Synthesis and crystallization of lead–zirconium–titanate (PZT) nanotubes at the low temperature using carbon nanotubes (CNTs) as sacrificial templates

Pb(Zr_0.52Ti_0.48)O₃ (PZT) nanotubes with diameters of 80–100 nm and a wall thickness of 15–20 nm were prepared by sol–gel template technique and using multi-walled carbon nanotubes (MWCNT) as sacrificial templates. The coating process of MWCNT with PZT precursor sol and removal of the carbon nanotubes by an interrupt heat treatment were discussed and studied by Raman spectroscopy. Simultaneous thermal analysis (STA) revealed that PZT nanotube crystallized at the low temperature of 410 °C by the significantly low activation energy of crystallization of 103.7 kJ/mol. Moreover, based on the X-ray diffraction (XRD) pattern and selected area electron diffraction pattern the crystal structure of the PZT nanotube was determined as perovskite. High resolution transmission electron microscope (HRTEM) and field-emission scanning electron microscope (FE-SEM) images proved that the final PZT had a tubular structure.     

Fabrication and characterization of a zirconia/multi-walled carbon nanotube mesoporous composite

A zirconia/multi-walled carbon nanotube (ZrO₂/MWCNT) mesoporous composite was fabricated via a simple method using a hydrothermal process with the aid of the cationic surfactant cetyltrimethylammonium bromide (CTAB). Transmission electron microscopy (TEM), N₂ adsorption–desorption, Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD) techniques were used to characterize the as-made samples. The cubic ZrO₂ nanocrystallites were observed to overlay the surface of MWCNTs, which resulted in the formation of a novel mesoporous–nanotube composite. On the basis of a TEM analysis of the products from controlled experiment, the role of the acid-treated MWCNTs and CTAB was proposed to explain the formation of the mesoporous–nanotube structure. The as-made composite possessed novel properties, such as a high surface area (312 m² · g^? 1) and a bimodal mesoporous structure (3.18 nm and 12.4 nm). It was concluded that this composite has important application value due to its one-dimensional hollow structure, excellent electric conductivity and large surface area.     

Synthesis of nanocrystalline GaN from Ga2O3 nanoparticles derived from salt-assisted spray pyrolysis

Gallium nitride (GaN) nanoparticles were successfully produced from nano-sized gallium oxide (Ga₂O₃) particles under a flow of ammonia gas. The gallium oxide nanoparticles were prepared by salt-assisted spray pyrolysis (SASP). Highly crystalline Ga₂O₃ nanoparticles with an average diameter of approximately 10 nm were obtained at various temperatures when a flux salt (LiCl, 5 mol/l) was added to the precursor solution. The effects of the crystallinity of the Ga₂O₃ particles and nitridation time on transformation to GaN were characterized using X-ray diffraction and scanning/transmission electron microscopy. Highly crystalline GaN nanoparticles with a mean size of 23.4 nm and a geometric standard deviation of 1.68 nm were obtained when Ga₂O₃ nanoparticles with relatively low crystallinity were used as the starting material. The resulting GaN nanoparticles showed a photoluminescence peak at 364 nm under UV excitation at 254 nm.     

Strong quantum confinement effect in nanocrystalline cerium oxide

Highly uniform and well-dispersed cerium oxide quantum dots were successfully synthesized by simple precipitation method by using cerium ammonium nitrate and ammonium hydroxide as precursor materials with suitable conditions. The X-ray diffraction pattern indicates the formation of cubic phase CeO₂. The average particle size of cerium oxide from high resolution transmission electron microscopy (HRTEM) was found to be 3 nm. The X-ray photoelectron (XPS) spectrum confirms the presence of Ce³⁺ in CeO₂. Optical studies by UV–vis spectroscopy for the synthesized CeO₂ nanoparticles exhibit a blue shift (E_g = 3.78 eV) with respect to the bulk material (E_g = 3.15 eV) due to quantum confined exciton absorption.     

Biopolymer-manganese oxide nanoflake nanocomposite films fabricated by electrostatic layer-by-layer assembly

Bio-nanocomposite films based on chitosan and manganese oxide nanoflake have been fabricated via the layer-by-layer (LBL) self-assembly technique. UV–vis absorption spectra showed that the subsequent growth of the nanocomposite film was regular and highly reproducible from layer to layer. X-ray photoelectron spectroscopy (XPS) spectra confirmed the incorporation of chitosan and manganese oxide nanoflake into the films. Scanning electron microscopy (SEM) images revealed that the nanocomposite film had a continuous surface and a layered structure. A sensitive hydrogen peroxide (H₂O₂) amperometric sensor was fabricated with the chitosan–manganese oxide nanoflake nanocompoite film. The sensor showed a rapid and linear response to H₂O₂ over the range from 2.5 × 10^? 6 to 1.05 × 10^? 3 M, with a sensitivity of 0.038 A M^? 1 cm^? 2.     

Nb2O5 hollow nanospheres as anode material for enhanced performance in lithium ion batteries

Nb₂O₅ hollow nanospheres of average diameter ca. ～29 nm and hollow cavity size ca. 17 nm were synthesized using polymeric micelles with core–shell–corona architecture under mild conditions. The hollow particles were thoroughly characterized by transmission electron microscope (TEM), X-ray diffraction (XRD), infrared spectroscopy (FTIR), thermal (TG/DTA) and nitrogen adsorption analyses. Thus obtained Nb₂O₅ hollow nanospheres were investigated as anode materials for lithium ion rechargeable batteries for the first time. The nanostructured electrode delivers high capacity of 172 mAh g^?1 after 250 cycles of charge/discharge at a rate of 0.5 C. More importantly, the hollow particles based electrodes maintains the structural integrity and excellent cycling stability even after exposing to high current density 6.25 A g^?1. The enhanced electrochemical behavior is ascribed to hollow cavity coupled with nanosized Nb₂O₅ shell domain that facilitates fast lithium intercalation/deintercalation kinetics.     

Facile synthesis,characterization and photocatalytic activity of niobium carbide

Niobium carbide (NbC) powders were prepared via a novel route at 550 °C and 8 h, using metallic magnesium powders, niobium pentoxide (Nb₂O₅), and potassium acetate (CH₃COOK) as starting materials. The structure and morphology of the product were characterized by X-ray powder diffraction (XRD) and scanning electron microscopy (SEM). The results indicated that as-prepared product was crystallized in pure cubic NbC phase and the size of the sample was estimated to be around 120 nm. The Rietveld refinement of the XRD data gives the cell constant a = 4.4718 Å. According to the Scherrer formula, the real grain size was about 70 nm. The BET surface area of the sample was ca.29.3 m²/g. The grain size distribution of the sample was about 467 nm, which was characterized by N4 PLUS submicron Particle Size Analyzer. The cubic NbC powders exhibited photocatalytic activity in degradation of Rhodamine-B (RhB) under 300 W mercury lamp light irradiation.     

Self-organized highly ordered TiO2 nanotubes in organic aqueous system

A simple method to achieve self-organized, freestanding TiO₂ nanotube array was constructed, free of corrosive etching process which was traditionally employed to separate TiO₂ nanotubes from the metallic Ti substrate. The TiO₂ nanotube arrays were constructed through potentiostatic anodization of Ti foil in aqueous electrolyte containing NH₄F and ethylene glycol. The nanotubes in the array were of 45 μm lengths and 100 nm average pore diameters. The effect of NH₄F concentration on the length of the self-organized nanotube arrays was investigated. Electrochemical and spectroscopic measurements showed that the as-prepared nanotubes possessed large surface areas, good uniformity, and were ready for enzyme immobilization. The as-prepared nanotube arrays were amorphous, but crystallized with annealing at elevated temperatures, as demonstrated by X-ray diffraction (XRD).     

Study of physical properties of cobalt oxide (Co3O4) nanocrystals

Cobalt oxide nanocrystals of size 10–15 nm have been prepared by a simple co-precipitation method. The structural investigations have been performed with X-ray diffraction and Transmission Electron Microscopy. Specific surface area of the nanocrystals is 77.5 × 10⁴ cm²/g which have been calculated by X-ray diffraction data. Optical properties are discussed with UV/visible spectroscopy which shows the multiple band gap energies 2.28 eV (O^? II → Co^II) and 1.57 eV (O^? II → Co^III) which suggest the possibility of degeneracy of the valence band. The magnetic behavior is investigated using Vibrating Sample Magnetometer. The Co₃O₄ nanocrystals possess paramagnetic character at room temperature.     

Comparative dielectric studies of nanostructured BaTiO3, CaCu3Ti4O12 and 0.5BaTiO3⋅ 0.5CaCu3Ti4O12 nano-composites synthesized by modified sol–gel and solid state methods

BaTiO₃ (BTO), CaCu₃Ti₄O₁₂ (CCTO) and 0.5BaTiO₃·0.5CaCu₃Ti₄O₁₂ (BTO–CCTO), as a new nano-composite ceramic, were successfully designed and fabricated by a semi-wet gel route and a modified solid state method. The dielectric properties of the BTO–CCTO ceramic were compared to those of the BTO and CCTO ceramics at lower sintering temperatures and durations. The X-ray diffraction analysis revealed that the BTO and CCTO ceramics form a single crystalline phase and the average crystalline sizes calculated from X-ray diffraction data were in the range of 40–65 nm. The particle sizes of the BTO, CCTO, and BTO–CCTO ceramics obtained from transmission electron microscopy images were in the ranges of 40–65 nm, 80–110 nm, and 70–95 nm, respectively. The phase composition and microstructure were studied by X-ray diffraction and scanning electron microscopy. The energy dispersive X-ray results demonstrated the purity and stoichiometry of the BTO–CCTO nano-composite. The grain sizes of the BTO, CCTO and BTO–CCTO ceramics were found to be in the ranges of 500 nm–1 μm, 4–24 μm, and 250 nm–4 μm, respectively. The AC conductivity as a function of frequency confirmed the semiconducting nature of all of the ceramics and obeyed the Jonscher's power law. The impedance spectrum measurement result showed that the CCTO ceramic possessed an exceptional grain boundary resistance, which supports the internal barrier layer capacitance (IBLC) mechanism present in this ceramic and is responsible for the high ε_r values.     

Synthesis and electrochemical properties of nanosized LiFeO2 particles with a layered rocksalt structure for lithium batteries

Layered rocksalt-type LiFeO₂ particles (O3-LiFeO₂) with average particle sizes of ca. 40 and 400 nm were synthesized by an ion exchange reaction from α-NaFeO₂ precursors. X-ray diffraction (XRD) patterns and scanning electron microscopy (SEM) images confirmed the formation of nanosized O3-LiFeO₂. 40-nm LiFeO₂ exhibited a higher discharge capacity (115 mAh g^?1) than 400-nm LiFeO₂ (80 mAh g^?1), and also had better rate characteristics. The downsizing effect and cation disorder between the lithium and iron layers may have improved the electrochemical activity of the LiFeO₂ particles. Transmission electron microscopy (TEM) observation indicated a phase transition from O3-LiFeO₂ to a cubic lattice system during the electrochemical process. The cubic lithium iron oxide exhibited stable electrochemical reactions based on the Fe²⁺/Fe³⁺ and Fe²⁺/Fe⁰ redox couples at voltages between 4.5 and 1.0 V. The discharge capacities of 40-nm LiFeO₂ were ca. 115, 210, and 390 mAh g^?1 under cutoff voltages of 4.5–2.0 V, 4.5–1.5 V, and 4.5–1.0 V, respectively.     

Rapid synthesis of cryptomelane-type manganese oxide under ultrasonic process

Cryptomelane-type manganese oxide (OMS-2) was rapidly prepared under ultrasonic irradiation in short time. Characterization results using X-ray powder diffraction (XRD), surface area analyzer, transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), oxygen temperature-programmed desorption (O₂-TPD) revealed that ultrasonic irradiation has tremendous effect on the surface area, morphology, surface defects, and redox properties of the OMS-2 materials. The OMS-2 prepared via ultrasonic irradiation shows nanoneedle morphology with smaller crystallite size, larger surface area (120.4 m²/g), more surface defects, and higher oxygen mobility, thus it demonstrates excellent activity in the catalytic combustion of dimethyl ether with a start-off temperature of 160 °C and a complete combustion temperature of 172 °C.     

Activated hydride-mediated solution phase synthesis of crystallized antimony(0) nanoparticles

This work presents a simple method to produce large quantities of crystallized antimony(0) nanoparticles through SbCl₃ chemical reduction using t-BuONa-activated sodium hydride. t-BuONa acts as a superficial stabilizer of Sb(0) nanoparticles inhibiting their growth and avoiding aggregation. The Sb(0) nanoparticles were characterized using transmission electron microscopy, XPS analysis and X-ray powder diffraction. Results obtained show that rhombohedral Sb(0) with diameters of ca. 4.7 ± 1.9 nm were produced. The influence of purification conditions on the aggregation state of Sb(0) particles is also described.     

Transparent with wide band gap InZnO nano thin film: Preparation and characterizations

Novel indium zinc oxide (InZnO) thin film of 100 nm thickness was prepared onto pre-cleaned glass plate by thermal evaporation technique from InZnO nanoparticles. The metal oxide (In–O and Zn–O) bond and In, Zn and O elements present in the films were confirmed by Fourier transform infrared spectroscopy and energy dispersive X-ray spectroscopy. The X-ray diffraction patterns revealed the mixed phase of cubic In₂O₃ and wurzite-hexagonal ZnO structure. SEM images showed smooth surface with uniform distribution of grains (201–240 nm) over the entire film surface. High transparency and low absorption obtained from optical study. The band gap energy was evaluated to be about 3.46–3.55 eV by Tauc’s plot. The structure, smooth surface and high transparency with wide band gap energy lead the thermally evaporated InZnO nano thin film to be used for transparent layer in optoelectronic devices in the future.     

Anionic surfactant-assisted hydrothermal synthesis of high-aspect-ratio ZnO nanowires and their photoluminescence property

ZnO nanowires with high-aspect-ratio of up to ca. 600 were synthesized in a quaternary reverse microemulsion containing sodium dodecyl sulfate (SDS) / water / heptane / n-hexane via a hydrothermal method. SDS, as an anionic surfactant, plays an important role in the formation of morphologies. Subsequently, we studied lots of key influencing factors including the molar ratio (w) value of NaOH to Zn(OAc)₂, the reaction temperature, and the instance without the quaternary reverse microemulsion. The selected-area electron diffraction (SAED) and high-resolution transmission electron microscopy (HRTEM) reveal the single-crystal nature of the ZnO nanowires. The morphologies and crystalline structure of the as-obtained products were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and powder X-ray diffraction (XRD), respectively. Through this route, we can obtain a mass of products and the method is both convenient and reproducible. Finally, we measured the photoluminescence (PL) spectra and found that the ZnO nanowires exhibited green-orange emission at 525 nm and short ultraviolet emission at 380 nm and the ZnO nanomaterials with different aspect ratio (length to diameter) (L / D) showed PL intensity disciplinary change. Aiming at this phenomenon, we propose a reasonable mechanism to explain the PL spectra of the ZnO nanomaterials in detail.     

Hydrothermal synthesis of single-crystal VO2(B) nanobelts

Single crystalline VO₂(B) nanobelts with a metastable structure were obtained through a simple hydrothermal synthetic method. The VO₂(B) nanobelts were characterized by means of X-ray diffraction, transmission electron microscopy, selected area electronic diffraction, field-emission scanning electron microscopy and X-ray energy-dispersive spectroscopy techniques. The as-obtained VO₂(B) nanobelts are 400–600 nm long, typically 100–150 nm wide and 20–30 nm thick. The belt-like VO₂(B) with a high surface area may be beneficial to lithium insertion between the VO₆ layers for application in batteries.     

Structure analysis of aluminium silicon manganese nitride precipitates formed in grain-oriented electrical steels

We report a detailed structural and chemical characterisation of aluminium silicon manganese nitrides that act as grain growth inhibitors in industrially processed grain-oriented (GO) electrical steels. The compounds are characterised using energy dispersive X-ray spectrometry (EDX) and energy filtered transmission electron microscopy (EFTEM), while their crystal structures are analysed using X-ray diffraction (XRD) and TEM in electron diffraction (ED), dark-field, high-resolution and automated crystallographic orientation mapping (ACOM) modes. The chemical bonding character is determined using electron energy loss spectroscopy (EELS). Despite the wide variation in composition, all the precipitates exhibit a hexagonal close-packed (h.c.p.) crystal structure and lattice parameters of aluminium nitride. The EDX measurement of ~ 900 stoichiometrically different precipitates indicates intermediate structures between pure aluminium nitride and pure silicon manganese nitride, with a constant Si/Mn atomic ratio of ~ 4. It is demonstrated that aluminium and silicon are interchangeably precipitated with the same local arrangement, while both Mn^2 + and Mn^3 + are incorporated in the h.c.p. silicon nitride interstitial sites. The oxidation of the silicon manganese nitrides most likely originates from the incorporation of oxygen during the decarburisation annealing process, thus creating extended planar defects such as stacking faults and inversion domain boundaries. The chemical composition of the inhibitors may be written as (AlN)_x(SiMn_0.25N_yO_z)_1 − x with x ranging from 0 to 1.     

Sol–gel synthesis and characterization of mesoporous manganese oxide

Mesoporous manganese oxide (MPMO) from reduction of KMnO₄ with maleic acid, was obtained and characterized in detail. The characterization of the material was confirmed by high-resolution transmission electron microscopy (HRTEM), X-ray powder diffractometry (XRD) and N₂ sorptometry. The results showed that MPMO is a pseudo-crystalline material with complex network pore structure, of which BET specific surface area is 297 m²/g and pore size distribution is approximately in the range of 0.7–6.0 nm. The MPMO material turns to cryptomelane when the calcinating temperature rises to 400 °C. The optimum sol–gel reaction conditions are KMnO₄/C₄H₄O₄ molar ratio=3, pH=7 and gelation time>6 h.     

Biologically formed hollow cuprous oxide microspheres

Hollow cuprous oxide (Cu₂O) microspheres with a diameter of ca. 1.8 μm are prepared by using yeast as template. The possible mechanism for the formation of the hollow Cu₂O spheres is revealed. The biotemplated sample is investigated by means of X-ray diffraction (XRD), scanning electron microscopy (SEM) and ultraviolet–visible (UV–vis) absorption spectra. The sample consists of the crystalline Cu₂O microspheres with diameters of about 59.5 nm and lattice parameter of 4.264 Å. The observed optical band gap of the product indicates that the blue–shift effect occurs, which is attributed to the hollow Cu₂O microspheres.