Facile synthesis of low dimensional CuO nanostructures and their gas sensing applications

A simple and cost effective hydrothermal method has been employed to synthesis morphology controlled pure and Cr doped (4 and 8 at. %) CuO nanostructures. Crystalline purity and structure of the nanostructures were validated by X‐ray diffraction and Retvield analyses. Field emission scanning electron microscopy revealed the evolution of rod‐like, sheet‐like and boat‐like morphologies for pure, 4 and 8 at. % Cr doped CuO nanostructures respectively. The optical band gap estimated using the K‐M function plot from diffused reflectance spectroscopy showed a shift in band gap from 1.68 to 1.90 eV with respect to Cr concentration. The synthesized CuO nanostructures were investigated for the efficient room temperature gas sensing of ammonia, ethanol and methanol vapours under different concentrations (100‐600 ppm). The 8 at. % Cr doped CuO nano‐boats showed enhanced gas sensitivity than other CuO nanostructures owing to their typical morphology, larger surface area and related properties.     

Facile electrochemical synthesis of tellurium nanorods and their photoconductive properties

Tellurium nanorods have been successfully fabricated by template and surfactant‐free electrochemical technique from an aqueous solution at room temperature. The as‐prepared tellurium nanorods were characterized by X‐ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectrometry, UV‐vis spectroscopy and photoluminescence spectroscopy. Films based on tellurium nanorods were constructed to study the photoresponse and I‐V curves. These photoresponse measurements demonstrate that tellurium nanorods exhibited enhanced conductivity under illumination compared to in the dark measurement.     

Synthesis and structural analysis of angled Te nanocrystals

In this paper, a new direct method to prepare angled Te nanocrystals (NCs) in the isotropic thiol‐ligand system from the transformation of MA‐stabilized CdTe nanoparticles (NPs) induced by the post‐addition of L‐cysteine was presented, without removing aforehand the protective shell of organic stabilizer. Besides nanorods, angled Te nanocrystals, including nanocheckmarks, X‐shaped, nanomoths, y‐shaped, and so on, also were obtained. By means of high‐resolution transmission electron microscopy (HRTEM), selected‐area electron diffraction (SAED) and powder X‐ray diffractometry (XRD), we further investigated intensively the internal crystal structure of angled Te NCs and the growth direction of the arms in this study. The experimental results obtained show that the preferential growth direction of either arms in nanocheckmarks is along the [001] direction of trigonal Te, and the corresponding contact plane should be (112) of hexagonal lattice. In the meantime, these results also confirm that L‐cysteine not only can be used as the stabilizer for the synthesis of aqueous CdTe NPs as reported previously, but also can act as a strong complexing agent like EDTA, inducing the decomposition of CdTe NPs, i.e. the transformation from CdTe NPs to Te nanocrystals. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Physical properties of Ag-doped cadmium telluride thin films fabricated by closed-space sublimation technique

Cadmium telluride (CdTe) thin films were prepared by the closed-space sublimation (CSS) technique, using CdTe powder as evaporant onto substrates of water-white glass. In the next step, the annealed films at 450 °C for 30 min were dipped in AgNO₃–H₂O solution at room temperature. These films were again annealed at 450 °C for 1 h to obtain silver-doped samples. The samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), electrically i.e. DC electrical resistivity as well as photo resistivity by van der Pauw method at room temperature, dark conductivity, activation energy analysis as a function of temperature by two-probe method under vacuum, and spectrophotometry. The electron microprobe analyzer (EMPA) results showed an increase of Ag content composition in the samples by increasing the immersion time of films in solution. The Hall measurements indicated the increase in mobility and carrier concentrations of CdTe films by doping of Ag. A significant change in the shape and size of the CdTe grains were observed.     

Effect of growth temperature on the structure and optical properties of ZnO nanorod arrays grown on ITO substrate

ZnO nanorod arrays have been successfully prepared on ITO substrate by a chemical‐bath deposition method at different growth temperatures. The influence of the growth temperature on the morphology and microstructure of the ZnO nanorods was investigated by scanning electron microscopy (SEM) and X‐ray diffraction (XRD). The results showed that the diameter of the ZnO nanorods decreased and the size of the nanocrystals increased with increasing growth temperature. Optical absorption measurements showed the absorption band edge has shifted to a lower‐energy region due to the quantum size effect. Green emission and UV emission bands were observed and they are found to be temperature dependent, which indicates that the deep‐level emission and band‐edge emission of ZnO nanorods is closely related to the rod diameter, and the related mechanism is discussed.     

Photostimulated changes of properties of CdTe films

The effect of illumination during the close‐spaced sublimation (CSS) growth on composition, structural, electrical, optical and photovoltaic properties of CdTe films and CdTe/CdS solar cells were investigated. Data on comparative study by using X‐ray diffraction (XRD), scanning electron microscopy (SEM), absorption spectra and conductivity‐temperature measurements of CdTe films prepared by CSS method in dark (CSSD) and under illumination (CSSI) were presented. It is shown that the growth rate and the grain size of CdTe films grown under illumination is higher (by factor about of 1.5 and 3 respectively) than those for films prepared without illumination. The energy band gap of CdTe films fabricated by both technology, determined from absorption spectra, is same (about of 1.50 eV), however conductivity of the CdTe films produced by CSSI is considerably greater (by factor of 10⁷) than that of films prepared by CSSD. The photovoltaic parameters of pCdTe/nCdS solar cells fabricated by photostimulated CSSI technology (J_sc = 28 mA/cm², V_oc =0.63 V) are considerably larger than those for cells prepared by CSSD method (J_sc = 22 mA/cm², V_oc = 0.52 V). A mechanism of photostimulated changes of properties of CdTe films and improvement of photovoltaic parameters of CdTe/CdS solar cells is suggested. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and spectrum stability of high quality CdTe quantum dots capped with stearate groups in N-oleoylmorpholine solvent

The stearate-capped CdTe quantum dots (QDs) have been first prepared via direct reaction of cadmium stearate with Te powder in N-oleoylmorpholine solvent, which was a kind of clean, air-stable and conveniently synthesized acylamide, and can readily dissolve precursors cadmium stearate and Te powder at a relative low temperature. The as-prepared CdTe QDs exhibited size-dependent optical properties, steep absorbance edge and narrow photoluminescence full width at half maximum. The high-resolution transmission electron microscopy images and X-ray diffraction revealed that the highly monodisperse CdTe QDs were of regular spherical morphology with zinc blende crystal structure displaying mean sizes of about 4 nm. The energy dispersed spectrometry measurement indicated the presence of Cd and Te, with the Cd:Te ratio being close to 1:1. Fourier transform infrared transmission spectra confirmed the existence of stearate on the CdTe QDs surfaces. The experimental results also demonstrated that the stearate-capped CdTe QDs had an unexpected good stability.     

Controllable one‐step synthesis of CuO,Cu2O and Cu

In the present report, CuO, Cu₂O and Cu have been successfully synthesized through a facile, one‐step hydrothermal method at a relative low temperature by controlling only the concentration of citric acid. Compared with other synthetic methods, the present method is mild, high‐efficient and nontoxic. The crystal structure and morphology of the as prepared samples were characterized by X‐ray diffraction and scanning electron microscopy, respectively. The mechanism for the crystal phase and morphological changes with different citric acid concentrations were discussed. The possible reaction process of the synthesis was also studied on the basis of the experimental results. We hope that this facile, one‐step hydrothermal method could be used in controlling synthesis of other metals and metal oxides under appropriate experimental conditions.     

Hydrothermal synthesis of nano‐crystalline BaMoO4 under mild conditions using simple additive

Large‐scale high‐quality BaMoO₄ nanocrystals have been synthesized in aqueous solutions under mild conditions with citrate as a simple additive. The crystals have bone‐like, spindle‐like and wheatear‐like morphologies assembled from nanoparticles, nanofibers and have been characterized by X‐ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM) techniques. The results showed that experimental parameters had great influences on the shape evolution of products. The adjustment of these parameters such as room temperature stirring time, reaction temperature and reaction time of hydrothermal reaction, can lead to obvious morphology changes of products, and the growth mechanism has been proposed. Room‐temperature photoluminescence indicated that the as‐prepared BaMoO₄ nanocrystals had a strong blue emission peak at 481.5 nm. This facile route could be employed to synthesize more promising nanomaterials with interesting self‐assembly structures. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Vapor growth of CdTe laser window materials

Vapor deposition of CdTe from elemental cadmium and tellurium sources was studied as a function of the Cd/Te ratio, the supersaturation and the substrate temperature, in order to achieve optimum growth conditions for CdTe windows with low optical absorptivity in the infrared. A multisubstrate arrangement was designed to enable acquisition of growth data simultaneously on up to six specimens, each exposed to different growth conditions. Polycrystalline blanks up to 15 cm² × 2 mm thick were grown at rates of 0.02-1.5 mm/h with the growth rate exhibiting sensitivity to all of the above variables. Our results show that stoichiometry (as well as free carrier concentrations) can be controlled by adjustments in the Cd/Te ratio and/or the substrate temperature. Similarly, microstructural aspects (e.g., grain and void size) are shown to exhibit strong sensitivity to variations in growth conditions.     

Influence of temperature on the microcrystalline structure of thermally evaporated Sb2S3 thin films

Thin films of antimony trisulfide (Sb₂S₃) were prepared by thermal evaporation under vacuum (p=5×10^–5 torr) on glass substrates maintained at various temperatures between 293 K and 523 K. Their microstructural properties have obtained by transmission electron microscopy (TEM). The electron diffraction analysis showed the occurrence of amorphous to polycrystalline transition in the films deposited at higher temperature of substrates (523 K). The polycrystalline thin films were found to have an orthorhombic structure. The interplanar distances and unit‐cell parameters were determined by high‐resolution transmission electron microscopy (HRTEM) and compared with the standard values for Sb₂S₃. The surface morphology of Sb₂S₃ thin films was investigated by scanning electron microscopy (SEM). The optical transmission spectra at normal incidence of Sb₂S₃ thin films have been measured in the spectral range of 400–1400 nm. The analysis of the absorption spectra revealed indirect energy gaps, characterizing of amorphous films, while the polycrystalline films exhibited direct energy gap. From the photon energy dependence of absorption coefficient, the optical band gap energy, E_g, were calculated for each thin films. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis of nanoflakes‐based self‐assembling crossed structure of stannous oxide and photocatalysis property

Self‐assembling nanoflakes‐based crossed architectures of stannous oxide (SnO) were successfully synthesized via template‐free hydrothermal growth method by using SnCl₂·2H₂O and KOH as precursors. Crystal structures, morphology, chemical composition and optical properties were examined by X‐ray diffraction (XRD), field‐emission scanning electron microscopy (FESEM), energy dispersive X‐ray analysis, and Raman spectroscopy, respectively. The results indicate that the as‐synthesized product belongs to tetragonal phase SnO with crossed morphology self‐assembled by nanoflakes. Furthermore, UV‐vis spectrophotometry was used to determine optical band gap of the SnO nanostructures and the direct band gap of 2.90 eV was obtained. The photocatalysis of the product has been evaluated with methyl orange and the high degradation ratio of 87% is obtained in 240 minutes under the measuring condition which is attributed to the wide band gap and large specific surface area of the nanoflakes‐based crossed SnO architectures. A possible growth mechanism is proposed in the end.     

Facile synthesis and characterization of hierarchical CuO nanoarchitectures by a simple solution route

The controlled synthesis of hierarchical CuO nanomaterials in a solution phase has been realized with high yield at low temperature using copper acetate hydrate and NaOH as starting materials with the assistance of surfactant under hydrothermal conditions. X‐ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and ultraviolet‐visible spectroscopy (UV‐Vis) were used to characterize the products. It was shown that the hierarchical CuO nanoarchitectures were formed through aggregation of tiny single‐crystal CuO nanorods. Experiments demonstrated that the morphology of CuO products was significantly influenced by hydrothermal temperature and reaction time. A rational growth mechanism based on oriented attachment was proposed for the selective formation of the hierarchical CuO nanoarchitectures. Our work demonstrated the growth of hierarchical CuO nanoarchitectures built from one‐dimentional nanorods through a one‐step solution‐phase chemical route under controlled conditions. In addition, The UV‐Vis spectrum of the hierarchical CuO nanoarchitectures showed large blue shift because of the quantum size effect. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Study of the structural and photoluminescence properties of CdTe polycrystalline films deposited by close-spaced vacuum sublimation

The polycrystalline CdTe films were deposited by the close-spaced vacuum evaporation at the different substrate temperatures (150–550 °C). The X-ray diffraction measurements of structural and substructural properties of these films were carried out to study their phase composition and texture. The films’ parameters such as the coherent scattering domain size, microdeformation level and mean density of dislocations were determined based on the broadening of diffraction peaks. In this case the Hall and three-fold convolution approximations were used. Surface morphology, grain size and growth mechanism of the films were determined by the scanning electron microscopy. The low temperature photoluminescence measurements allowed us to establish the correlation between the point and extended defect structure on the one hand and the growth conditions on the other. As a result, the growth conditions of CdTe polycrystalline films with fairly good crystal and optical quality were determined.     

Optical properties of the complex perovskite ceramic oxide Ba2YZrO6‐d

Nanocrystalline Ba₂YZrO_6‐dhas been successfully synthesized through a single step auto‐ignition combustion route. The samples were analyzed by powder X‐ray diffraction, transmission electron microscopy and Ultraviolet‐Visible spectroscopy. The XRD analysis revealed that the material has an ordered complex cubic perovskite structure. The basic optical properties and optical constants of the as‐prepared nanopowder of Ba₂YZrO_6‐dhave been reported for the first time. The spectral analysis revealed that the material is a wide band gap direct transition semiconductor with band gap of 3.70 eV at room temperature. The poor transmittance in ultraviolet but good transmittance in visible‐near infrared regions make the material potentially important for poultry protection and warming coatings, solar control, antireflection coatings and window layer in solar cells. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

High yield synthesis and characterization of well-ordered Mesoporous silica nanoparticles using Sodium Carboxy Methyl Cellulose

In the present work, mesoporous silica nanoparticles (MSNs) with well-ordered hexagonal structure were synthesized using Sodium Carboxy Methyl Cellulose. The MSNs were characterized by scanning electron microscopy, dynamic light scattering, powder XRD, nitrogen physisorption and Transmission electron microscopy. The MSNs were also functionalized with thiol groups and its capacity toward adsorption of a large cation, i.e. lead was investigated. Scanning electron microscopy reveals that MSNs have semi-spherical shapes. The XRD pattern of the calcined sample shows at least five well-defined peaks which point out that silicate nanoparticles have hexagonal array of pores as MCM-41 structure. The nitrogen adsorption isotherm displays a type IV isotherm according to the IUPAC classification. A sharp inflection in capillary condensation/evaporation step specifies that well-ordered MCM-41 nanoparticles were synthesized. TEM image shows the well-ordered hexagonal structure of MSNs. The adsorption capacity of functionalized MSNs was higher than functionalized MCM-41 in which one reason for such behavior might be explained by higher accessibility of pores of functionalized MSNs. This approach was carried out using relatively low-cost and nonhazardous reactants in concentrated reaction medium and also the yield of this approach was high up to 96% by weight.     

Dependence of photoluminescence properties on excitation power in ZnO and ZnCdO microrods

ZnO and ZnCdO microrods have been prepared through a chemical bath deposition method. The structure of microrods has been characterized using X‐ray diffraction (XRD) and transmission electron microscopy (TEM). Photoluminescence spectra were recorded for ZnO and ZnCdO microrods at different excitation powers. The intensity of UV emission is enhanced with increasing excitation power. The width of UV emission increases for spectra at higher excitation powers. In particular, the paper shows that the influence of excitation power on the shift of emission band for ZnCdO microrods is more remarkable than that of ZnO microrods with the increase of excitation power. The definite experimental evidence demonstrated that the temperature coefficient β of ZnCdO microrods is much larger than the temperature coefficient of ZnO microrods. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Substrate temperature effect on the optical properties of amorphous Sb2S3 thin films

Sb₂S₃ amorphous thin films were prepared by thermal evaporation of corresponding powder on thoroughly cleaned glass substrates held at temperature in the range 300‐473 K. X‐ray diffraction and atomic force microscopy have been used to order to identify the structure and morphology of surface thin films. The optical constants of the deposition films were obtained from the analysis of the experimental recorded transmission data over the wavelength range 400‐1400 nm. An analysis of the absorption coefficient values revealed an optical indirect transition with the estimation of the corresponding band gap values. It was found that the optical band gap energy decrease with substrate temperature from 1.67 eV at 300 K to 1.48 eV at 473K. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Microstructure of high-temperature plastically deformed Zn-doped CdTe; comparison with In-doped GaAs

We investigated the microstructure of CdTe and Cd_0.96Zn_0.04Te samples plastically deformed by uniaxial compression at constant strain rate between 0.6T_m and 0.85T_m (where T_m is the melting temperature, 1365 K). We used scanning electron microscopy (SEM) in the cathodoluminescence (CL) mode to observe dislocation arrangements and transmission electron microscopy (TEM) to measure dislocation dissociation widths. These results are compared to those reported for In doped GaAs, as well as results concerning high temperature plastic deformation of both types of materials. In both cases, isoelectronic doping strongly increases yield stresses and hardening rates. A cell structure appears for larger stresses and strains. The increase of dissociation width in Ga_0.99In_0.01As with respect to GaAs was not observed in Cd_0.96Zn_0.04Te compared to CdTe. On the basis of macroscopic and microscopic studies, a better understanding of the hindering by doping of dislocation multiplication during crystal growth is possible. The involved mechanisms can reduce the as-grown dislocation density in CdTe and GaAs.     

X-Ray Diffraction Studies on Point Defects in II–VI Compounds

The point defect concentration in Te-rich CdTe and Hg_1-xCd_xTe annealed at various temperatures has been estimated from precision lattice parameters using a simple continuum inclusion model and compared with densities of electrically charged defects determined by high-temperature Hall and conductivity measurements. The nonstoichiometry is realized by cation vacancies. Dependent on the CdTe content, the ratio of total to charged defect concentrations varies between about unity for HgTe-rich composition and 75 for CdTe. Therefore, it is necessary to distinct between “electrical” and “chemical” stability regions.