Growth of CuInTe2 single crystals by iodine transport and their characterization

The single crystals with stoichiometry close to 1:1:2 of CuInTe₂ (CIT) have been grown by chemical vapor transport (CVT) technique using iodine as the transporting agent at different growth temperatures. Single crystal X-ray diffraction studies have confirmed the chalcopyrite structure for the grown crystals and the volume of unit cell is found to be the same for the crystals grown at different conditions. Energy dispersive X-ray (EDAX) analysis of CIT single crystals grown shows almost the same stoichiometric compositions. Scanning electron microscope (SEM) analysis reveals kink, step and layer patterns on the surface of CIT single crystals depending on the growth temperatures. The optical absorption spectra of as-grown CIT single crystals grown at different conditions show that they have same band gap energies (1.0405 eV). Raman spectra exhibit a high intensity peak of A₁ mode at 123 cm^?1. Annealed at 473 K in nitrogen atmosphere for 40 h CIT single crystals have higher hole mobility (105.6 cm²V^?1s^?1₎ and hole concentration (23.28 × 10¹⁷ cm^?3) compared with values of hole mobility (63.69 cm² V^?1 s^?1) and hole concentration (6.99 × 10¹⁵ cm^?3) of the as-grown CIT single crystals.     

Trypsin immobilization on discs of polyvinyl alcohol glutaraldehyde/polyaniline composite

Discs of polyvinyl alcohol cross-linked with glutaraldehyde (PVAG) were synthesized and covered with polyaniline activated with glutaraldehyde (PANIG). Trypsin was covalently immobilized on this composite yielding a preparation containing 21.1 units per disc. The FT-IR spectra of the discs showed bands of PVA (3300 cm^?1, 2930 cm^?1 and 1440 cm^?1) and PANI (1594 cm^?1 and 1100 cm^?1). The best immobilization conditions were: trypsin concentration at 0.2 mg mL^?1, pH 7.6 and 60 min of incubation, similar to polyaniline–trypsin systems reported in the literature. The PVAG–PANIG–trypsin derivative showed an optimal pH and an optimal temperature of 7.0 and 35 °C, respectively. Hydrolysis of casein showed variations in the size of the products, revealing differences between the immobilized enzyme and the mechanism catalyzed by the native enzyme.     

A facile low temperature hydrothermal route to CdSO4 nanotubes/rods

Cadmium sulphate nanotubes/rods have been synthesized by hydrothermal treatment using CdSO₄ powder as precursor and hexadecylamine (HDA) as surfactant at 180 °C for 7 days. The powder X-ray diffraction (PXRD) pattern reveals that the CdSO₄ nanotubes/rods are of orthorhombic phase. Fourier transform infrared (FTIR) spectrum shows characteristic bands due to the sulfate ion in 1114 cm^? 1 and 617 cm^? 1 region, besides bands due to the amine moiety. Transmission electron micrograph (TEM) images reveal the nanorods are of 10–15 nm in thickness and nanotubes of wall thickness 5–8 nm. UV–visible absorption spectrum of CdSO₄ nanotubes/rods shows the peak at 221 nm. Photoluminescence (PL) spectrum exhibits an intense UV band at 372 nm and weak green band at 484 nm.     

Synthesis,characterization and cation adsorption of p-aminobenzoic acid intercalated on calcium phosphate

Crystalline lamellar calcium phosphate retained 4-aminobenzoic acid inside its cavity without leaching. The intense infrared bands in the 1033 and 1010 cm^?1 interval confirmed the presence of the phosphonate groups attached to the inorganic layer, with sharp and intense peaks in X-ray diffraction patterns, which gave basal distances of 712 and 1578 pm for the original and the intercalated compounds, respectively. Solid-state ³¹P nuclear magnetic resonance spectra presented only one peak for the phosphate groups attached to the main inorganic polymeric structure near ?2.4 ppm. The adsorption isotherms from ethanol gave the maximum adsorption capacities of 6.44 and 3.34 mmol g^?1 for nickel and cobalt, respectively, which stability constant and distribution coefficient followed Co > Ni.     

Characterization of sodium dodecyl sulfate modified iron pillared montmorillonite and its application for the removal of aqueous Cu(II) and Co(II)

Anionic surfactant modified Fe-pillared montmorillonites were prepared by Fe-hydrate solution and sodium dodecyl sulfate (SDS) solution. These organo–inorgano complex montmorillonites were divided into three types (CM1, CM2 and CM3) depending on different intercalation processes. X-ray diffraction spectra, the Fourier transform infrared (FTIR) spectra were used to analyze the structure of the raw and modified montmorillonites. X-ray photoelectron spectra of the simples have been studied to determine spectral characteristics to allow the identification of Fe(III) hydroxide. The specific surface area of the host montmorillonite (M0) is 73.2 m²/g, while for the modified montmorillonites it is 114.0 m²/g, 117.2 m²/g, and 115.8 m²/g, respectively. The mesopore volumes of the montmorillonites decrease after modification. Ions of copper and cobalt were selected as adsorbates to evaluate the adsorption performance of each montmorillonite. The adsorption data was analyzed by both Freundlich and Langmuir isotherm models and the data was well fit by the Langmuir isotherm model. The adsorption was efficient and significantly influenced by metal speciation, metal concentration, contact time, and pH. Higher adsorption capacity of the modified montmorillonites were obtained at pH 5–6. The results of desorption indicated that the metal ions were covalently bound to the modified montmorillonites.     

Tungsten-doped tin oxide thin films prepared by pulsed plasma deposition

Transparent conductive oxide tungsten-doped tin oxide thin films were deposited on glass substrates from ceramic targets by the pulsed plasma deposition method. The structural, electrical and optical properties have been investigated as functions of tungsten doping content and oxygen partial pressure. The lowest resistivity of 2.1 × 10^? 3 Ω?cm was reproducibly obtained, with carrier mobility of 30 cm²V^? 1s^? 1 and carrier concentration of 9.6 × 10¹⁹ cm^? 3 at the oxygen partial pressure of 1.8 Pa. The average optical transmission was in excess of 80% in the visible region from 400 to 700 nm, with the optical band gap ranging from 3.91 to 4.02 eV.     

FTIR and ellipsometry characterization of ultra-thin ALD TaN films

In this paper, Fourier-transform infrared (FTIR) spectroscopy and ellipsometric spectroscopy were used to characterize the optical properties of atomic layer-deposited (ALD) ultra-thin TaN films on a Si(1 0 0) single crystal. The analysis of FTIR spectra indicates that the incorporated impurities are in the form of radicals of NH_x, CH_x and OH_x. SiH_x is also detected due to interfacial reactions between NH_x and the Si substrate native oxide. These H-containing radicals can be removed by post-annealing the samples. The vibration of Ta–N bonding is at the wavenumber of 1190 cm⁻¹, which is independent of the film thickness and post-annealing temperature. The results of ellipsometric spectra show that the band gaps are 3.28 eV, 2.65 eV and 2.50 eV as the films thicknesses are 1 nm, 5 nm and 10 nm, respectively. A slight red-shift of the band gap takes place after annealing the ultra-thin films. The mechanisms of the film optical properties were analyzed in the paper.     

Evolution characteristic of OH absorption in Mg (5 mol% in melt):LiNbO3 crystal with post-grown Li-poor vapor transport equilibration

We have measured OH absorption spectra of a 0.47-mm-thick Z-cut MgO (5 mol% in melt):LiNbO₃ crystal subjected to post-growth Li-poor vapor transport equilibration (VTE) treatments at 1100 °C for different durations ranging from zero to 395 h. These spectra allow the evolution of OH absorption characteristics with prolonged VTE to be followed. After 2 h of VTE process an additional absorption appears at 3483 cm^? 1. A transition regime that the original 3536 cm^? 1 and new 3483 cm^? 1 absorptions simultaneously appear exists within the VTE duration range of 2–16 h. In this regime, the 3536 cm^? 1 absorption becomes weak gradually and eventually disappears around 16 h while the 3483 cm^? 1 absorption increases remarkably with the prolonged VTE. The presence of transition regime gives a hint that the 3483 cm^? 1 absorption is due to the VTE-induced formation of a new center. Based upon the spectral features, we have suggested a simple three-layer (two on surface and one in the center of crystal plate) model to describe the depth profile of the photorefractive damage MgO concentration threshold in the crystal in the transition regime. A Li out-diffusion theory is suggested and correlated with the model. To support the Li out-diffusion theory, some additional experiments have been done. These include the depth profile characterization of VTE-induced Li₂O content reduction and the measurement of the surface Li₂O content as a function of the VTE duration. A quantitative analysis and discussion shows that the model is well supported by the experimental results.     

Photoluminescence and thermoluminescence studies of Tb3+ doped ZnO nanorods

Here in, the synthesis of the terbium doped zinc oxide (ZnO:Tb³⁺) nanorods via room temperature chemical co-precipitation was explored and their structural, photoluminescence (PL) and thermoluminescence (TL) studies were investigated in detail. The present samples were found to have pure hexagonal wurtzite crystal structure. The as obtained samples were broadly composed of nanoflakes while the highly crystalline nanorods have been formed due to low temperature annealing of the as synthesized samples. The diameters of the nanoflakes are found to be in the range 50–60 nm whereas the nanorods have diameter 60–90 nm and length 700–900 nm. FTIR study shows ZnO stretching band at 475 cm^?1 showing improved crystal quality with annealing. The bands at 1545 and 1431 cm^?1 are attributed to asymmetric and symmetric CO stretching vibration modes. The diffuse reflectance spectra show band edge emission near 390 nm and a blue shift of the absorption edge with higher concentration of Tb doping. The PL spectra of the Tb³⁺-doped sample exhibited bright bluish green and green emissions at 490 nm (⁵D₄ → ⁷F₆) and 544 nm (⁵D₄ → ⁷F₅) respectively which is much more intense then the blue (450 nm), bluish green (472 nm) and broad green emission (532 nm) for the undoped sample. An efficient energy transfer process from ZnO host to Tb³⁺ is observed in PL emission and excitation spectra of Tb³⁺-doped ZnO ions. The doped sample exhibits a strong TL glow peak at 255 °C compared to the prominent glow peak at 190 °C for the undoped sample. The higher temperature peaks are found to obey first order kinetics whereas the lower temperature peaks obey 2nd order kinetics. The glow peak at 255 °C for the Tb³⁺ doped sample has an activation energy 0.98 eV and frequency factor 2.77 × 10⁸ s^?1.     

Formation of F-doped ZnO transparent conductive films by sputtering of ZnF2

Fluorine-doped ZnO transparent conductive thin films were successfully deposited on glass substrate by radio frequency magnetron sputtering of ZnF₂. The effects of rapid thermal annealing in vacuum on the optical and electrical properties of fluorine-doped ZnO thin films have been investigated. X-ray diffraction spectra indicate that no fluorine compounds, such as ZnF₂, except ZnO were observed. The specimen annealed at 500 °C has the lowest resistivity of 6.65 × 10^? 4 Ω cm, the highest carrier concentration of 1.95 × 10²¹ cm^? 3, and the highest energy band gap of 3.46 eV. The average transmittance in the visible region of the F-doped ZnO thin films as-deposited and annealed is over 90%.     

Hexadecylpyridinium surfactant modified zeolite A as an active component of a polymeric membrane sulfite selective electrode

Zeolite A was synthesized from waste porcelain and modified by hexadecylpyridinium surfactant to change the cation exchanger property of the raw zeolite to anion exchanger property in the obtained surfactant modified zeolite (SMZ). The SMZ was used as an active ingredient component of a membrane selective sulfite electrode. The electrode was fully characterized in terms of composition, response time, thermal stability and usable pH range. The sensor showed suitable response to sulfite in the concentration range of 8.0 × 10^? 7 to 1.0 × 10^? 1 mol L^? 1, with a detection limit of 5.0 × 10^? 7 mol L^? 1 and a slope of ? 29.5 ± 0.8 mV per decade of sulfite concentration.     

Hydrothermal synthesis of mesoporous VO2·½(H2O) nanosheets and study of their electrical properties

Layered sheet-like nanocrystalline VO₂·½(H₂O) has been synthesized by hydrothermal process using V₂O₅ as vanadium source and 2-phenylethylamine as a reducing agent and a structure-directing template. Techniques X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR) and nitrogen adsorption/desorption isotherms have been used to characterize the structure, morphology and composition of the materials. Electrical conductivity measurements showed that the as synthesized VO₂·½(H₂O) nanosheets has a conductivity value which goes from 75 × 10^?6 Ω^?1 cm^?1 at 298 K, to 68 10^?5 Ω^?1 cm^?1 at 386 K with activation energy of 0.24 eV.     

Hydrothermal synthesis,characterization and electrical investigation of poly(para-phenylenediamine)/vanadium oxide nanocomposite nanosheets

Sheet-like mesoporous poly(paraphenylenediamine)/vanadium oxide nanocomposite has been synthesized by the hydrothermal process using the vanadium oxide V₂O₅ as inorganic precursor and paraphenylendiamine as reducing and a structure-directing agent. Such techniques as X-ray diffraction (XRD), scanning electron microscopy (SEM), thermal analysis (TG-DTA), Fourier transform infrared spectroscopy (FTIR), Raman Spectroscopy, X-ray photoelectron spectroscopy (XPS) and nitrogen adsorption/desorption isotherms (BET) have been used to characterize the structure, morphology and the texture of the material. The conductivity of the material was measured by complex impedance spectroscopy which increases from 72 × 10^?5 Ω^?1 cm^?1 at 298 K to 95 × 10^?4 Ω^?1 cm^?1 at 493 K. The Arrhenius diagram is not linear, it presents a rupture situated at 407 K and the activation energies’ average values are 0.044 eV and 0.13 eV.     

Extremely high surface area of ordered mesoporous MCM-41 by atrane route

Silatrane synthesized from inexpensive oxide precursor, silica and TEA was used as the precursor for MCM-41 synthesis at low temperature because of its stability in aqueous solutions. Using cationic surfactant hexadecyltrimethyl ammonium bromide (CTAB) as a template, the resulting meso-structure mimics the liquid crystal phase. Varying the surfactant concentration, ion concentration and temperature of the system, changes the structure of the liquid crystal phase, resulting in different pore structures and surface area. After heat treatment, very high surface area mesoporous silica was obtained and characterized using XRD, BET and TEM. XRD and TEM results show a clear picture of hexagonal structure. The surface area is extraordinarily high, up to more than 2400 m² g⁻¹ at a pore volume of 1.29 cm³ g⁻¹. However, the pore volume is up to 1.72 cm³ g⁻¹ when the surface area is greater than 2100 m² g⁻¹.     

Synthesis of carbon nano-fibers on p-Si having improved temperature sensing capability

Synthesis of an innovative material for temperature sensor based on carbon nano-fibers (CNFs) on p-Si substrates has been demonstrated. The CNF films were characterized by SEM, Raman and FTIR studies. First order Raman spectra indicated a G band at ～1597 cm^?1 corresponding to the E_2g tangential stretching mode of an ordered graphitic structure with sp² hybridization and a D band located ～1350 cm^?1 originated from disordered carbon. Gold fingers were deposited on the p-Si/CNF surface for resistance measurement. Temperature sensing properties were also investigated critically. Resistance changes with temperature (ΔR/R) in p-Si/CNF films are found to be significantly large 30–60% Very stable, reproducible and improved temperature sensing properties would make this material superior to commonly available temperature sensors.     

Electrical properties and deep traps spectra of a-plane GaN films grown on r-plane sapphire

Electrical properties, deep traps spectra and luminescence spectra were studied for two undoped a-plane GaN (a-GaN) films grown on r-plane sapphire using metalorganic chemical vapor deposition and differing by structural perfection. For sample A, the a-GaN film was directly deposited on AlN buffer. A two-step growth scheme was implemented for sample B, including an initial islanding growth stage and a subsequent enhanced lateral growth. Preliminary detailed X-ray analysis showed that the stacking faults density was 8 × 10⁵ cm^?1 for sample A and 1.7 × 10⁵ cm^?1 for sample B. Electrical properties of a-GaN films were largely determined by deep traps with a level near E_c ?0.6 eV, with other prominent traps having the activation energy of 0.25 eV. The Fermi level was pinned by the E_c ?0.6 eV deep traps for sample A, but shifted to the vicinity of the shallower 0.25 eV traps for sample B, most likely due to the reduced density of the 0.6 eV traps. This decrease of deep traps density is accompanied by a very pronounced improvement in the overall luminescence intensity. A correlation of the observed improvement in deep traps spectra and luminescence efficiency with the improved crystalline quality of the films is discussed.     

Pb(Zr0.52Ti0.48)O3 nanotubes synthesis and infrared absorption properties

Herein a useful methodology to synthesize the lead zirconate titanate (PZT) nanotubes via a dip-coating deposition process with anodic aluminum oxide (AAO) template is proposed. The nano-porous AAO templates were produced using a controlled two-step electrochemical anodization technique. The PZT/AAO composite was formed using the dip-coating wetting technique. The prepared PZT precursor solution was driven into the nanopore channels of AAO template under the driving force of capillary action, subsequently the sintering process of the as-filled templates was carefully tuned to obtain Pb(Zr_0.52Ti_0.48)O₃ nanotubes of crystalline tetragonal phase with uniform pore size and ordered arrange. Fourier transform infrared spectroscopy (FTIR) results show that in the 1200–1900 cm⁻¹ band, the composite structure of PZT/AAO has obvious absorption peaks at 1471.56 cm⁻¹ and 1556.09 cm⁻¹, the absorption intensity of the composite structure is about six times of pure AAO template. The unusual optical properties found in PZT/AAO composite will stimulate further theoretical and experimental interests in ferroelectric nanostructures.     

Preparation and characterization of organo-montmorillonites. Application in adsorption of the 2,4,5-trichlorophenol from aqueous solution

X-ray diffraction has been used to study the changes in the surface properties of montmorillonitic clay through the changes in the basal spacings of sodium-montmorillonite (NaMt), acid-activated montmorillonite (AMt), pillared-montmorillonite (AlMt) and surfactant-intercalated organoclays. The basal spacing value of the NaMt increased from 12.01 to 18.1 Å by pillaring with Keggin ions ((hydroxyaluminum polycation) and until 21 Å by intercalation of the cationic surfactant in the interlayer space of the clay. Confirmations of the intercalated cationic surfactant have been characterized using Fourier transform infrared spectroscopy (FTIR). Thermogravimetric analysis shows that the thermal decomposition of montmorillonites modified with the cationic surfactant hexadecyltrimethylammonium (HDTMA) takes place in four steps. The surface areas of organo-montmorillonites were found to be much lower than that of raw montmorillonite. Surface areas of pillared and acid-activated montmorillonite are very high. This was explained by the emergence of the micropores and mesopores in the structure of the sample resulting from treatment. Adsorption of the 2,4,5-trichlorophenol (2,4,5-TCP) onto samples was studied. The greatest value of adsorption capacity of samples is attributed to the organo-montmorillonite (MtC16).     

Anomalous activation of shallow B+ implants in Ge

The electrical activation of B⁺ implantation at 2 keV to doses of 5.0 × 10¹³–5.0 × 10¹⁵ cm^?2 in crystalline and pre-amorphized Ge following annealing at 400 °C for 1.0 h was studied using micro Hall effect measurements. Preamorphization improved activation for all samples with the samples implanted to a dose of 5.0 × 10¹⁵ cm^?2 displaying an estimated maximum active B concentration of 4.0 × 10²⁰ cm^?3 as compared to 2.0 × 10²⁰ cm^?3 for the crystalline sample. However, incomplete activation was observed for all samples across the investigated dose range. For the sample implanted to a dose of 5.0 × 10¹³ cm^?2, activation values were 7% and 30%, for c-Ge and PA-Ge, respectively. The results suggest the presence of an anomalous clustering phenomenon of shallow B⁺ implants in Ge.     

Zinc incorporation into CdTe quantum dots in glass

We report zinc incorporation into CdTe nanoparticles grown by two-step solid phase precipitation in commercial borosilicate glass quenched from the melt, based on a co-evaluation of the results of resonant Raman and optical absorption measurements. Resonant Raman spectra display a two-peak structure at wave-number positions corresponding to ternary compound Zn_xCd_1?xTe. We attribute the higher intensity peak between 190 and 195 cm^?1 to the first harmonic of the zone-center longitudinal optical mode (LO₁) and, the lower intensity peak between 157 and 160 cm^?1 to the second harmonic (LO₂) of Zn_xCd_1?xTe crystal. The wave-number of vibrational Raman modes indicates that zinc content varies between 39 and 50% during the growth of quantum dots. The asymptotic absorption edge against heat-treatment time plot extrapolates to a bulk band gap of 1.714 eV which sets a lower limit of 31% for zinc incorporated into quantum dots which is consistent with the results of resonant Raman measurements. The energetic position of asymptotic absorption edge of 1.592 eV and an additional unresolved weak structure in Raman spectrum between 166 and 182 cm^?1 observed for as-received glass might serve as a evidence for the occurrence of a different nanocrystalline phase with 13% zinc content.