Synthesis and characterization of a polyaniline-modified SnO<Subscript>2</Subscript> nanocomposite

Polyaniline-modified tin oxide and tin oxide nanoparticles were synthesized using a solution route technique. The obtained pristine products were characterized with X-ray diffraction, thermogravimetric analysis, scanning electron microscopy, and optical absorption spectroscopy. Thermogravimetric analysis results showed that the polyaniline-modified SnO₂ nanoparticles exhibit higher thermal stability than the SnO₂ nanoparticles. Scanning electron microscopy analysis on the as-synthesized powders showed spherical particle in the range of 50–100 nm.     

Antiferromagnetic interactions in Er-doped SnO<Subscript>2</Subscript> DMS nanoparticles

Diluted magnetic semiconductor (DMS) nanoparticles of Sn_1−x Er _x O₂ (x = 0.0, 0.02, 0.04, and 0.1) were prepared by sol–gel method. The X-ray diffraction patterns showed SnO₂ rutile structure for all samples with no impurity peaks. The decrease in crystallite size with Er concentration was confirmed from TEM measurements (from 12 to 4 nm). The UV–Visible absorption spectra of Er-doped SnO₂ nanoparticles showed blue shift in band gap compared to undoped SnO₂. The electron spin resonance analysis of Er-doped SnO₂ nanoparticles indicate Er³⁺ in a rutile lattice and also decrease in intensity with Er concentration above x = 0.02. Temperature-dependent magnetization studies and the inverse susceptibility curves indicated increased antiferromagnetic interaction with Er concentration.     

Synthesis of MgAl<Subscript>2</Subscript>O<Subscript>4</Subscript> spinel nanoparticles using a mixture of bayerite and magnesium sulfate

This article reports a novel method to prepare MgAl₂O₄ spinel nanoparticles. By calcining a powder mixture of bayerite and magnesium sulfate at 800 °C and washing with water, single-phase MgAl₂O₄ spinel nanoparticles were prepared. The powder mixture and the calcined products were characterized by differential thermal and thermogravimetric analysis (DSC-TG), X-ray diffraction (XRD), transmission electron microscopy (TEM), and Brunauer–Emmett–Teller (BET) nitrogen-gas adsorption method. The obtained MgAl₂O₄ spinel nanoparticles have an average particle size of 12 nm, a narrow size distribution, and weak agglomeration. The specific surface area of the MgAl₂O₄ spinel powder is 110 m²/g. The formation of MgAl₂O₄ spinel is attributed to a solid-state reaction between γ-Al₂O₃ and MgSO₄.     

Biotemplate fabrication of SnO<Subscript>2</Subscript> nanotubular materials by a sonochemical method for gas sensors

A sonochemical method is developed to fabricate SnO₂ nanotubular materials from biological substances (here, it is cotton). The cotton fibers in SnCl₂ solution were first treated with ultrasonic waves in air, followed by calcinations to give nanotubular materials that faithfully retain the initial cotton morphology. The microstructure and morphology of the obtained SnO₂ nanotubules were characterized by the combination of field-emission scanning electron microscope (FE-SEM), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR), X-ray diffraction (XRD), and N₂ adsorption/desorption measurements. The thermal behavior and crystalline properties were examined in the temperature range of 450–700 °C. The nanocrystals composing of SnO₂ nanotubules were estimated about 8.5, 13.2, and 14.2 nm corresponding to calcination temperatures of 450, 550, and 700 °C, respectively. The sensor performance of biomorphic SnO₂ nanotubules calcined at 700 °C was investigated in the atmosphere of ethanol, formaldehyde, carbinol, carbon monoxide, hydrogen, ammonia, and acetone, respectively, which exhibited a good selectivity for acetone at a working temperature of 350 °C. The sensitivity to 20 ppm acetone, S, was 6.4 at 350 °C with rapid response and recovery (around 10–9 s). These behaviors were well explained in relation to the morphology of the nanotubules thus produced.     

Conventional wet impregnation versus microwave-assisted synthesis of SnO<Subscript>2</Subscript>/CNT composites

Carbon nanotubes decorated with SnO₂ nanoparticles were prepared by conventional and microwave-assisted wet impregnation. The composites were thoroughly characterized by X-ray diffraction, Raman spectroscopy, BET-surface area measurement, Scanning and transmission electron microscopy. The XRD studies revealed the formation of tetragonal phase of SnO₂. The microwave method produced CNTs heavily decorated with SnO₂ nanoparticles with average size 5 nm in a total reaction time of 10 min because of the rapid volumetric heating. DC conductivity increased significantly for the nanocomposite samples when compared with the pure CNTs. In electrical conductivity properties, sample prepared by microwave method was found to be superior to the one prepared by conventional procedure due to homogeneous distribution of nanoparticles.     

Synthesis of nanocrystalline SnO<Subscript>2</Subscript> in supercritical water

Nanocrystalline SnO₂ was synthesized in supercritical water at 385–415°C and 30 MPa (38–106 s residence time) in a tubular flow reactor from an aqueous solution of 0.1–0.4 M SnCl₄. The conversion rate was between 53 and 81%, but increased to 97.8% when 0.1 M NaOH was added. Nanoparticles were analyzed by a series of independent analytical techniques, including TEM, Raman, XRD, SEM, EDX and FT-IR. The initial size of the particles was about 3.7 nm. After calcination at 450°C for 2 h, the particle size increased to 4 nm. The particles were of low crystallinity, as indicated by the weak Raman and XRD signals. All particles were composed of Sn and O, as verified by the EDX spectra. The crystals were tetragonal, as confirmed by the weak XRD spectrum. After calcination at 600°C for 10 h, the particle size increased to 9 nm, while high crystallinity was confirmed by Raman and XRD analyses. All the crystals had the same structure, as indicated by TEM electron diffraction patterns. Using this one-step supercritical water process, nanoparticles of SnO₂ can be conveniently produced continuously in a flow reactor in less than 2 min.     

Rapid extra-/intracellular biosynthesis of gold nanoparticles by the fungus <Emphasis Type="Italic">Penicillium</Emphasis> sp.

In this work, the fungus Penicillium was used for rapid extra-/intracellular biosynthesis of gold nanoparticles. AuCl₄ ⁻ ions reacted with the cell filtrate of Penicillium sp. resulting in extracellular biosynthesis of gold nanoparticles within 1 min. Intracellular biosynthesis of gold nanoparticles was obtained by incubating AuCl₄ ⁻ solution with fungal biomass for 8 h. The gold nanoparticles were characterized by means of visual observation, UV–Vis absorption spectroscopy, X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and energy-dispersive X-ray spectroscopy (EDX). The extracellular nanoparticles exhibited maximum absorbance at 545 nm in UV–Vis spectroscopy. The XRD spectrum showed Bragg reflections corresponding to the gold nanocrystals. TEM exhibited the formed spherical gold nanoparticles in the size range from 30 to 50 nm with an average size of 45 nm. SEM and TEM revealed that the intracellular gold nanoparticles were well dispersed on the cell wall and within the cell, and they are mostly spherical in shape with an average diameter of 50 nm. The presence of gold was confirmed by EDX analysis.     

Synthesis and enhanced acetone gas-sensing performance of ZnSnO<Subscript>3</Subscript>/SnO<Subscript>2</Subscript> hollow urchin nanostructures

A kind of novel ZnSnO₃/SnO₂ hollow urchin nanostructure was synthesized by a facile, eco-friendly two-step liquid-phase process. The structure, morphology, and composition of samples were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and nitrogen adsorption–desorption techniques. The results revealed that many tiny needle-like SnO₂ nanowires with the average diameter of 5 nm uniformly grew on the surface of the ZnSnO₃ hollow microspheres and the ZnSnO₃/SnO₂ hollow urchin nanostructures with different SnO₂ content also were successfully prepared. In order to comprehend the evolution process of the ZnSnO₃/SnO₂ hollow urchin nanostructures, the possible growth mechanism of samples was illustrated via several experiments in different reaction conditions. Moreover, the gas-sensing performance of as-prepared samples was investigated. The results showed that ZnSnO₃/SnO₂ hollow urchin nanostructures with high response to various concentration levels of acetone enhanced selectivity, satisfying repeatability, and good long-term stability for acetone detection. Specially, the 10 wt% ZnSnO₃/SnO₂ hollow urchin nanostructure exhibited the best gas sensitivity (17.03 for 50 ppm acetone) may be a reliable biomarker for the diabetes patients, which could be ascribed to its large specific surface area, complete pore permeability, and increase of chemisorbed oxygen due to the doping of SnO₂.     

Controlled synthesis of CeO<Subscript>2</Subscript> nanoparticles using novel amphiphilic cerium complex precursors

Maleic anhydride was grafted by long-chain alcohols (1-hexadecanol, 1-octadecanol) to amphiphilic mono-L cis-butene dicarboxylates (L = hexadecyl, octadecyl), i.e., MAH, MAO, respectively. Subsequently, corresponding amphiphilic cerium complexes with these two mono-L cis-butene dicarboxylate ligands (Ce(L')₃, L'= MAH, MAO) were synthesized and behaved as the precursors to prepare CeO₂ nanoparticles for both of which can form nanosized micelle-like aggregates by special self-assembly in the wet chemical process. The nanoparticles were further characterized by Fourier transform-infrared spectroscopy (FTIR), Diffuse reflectance ultraviolet-visible spectra (DRUVS), scanning electron microscope (SEM), transmission electron microscope (TEM), and x-ray diffraction (XRD). Both the CeO₂ nanoparticles are in a cubic fluorite structure and present regular and well-dispersion club-like morphology with average particle size in the range of 40–70 nm. Besides, the strong ultraviolet–visible absorption for these CeO₂ nanoparticles can be found at the long-wavelength ultraviolet to visible region of 200–500 nm.     

Synthesis and gas sensing properties of perovskite CdSnO<Subscript>3</Subscript> nanoparticles

The CdSnO₃ semiconducting oxide that can be used as a gas-sensitive material for detecting ethanol gas is reported in this paper. CdSnO₃ nanoparticles were prepared by a chemical co-precipitation synthesis method, in which the preparation conditions were carefully controlled. The n-type gas-sensing semiconductors were obtained from the as-synthesized powders calcined at 600°C for 1 h. The phase and microstructure of the obtained nanoparticles were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and Brunauer–Emmett–Teller (BET) method with a gas adsorption analyzer. CdSnO₃ has a small particle size range of 30–50 nm and a high surface area of 9.12 m²/g, and a uniformity global shape. The gas sensitivity and operating temperature, and selectivity of CdSnO₃-based sensors were measured in detail. The gas sensors fabricated by CdSnO₃ nanoparticles had good sensitivity and selectivity to vapor of C₂H₅OH when working temperature at 267°C, the value of gas sensitivity at 100 ppm of C₂H₅OH gas can reach 11.2 times. Furthermore, gas-sensing mechanism was studied by using chromatographic analysis.     

Sonochemical fabrication of morpho-genetic TiO<Subscript>2</Subscript> with hierarchical structures for photocatalyst

Titanium oxides (TiO₂) with hierarchical structures have been successfully replicated from biotemplate using a sonochemical method. The bio-templates, cedarwoods, were irradiated under ultrasonic waves in TiCl₄ solutions and then calcined at temperatures between 450 and 600 °C. The fine replications of the biotemplates in TiO₂ down to nanometer’s level were verified using X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), and transmission electron microscopy (TEM). The photocatalytic activities were assessed by measuring the percentage degradation of methylene blue using UV–vis spectroscopy. The calcination temperature has a strong effect on the structural replication and photocatalytic activity of the replicas. It appears that the calcination temperature of 450 °C results in the best structural replication with the highest surface area of 54.8 m² g⁻¹, and thus has the best photocatalytic properties. This method provides a simple, efficient, and versatile technique for fabricating TiO₂ with hierarchical structures, and it has the potential to be applied to other systems for producing functional hierarchical materials for chemical sensor and nanodevices.     

Self-organization of bimetallic PdAu nanoparticles on SiO<Subscript>2</Subscript> surface

Bimetallic PdAu nanoparticles on SiO₂ substrate were produced by a sequential room-temperature sputtering deposition method. By the atomic force microscopy technique we studied the nanoparticles self-organization mechanisms in various conditions. First, Pd nucleation and growth proceeds at the substrate defects and the Pd nanoparticles density increase rapidly. During the second sputtering deposition, Au atoms adsorb on the SiO₂ and diffuse toward Pd nanoparticles without forming new nuclei. The Au atoms are trapped by the preformed Pd nanoparticles, forming PdAu bimetallic nanoparticles which size increases. Furthermore, fixing the amount of deposited Pd and increasing the amount of deposited Au, we analyzed the evolution of the PdAu film surface morphology: we observe that the PdAu grows initially as three-dimensional islands; then the PdAu film morphology evolves from compact three-dimensional islands to partially coalesced worm-like structures, followed by a percolation morphology and finally to a continuous and rough film. The application of the interrupted coalescence model allowed us to evaluate the critical mean island diameter R _c ≈ 2.8 nm for the partial coalescence process. The application of the dynamic scaling theory of growing interfaces allowed us to evaluate the dynamic growth exponent β = 0.21 ± 0.01 from the evolution of the film surface roughness. Finally, fixing the amount of deposited Pd and Au we studied the self-organization mechanism of the PdAu nanoparticles induced by thermal processes performed in the 973–1173 K temperature range. The observed kinetic growth mechanism is consistent with a surface diffusion-limited ripening of the nanoparticles with a temperature-dependent growth exponent. The dependence of the growth exponent on the temperature is supposed to be linked to the variation with the temperature of the characteristics of the PdAu alloy. The activation energy for the surface diffusion process was evaluated in 0.54 ± 0.03 eV.     

Structural and sensing properties of nanocrystalline SnO<Subscript>2</Subscript> films deposited by spray pyrolysis from a SnCl<Subscript>2</Subscript> precursor

We report the fabrication and characterization of tin dioxide gas sensing layers. The tin dioxide layers were synthesized using a convenient, simple and low-cost technique of spray pyrolysis. The formation of stoichiometric SnO₂ layers with fine-grain structure is revealed by Rutherford backscattering spectroscopy. The microstructure, phase, nanoparticle size distribution and surface morphology were studied by transmission electron microscopy, electron diffraction and atomic force microscopy. Most of the grains were of 10–20 nm size; however, some particles were up to 100 nm in size and had a microtwin lamellae structure of SnO₂ phase (cassiterite) with lattice parameters a= 0.474 nm and c= 0.319 nm. The sensitivity of the layers with respect to 1000–10000 ppm CH₄ in air was obtained from both resistivity (S_R) and capacity (S_C) measurements at 330 °C and values of S_R=5–7 and S_C=22–31 were extracted. PACS 68.43.-h; 68.55.-a; 81.05.Hd; 81.07.-b; 81.15.Rs     

Chemical synthesis of nanocrystalline SnO2 thin films for supercapacitor application

Nanocrystalline SnO₂ thin films were deposited by simple and inexpensive chemical route. The films were characterized for their structural, morphological, wettability and electrochemical properties using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy techniques (SEM), transmission electron microscopy (TEM), contact angle measurement, and cyclic voltammetry techniques. The XRD study revealed the deposited films were nanocrystalline with tetragonal rutile structure of SnO₂. The FT-IR studies confirmed the formation of SnO₂ with the characteristic vibrational mode of Sn-O. The SEM studies showed formation of loosely connected agglomerates with average size of 5-10 nm as observed from TEM studies. The surface wettability showed the hydrophilic nature of SnO₂ thin film (water contact angle 9°). The SnO₂ showed a maximum specific capacitance of 66 F g⁻¹ in 0.5 Na₂SO₄ electrolyte at 10 mV s⁻¹ scan rate.     

Crystal structure of iron-oxide nanoparticles synthesized from ferritin

We have investigated the crystal structure of nanosized iron-oxide by X-ray diffraction (XRD), extended X-ray absorption fine structure measurements at the iron K-edge as well as by transmission electron microscopy (TEM). Iron-oxide nanoparticles were produced by thermal treatment of horse spleen ferritin molecules. The structure of these particles was compared to α-Fe₂O₃ and γ-Fe₂O₃ nanopowder references. The thermal treatment of a submonolayer film of ferritin molecules results in pure γ-Fe₂O₃ nanoparticles, while for films above a certain thickness α-Fe₂O₃ and γ-Fe₂O₃ coexist, exhibiting two different crystallite sizes. TEM shows a characteristic particle diameter of ~7 nm for γ-Fe₂O₃ resulting from thermal treatment of monolayers, consistent with the crystallite size of the γ-phase as obtained from XRD measurements on multi-layered samples. XRD shows the α-Fe₂O₃ phase to be characterized by a crystallite size of ~34 nm.     

Fabrication and characterization of CdS-sensitized TiO<Subscript>2</Subscript> nanotube photoelectrode

CdS quantum dot (Qd)-sensitized TiO₂ nanotube array photoelectrode is synthesised via a two-step method on tin-doped In₂O₃-coated (ITO) glass substrate. TiO₂ nanotube arrays are prepared in the ethylene glycol electrolyte solution by anodizing titanium films which are deposited on ITO glass substrate by radio frequency sputtering. Then, the CdS Qds are deposited on the nanotubes by successive ionic layer adsorption and reaction technique. The resulting nanotube arrays are characterized by scanning electron microscopy, X-ray diffraction (XRD) and UV–visible absorption spectroscopy. The length of the obtained nanotubes reaches 1.60 μm and their inner diameter and wall thickness are around 90 and 20 nm, respectively. The XRD results show that the as-prepared TiO₂ nanotubes array is amorphous, which are converted to anatase TiO₂ after annealed at 450 °C for 2 h. The CdS Qds deposited on the TiO₂ nanotubes shift the absorption edge of TiO₂ from 388 to 494 nm. The results show that the CdS-sensitized TiO₂ nanotubes array film can be used as the photoelectrode for solar cells.     

A new green synthesis method of CuInS<Subscript>2</Subscript> and CuInSe<Subscript>2</Subscript> nanoparticles and their integration into thin films

A new preparation method for CuInS₂ and CuInSe₂ nanoparticles synthesis is described without using any organic solvent. Heating Cu, In, and S/Se precursors dissolved in water for 30 min in a microwave oven in the presence of mercapto-acetic acid leads to monodispersed chalcopyrite nanoparticles. No precipitation of these nanoparticles is observed after several months at room temperature. These new materials have been thoroughly characterized to confirm their compositions, sizes, and structure without any filtration. Transmission electron microscopy (TEM) confirmed particle sizes below 5 nm. Energy dispersive X-ray analysis (EDXA) confirmed the chemical composition of these samples. X-ray diffraction (XRD) showed a chalcopyrite-type structure with crystallite size of about 2 nm. No difference has been observed between batch and continuous synthesis processes. Cu _x InS₂ and Cu _x InSe₂ nanoparticles, with x < 1, have been also synthesized and identified. Simulation using a commercial software confirmed the difference between copper poor (Cu _x InS₂) and copper rich (CuInS₂) chalcopyrite structures. Conventional spray deposition techniques have been used to form relatively thin films on solid substrates.     

A novel synthesis of FeNbO<Subscript>4</Subscript> nanorod by hydrothermal process

This study reports a facile, gram-scale synthesis of FeNbO₄ nanorods via hydrothermal route, using iron nitrate [Fe(NO₃)₃] and niobium tartarate (Nb tartarate) in presence of potassium peroxosulfate. The formation of single phase, polycrystalline orthorhombic structure of FeNbO₄ was confirmed by the careful analysis of the X-ray diffraction (XRD) pattern. The average crystallite size, calculated using a few XRD peaks, was found to be 12.8 nm. As indicated by transmission electron microscopy (TEM) and field emission scanning electron microscopy, the average length and diameter of the rods were found to be only 25 × 7 nm and 47 × 14 nm, respectively. The selected area electron diffraction and high-resolution transmission electron microscopy (HRTEM) data of the single rod implied that FeNbO₄ nanorods were polycrystalline in nature and grew up along the c-axis. HRTEM also revealed that the fringes are equidistant with a lattice separation of 0.91 Ǻ, which corresponded to the (111) plane of the FeNbO₄ crystal. Elemental composition of the nanorods was confirmed using electron dispersive X-ray spectroscopy analysis while binding state of the surface was intervened through X-ray photoelectron spectroscopy. Mechanistic investigations suggested that potassium peroxosulfate played a crucial role in the unidirectional growth of particles. The synthetic method is simple, amenable to scale up and contributes a new tool box for the development of FeNbO₄-based one-dimensional (1D) structures that appears to be more promising for a myriad of applications, compared to their 3D counterparts.     

Structural,dielectric and photoluminescence properties of co-precipitated Zn-doped SnO2 nanoparticles

Zn-doped SnO₂ nanoparticles were prepared by the chemical co-precipitation route. X-ray diffraction (XRD) and transmission electron microscopy (TEM) analyses of these prepared nanoparticles were carried out for structural and morphological studies. All the samples have been found to have tetragonal rutile structure of the polycrystalline SnO₂ having crystallite size in the range 13–25 nm. TEM micrographs show agglomeration of nanoparticles in all the samples. At a particular temperature, the dielectric constant of all the samples has been found to decrease with increasing frequencies which may be due to rapid polarization processes occurring in SnO₂ nanoparticles. The ac conductivity, σ (ω), has been found to vary with frequency according to the relation σ (ω) ∝ ω^S. The value of S has been found to be temperature dependent, decreasing with increasing frequency which suggests that a hopping process is the most likely conduction mechanism in these nanoparticles. The room temperature photoluminescence (PL) spectra of the undoped and Zn-doped SnO₂ nanoparticles consist of the near band-edge ultraviolet (UV) emission and the defect related visible emissions. The origin of emission peaks in the visible region is attributed to oxygen-related defects that are introduced during growth.     

Electrochemical supercapacitor studies of hierarchical structured Co2+-substituted SnO2 nanoparticles by a hydrothermal method

Hierarchical structured Co-doped SnO₂ nanoparticles are prepared by a low temperature hydrothermal process. The structural and surface morphologies of the SnO₂ and Sn_1?xCo_xO₂ nanoparticles are studied by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). The Sn_1?xCo_xO₂ nanoparticles form with a tetragonal rutile structure during the hydrothermal process without further calcination. The pseudocapacitance behavior of the Sn_1?xCo_xO₂ nanoparticles is characterized by cyclic voltammetry (CV) in 1.0 M H₂SO₄ electrolyte. The specific capacitance (SC) is found to increase with an increase in cobalt content. A maximum SC of 840 F g^?1 is obtained for a Sn_0.96Co_0.04O₂ composite at a 10 mV s^?1 scan rate.