduction mechanism.     

One-step synthesis of UV-induced Pt nanotrees on the surface of DNA network

Platinum metal nanotrees were prepared with assembling Pt nanoparticles onto DNA network template and reducing metal ions by photoinduced method. The concentration of DNA network and the reaction time play important roles in forming platinum nanotrees. The mechanism on the formation of the Pt nanotree is also discussed.