Influence of the solvent on ultrasonically produced SbSI nanowires

The influence of the substitution of methanol in place of ethanol during the ultrasonic production of antimony sulfoiodide (SbSI) nanowires is presented. The new technology is faster and more efficient at temperatures greater than 314 K. The products were characterized by using techniques such as powder X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDXA), high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), optical diffuse reflection spectroscopy (DRS) and IR spectroscopy. The coexistence of Pna2₁ (ferroelectric) and Pnam (paraelectric) phases at 298 K was observed in the SbSI nanowires produced in methanol. The methanol decomposes during the sonication or due to the adsorption process on SbSI nanowires.     

Using of sonochemically prepared SbSI for electrospun nanofibers

A novel polymeric, polyacrylonitrile (PAN) nanofibers containing ferroelectric and semiconducting antimony sulfoiodide (SbSI) have been made by electrospinning. SbSI nanowires, used as the filler, have been prepared sonochemically from antimony sulphide (Sb₂S₃) and antimony tri-iodide (SbI₃) for the first time. Nanocrystalline SbSI has been fabricated in ethanol under ultrasonic irradiation (20 kHz, 565 W/cm²) at 323 K within 2 h. The products have been characterized by using techniques such as powder X-ray diffraction, scanning electron microscopy, energy dispersive X-ray analysis, high-resolution transmission electron microscopy, selected area electron diffraction and optical diffuse reflection as well as transmission spectroscopy. The good quality of the nanocrystals and their dispersion in the nanofiber’s volume is important because this material is attractive for nanogenerators due to its ferroelectric and piezoelectric properties. The amplitude of the voltage pulse, generated under shock pressure of 3.0 MPa, has reached 180 V in the prototype PAN/SbSI piezoelectric nanogenerator. The peak output voltage of about 0.2 V was measured in bending/releasing conditions with the deformation frequency of 1 Hz.     

Sonochemical growth of antimony selenoiodide in multiwalled carbon nanotube

This paper presents, for the first time, the nanocrystalline, semiconducting antimony selenoiodide (SbSeI) grown in multi-walled carbon nanotubes (CNTs). It was prepared sonochemically using elemental Sb, Se, and I in the presence of ethanol under ultrasonic irradiation (35 kHz, 2.6 W/cm²) at 323 K for 3 h. The CNTs filled with SbSeI were characterized by using techniques such as powder X-ray diffraction, scanning electron microscopy, energy dispersive X-ray analysis, high-resolution transmission electron microscopy, selected area electron diffraction, and optical diffuse reflection spectroscopy. These investigations exhibit that the SbSeI filling the CNTs is single crystalline in nature and in the form of nanowires. It has indirect allowed energy band gap E_gIf = 1.61(6) eV.     

Synthesis of multi-wall carbon nanotubes by the pyrolysis of ethanol on Fe/MCM-41 mesoporous molecular sieves

Ordered hexagonal arrangement MCM-41 mesoporous molecular sieves were synthesized by the traditional hydrothermal method, and Fe-loaded MCM-41 mesoporous molecular sieves (Fe/MCM-41) were prepared by the wet impregnation method. Their mesoporous structures were testified by X-ray diffraction (XRD) and the N₂ physical adsorption technique. Carbon nanotubes (CNTs) were synthesized by the chemical vapor deposition (CVD) method via the pyrolysis of ethanol at atmospheric pressure using Fe/MCM-41 as a catalytic template. The effect of different reaction temperatures ranging from 600 to 800 ^°C on the formation of CNTs was investigated. The resulting carbon materials were characterized by various physicochemical techniques such as transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), and Raman spectroscopy. The results show that multi-wall carbon nanotubes (MWCNTs) with an internal diameter of ca. 7.7 nm and an external diameter of ca. 16.9 nm were successfully obtained by the pyrolysis of ethanol at 800 ^°C utilizing Fe/MCM-41 as a catalytic template.     

Sonochemical preparation of antimony subiodide

The substantiated isolation of the antimony subiodide (Sb₃I) is presented for the first time. It has been prepared using elemental Sb and I in ethanol under ultrasonic irradiation at 323 K. Its composition was characterized using X-ray photoelectron spectroscopy (XPS) and energy dispersive X-ray analysis (EDAX). The scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HRTEM) investigations exhibit that the samples are made up of large quantity of nanoparticles with diameters smaller than 20 nm and single crystalline in nature. The interplanar spacings in Sb₃I that have been determined using powder X-ray diffraction (XRD), selected area electron diffraction (SAED) and HRTEM are very similar. Surprisingly, the registered XRD patterns are identical to the one reported earlier for Sb₄O₅I₂.     

Synthesis of carbon nanotubes via Fe-catalyzed pyrolysis of phenolic resin

Carbon nanotubes (CNTs) with 40–100 nm in diameter and tens of micrometers in length were prepared via catalytic pyrolysis of phenol resin in Ar at 673–1273 K using ferric nitrate as a catalyst precursor. Structure and morphology of pyrolyzed resin were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Raman spectroscopy. Ferric nitrate was transformed to Fe₃O₄ at 673 K, and to metallic Fe and Fe_xC carbide at 873–1273 K. The optimal weight ratio of Fe catalyst to phenol resin for growing CNTs was 1.00 wt%, and the optimal temperature was 1073 K. In addition, use of a high pressure increased the yield of CNTs. Density functional theory (DFT) calculations suggest that Fe catalysts facilitate the CNTs growth by increasing the bond length and weakening the bond strength in C₂H₄ via donating electrons to the C atoms in it.     

Synthesis of a composite consisting of carbon nanotubes and graphite shell-encapsulated cobalt nanoparticles using plasma-enhanced chemical vapor deposition

We report a simple and effective one-step synthesis route for synthesizing a composite consisted of carbon nanotubes (CNTs) and graphite shell-encapsulated cobalt nanoparticles using plasma-enhanced chemical vapor deposition on Si (1 0 0) substrate covered with catalyst Co particles, discharging a mixture of H₂ and CH₄ gas, and characterize the obtained composite by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, high resolution transmission electron microscope, and X-ray photoelectron spectroscopy. The results show that CNTs align perpendicularly to the substrate and graphite shell-encapsulated Co nanoparticles clung to the external surfaces of aligned CNTs. The diameter of the graphite shell-encapsulated Co nanoparticles increases with increasing the H₂ content in H₂ and CH₄ carbonaceous gas. A possible growth mechanism of the CNTs and graphite shell-encapsulated cobalt nanoparticles composite has been explored.     

Room temperature chemical synthesis of lead selenide thin films with preferred orientation

Room temperature chemical synthesis of PbSe thin films was carried out from aqueous ammoniacal solution using Pb(CH₃COO)₂ as Pb²⁺ and Na₂SeSO₃ as Se²⁻ ion sources. The films were characterized by a various techniques including, X-ray diffraction (XRD), energy dispersive X-ray analysis (EDAX), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HR-TEM), selected area electron diffraction (SAED), Fast Fourier transform (FFT) and UV-vis-NIR techniques. The study revealed that the PbSe thin film consists of preferentially oriented nanocubes with energy band gap of 0.5 eV.     

Characterization and applications of as-grown β-Fe<Subscript>2</Subscript>O<Subscript>3</Subscript> nanoparticles prepared by hydrothermal method

The production of low-dimensional nanoparticles (NPs) with appropriate surface modification has attracted increasing attention in biological, biochemical, and environmental applications including chemical sensing, photocatalytic degradation, separation, and purification of toxic molecules from the matrices. In this study, iron oxide NPs have been prepared by hydrothermal method using ferric chloride and urea in aqueous medium under alkaline condition (pH 9 ~ 10). As-grown low-dimensional NPs have been characterized by UV–vis spectroscopy, FT-IR, X-ray diffraction, Field emission scanning electron microscopy, Raman spectroscopy, High-resolution Transmission electron microscopy, and Electron Diffraction System. The uniformity of the NPs size was measured by the scanning electron microscopy, while the single phase of the nanocrystalline β-Fe₂O₃ was characterized using powder X-ray diffraction technique. As-grown NPs were extensively applied for the photocatalytic degradation of acridine orange (AO) and electrochemical sensing of ammonia in liquid phase. Almost 50% photo-catalytic degradation with AO was observed in the presence of UV sources (250 W) with NPs. β-Fe₂O₃ NP-coated gold electrodes (GE, surface area 0.0216 cm²) have enhanced ammonia-sensing performances in their electrical response (I–V characterization) for detecting ammonia in liquid phase. The performances of chemical sensor were investigated, and the results exhibited that the sensitivity, stability, and reproducibility of the sensor improved significantly using β-Fe₂O₃ NPs on GE surface. The sensitivity was approximately 0.5305 ± 0.02 μAcm⁻²mM⁻¹, with a detection limit of 21.8 ± 0.1 μM, based on a signal/noise ratio of 3 with short response time.     

Pyridine-thermal synthesis and high catalytic activity of CeO2/CuO/CNT nanocomposites

Carbon nanotubes (CNTs) were controllably coated with the uninterrupted CuO and CeO₂ composite nanoparticles by a facile pyridine-thermal method and the high catalytic performance for CO oxidation was also found. The obtained nanocomposites were characterized by transmission electron microscopy, scanning electron microscopy, X-ray diffraction as well as X-ray photoelectron spectroscopy. It is found that the CuO/CeO₂ composite nanoparticles are distributed uniformly on the surface of CNTs and the shell of CeO₂/CuO/CNT nanocomposites is made of nanoparticles with a diameter of 30-60 nm. The possible formation mechanism is suggest as follows: the surface of CNTs is modified by the pyridine due to the π-π conjugate role so that the alkaline of pyridine attached on the CNT surface is more enhanced as compared to the one in the bulk solvent, and thus, these pyridines accept the proton from the water molecular preferentially, which result in the formation of the OH⁻ ions around the surface of CNTs. Subsequently, the metal ions such as Ce³⁺ and Cu²⁺ in situ react with the OH⁻ ions and the resultant nanoparticles deposit on the surface of CNTs, and finally the CeO₂/CuO/CNT nanocomposites are obtained. The T₅₀ depicting the catalytic activity for CO oxidation over CeO₂/CuO/CNT nanocomposites can reach ∼113 °C, which is much lower than that of CeO₂/CNT or CuO/CNT nanocomposites or CNTs.     

Investigation of hydrogen storage in MWCNT–TiO2 composite

The hydrogen storage capacity of MWCNT–TiO₂ composite has been evaluated in the present work. The composite has been prepared by means of ultrasonication followed by drop casting on substrates. Morphology, structural and functional group studies of the prepared samples are carried out by transmission electron microscopy (TEM), scanning electron microscopy (SEM), powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and Raman spectroscopy. Then, the samples are hydrogenated in the hydrogenation chamber as a function of time. Hydrogen storage capacity of the composite sample is found to be 0.9 wt% at 100 °C. Hydrogen uptake of the composite is accounted for the spillover mechanism in CNTs–metal oxide composite. Desorption temperature range, activation energy of desorption, binding energy of hydrogen are determined from thermogravimetric (TG) analysis.     

Magnetic properties of Ni/NiO nanocomposites synthesized by one step solution combustion method

Ni/NiO nanocomposites were synthesized using solution combustion method and characterized with X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDAX) and carbon, hydrogen, nitrogen (CHN) analyser. The Ni or NiO content in Ni/NiO nanocomposites vary with the quantity of HNO₃ used for the synthesis. Magnetic coercivity (H_c) of Ni/NiO nanocomposites is found to be 413 Oe which can be used in magnetic applications. A feeble exchange bias of 7 Oe is seen from the NiO rich Ni/NiO.     

Influence of Fe ions in characteristics and optical properties of mesoporous titanium oxide thin films

Fe-doped mesoporous titanium dioxide (M-TiO₂-Fe) thin films have been prepared on indium tin oxide (ITO) glass substrates by sol–gel and spin coating methods. All films exhibited mesoporous structure with the pore size around 5–9 nm characterized by small angle X-ray diffraction (SAXRD) and further confirmed by high resolution transmission electron microscopy (HRTEM). Raman spectra illustrated that lower Fe-doping contributed to the formation of nanocrystalline of M-TiO₂-Fe thin films. X-ray photoelectron spectroscopy (XPS) data indicated that the doped Fe ions exist in forms of Fe³⁺, which can play a role as e⁻ or h⁺ traps and reduce e⁻/h⁺ pair recombination rate. Optical properties including refractive indices/n, energy gaps/E_g and Urbach energy width/E₀ of the thin films were estimated and investigated by UV/vis transmittance spectra. The presence of Fe content extended the light absorption band and decreased the values of n, implying enhanced light response and performance on dye-sensitized solar cells (DSSC). The optimum Fe content in M-TiO₂-Fe thin films is determined as 10 mol%, for its compatibility of well crystalline and well potential electron transfer performance.     

Preparation and luminescence study of Eu(III) titanate nanotubes and nanowires using carbon nanotubes as removable templates

Eu(III) titanate nanotubes and nanowires have been successfully synthesized by solvothermal method using carbon nanotubes (CNTs) as removable templates. The products were characterized by X-ray diffraction spectroscopy, transmission electron microscopy, energy-dispersive X-ray spectrometry, thermogravimetric and differential thermal analysis. It is demonstrated that CNTs are fully coated with an amorphous Eu₂(TiO₃)₃ layer, which is about 10 nm thick and almost continuous and uniform. After the Eu₂(TiO₃)₃/CNTs composites have been calcined at various temperatures, Eu₂(TiO₃)₃ nanotubes and nanowires are obtained by removing the CNTs templates. The diameter of the Eu₂(TiO₃)₃ nanotubes is 40–60 nm, which is consistent with that of CNTs. Both nanotubes and nanowires have a narrow distribution of diameters. The fluorescence properties of the Eu₂(TiO₃)₃ nanotubes and nanowires calcined at various temperatures have been investigated. The results indicate that when the Eu₂(TiO₃)₃/CNTs composites were calcined at 700 °C for 5 h, the Eu₂(TiO₃)₃ nanotubes obtained can be effectively excited by 395 nm light, and exhibit strong red emission around 616 nm. It is very interesting to discover that a few residual carbons doped in Eu₂(TiO₃)₃ nanotubes and many oxygen vacancies could promote the intensity of red emission peak of Eu³⁺ ions. In addition, Eu₂(TiO₃)₃ nanowires calcined at 900 °C for 5 h also have a strong red emission peak due to many oxygen vacancies and defects formed on the surface of the nanowires and inside them.     

Sonochemical preparation of SbSI gel

A novel sonochemical method for direct preparation of nanocrystalline antimony sulfoiodide (SbSI) has been established. The SbSI gel was synthesized using elemental Sb, S and I in the presence of ethanol under ultrasonic irradiation (35 kHz, 2 W/cm²) at 50 °C for 2 h. The products were characterized by using techniques such as powder X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDAX), high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), and optical diffuse reflection spectroscopy (DRS). The SEM and HRTEM investigations exhibit that the as-prepared samples are made up of large quantity nanowires with diameters of about 10–50 nm and lengths reaching up to several micrometers and single-crystalline in nature.     

Galvanostatically deposited Fe: MnO2 electrodes for supercapacitor application

The present investigation describes the addition of iron (Fe) in order to improve the supercapacitive properties of MnO₂ electrodes using galvanostatic mode. These amorphous worm like Fe: MnO₂ electrodes are characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), energy dispersive X-ray analysis (EDAX), Fourier transform infrared spectroscopy (FTIR) and wettability test. The supercapacitive properties of MnO₂ and Fe: MnO₂ electrodes are investigated using cyclic voltammetry, chronopotentiometry and impedance techniques. It is seen that the supercapacitance increases with increase in Fe doping concentration and achieved a maximum of 173 F g^?1 at 2 at% Fe doping. The maximum supercapacitance obtained is 218 F g^?1 for 2 at% Fe: MnO₂ electrode. This hydrous binary oxide exhibited ideal capacitive behavior with high reversibility and high pulse charge–discharge property between ?0.1 and +0.9 V/SCE in 1 M Na₂SO₄ electrolyte indicating a promising electrode material for electrochemical supercapacitors.     

Improved performance of porous LiFePO4/C as lithium battery cathode processed by high energy milling comparison with conventional ball milling

Porous LiFePO₄ is synthesized and coated with amorphous carbon by using high energy nano-mill (HENM) processed solid-state reaction method. FeCl₃ (38%) containing water solution which is originated from pickling of steel scrap (waste liquid) is used as a source material in this study. The result indicates that LiFePO₄ powders are well coated with the amorphous carbon. HENM process successfully produces the porous LiFePO₄ with homogeneously distributed pores and a well networked carbon web, which delivers an enhanced electrochemical rate capability. HENM process is incorporated as an effective route for reducing particle size, distributing particle homogeneously and averting agglomeration of particles of precursor in this study. X-ray diffraction, scanning electron microscopy with elemental mapping, transmission electron microscopy with selected area (electron) diffraction, Raman spectroscopy, cyclic voltammetry, and galvanostatic charge/discharge are employed to characterize the final product. Electrochemical measurement shows that the synthesized LiFePO₄/C composite cathode delivers an initial discharge capacity of 161 mAhg⁻¹ at 0.1C-rate between 4.2 and 2.5 V. Remarkably, the cathode delivers 101.9 mAhg⁻¹ at high charge/discharge rate (10 C).     

Hydrothermal synthesis of chalcopyrite CuInS2, CuInSe2 and CuInTe2 nanocubes and their characterization

CuInS₂, CuInSe₂ and CuInTe₂ nanocubes of chalcopyrite structure have been successfully synthesized by hydrothermal process using deionized water as solvent at 180 °C for 20 h. The crystallinity, compositional, morphological and optical properties of the synthesized samples were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray (EDX), Raman and photoluminescence (PL) spectra analyses. The Raman spectra of the synthesized CuInS₂, CuInSe₂ and CuInTe₂ samples show the dominant A₁ modes at 293, 172 and 121 cm⁻¹ respectively. The possible chemical reaction and mechanism of nanocubes formation were discussed. The emission wavelength of as synthesized CuInS₂, CuInSe₂ and CuInTe₂ samples were blue shifted at 746 nm (1.66 eV), 863 nm (1.43 eV) and 859 nm (1.44 eV) respectively.     

Sonochemical preparation of SbS1−xSexI nanowires

A sonochemical method for direct preparation of nanowires of SbS_1?xSe_xI solid solution has been established. The SbS_1?xSe_xI gel was synthesized using elemental Sb, S, Se and I in the presence of ethanol under ultrasonic irradiation (35 kHz, 2 W/cm²) at 50 °C for 2 h. The product was characterized by using techniques such as powder X-ray diffraction, scanning electron microscopy, high-resolution transmission electron microscopy, energy dispersive X-ray analysis, selected area electron diffraction, and optical diffuse reflection spectroscopy. The SEM and HRTEM investigations exhibit that the as-prepared samples are made up of large quantity nanowires with lateral dimensions of about 10–50 nm and lengths reaching up to several micrometers and single-crystalline in nature. The increase of molar composition of Se affects linear decrease of the indirect forbidden optical energy gap as well as the distance between (121) planes of the SbS_1?xSe_xI nanowires.     

Nanocrystalline GdAlO3: XPS,EPR and magnetic susceptibility studies

Nanocrystalline gadolinium monoaluminate (GdAlO₃) has been synthesized by sol–gel method after sintering the precursor gel at 950°C. The microstructural features have been proved by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and energy-dispersive X-ray analysis (EDX). The XRD pattern confirms the formation of single-phase GdAlO₃ while EDX shows that this nanomaterial is stoichiometric; the average size of the nanoparticles is 40 nm. X-ray photoelectron spectroscopy (XPS) has been used to study the chemical composition and bonding in the as-prepared samples. The binding energies of core-level electrons in Gd, Al and O in GdAlO₃ nanopowder have been found slightly shifted compared to the corresponding values of the same elements. The electron paramagnetic resonance (EPR) spectra at 9.23 GHz (X-band) and different temperatures indicate the existence of magnetically concentrated solid containing Gd³⁺ ions. Nèel temperature, T _N =3.993 K, effective Bohr magneton number, μ _eff=8.18, and constant of magnetic exchange interaction, J _ex=−0.069 cm⁻¹, have been determined from DC magnetic susceptibilities measured in the range 2–300 K.