Synthesis and characterization of electrochemically-reduced graphene

Graphene has superior electrical conductivity than graphite and other allotropes of carbon because of its high surface area and chemical tolerance. Electrochemically processed graphene sheets were obtained through the reduction of graphene oxide from hydrazine hydrate. The prepared samples were heated to different temperatures such as 673 and 873 K. X-ray diffraction (XRD), fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDXS), transmission electron microscopy (TEM), Raman spectra and conductivity measurements were made for as-prepared and heat-treated graphene samples. XRD pattern of graphene shows a sharp and intensive peak centred at a diffraction angle (2θ) of 26·350. FTIR spectra of as-prepared and heated graphene were used to confirm the oxidation of graphite. TEM results indicated that the defect density and number of layers of graphene sheets were varied with heating temperature. The hexagonal sheet morphology and purity of as-prepared and heat treated samples were confirmed by SEM–EDX and Raman spectroscopy. The conductivity measurements revealed that the conductivity of graphene was decreased with an increase in heating temperature. The present study explains that graphene with enhanced functional properties can be achieved from the as-prepared sample.     

Synthesis and structural studies on Ni0.5+x Zn0.5Cu x Fe2−2x O4

The mixed ferrites of Ni–Zn–Cu are synthesized using ceramic double sintering technique. Cu and Ni are substituted in steps of x=0.1 at the interstitial sites of Fe. Powders of mixed ferrites of Ni–Zn–Cu are studied using XRD. The mixed ferrites show a single phase and face center cubic structure for all concentrations. The substitution of Cu and Ni are confirmed from the variation of lattice constant. The cation distribution in the A and B sites of the ferrites is estimated. Mixed ferrites of Ni–Zn–Cu are characterized using a.c. conductivity and magnetic susceptibility methods. The variation of activation energy, magnetic moment and Curie temperature with concentration of Fe ions explains the alterations of the energy levels of d bands. Hopping of charge carriers and the presence of different ionic states of Ni, Cu, and Fe ions are discussed using the FTIR and EPR spectra.     

Gas sensing study of hydrothermal reflux synthesized NiO/graphene foam electrode for CO sensing

Nickel oxide nanosheets have been successfully synthesized on the graphene foam (GF) using hydrothermal reflux process for their application as carbon monoxide (CO) gas sensor. X-ray diffraction (XRD), scanning electron microscopy (SEM), Raman spectroscopy, energy dispersive spectroscopy, and gas sorption analysis were used to characterize the structure and morphology of the samples. The morphology (SEM), crystal structure (XRD and Raman), and elemental composition (EDS) analysis of NiO/GF composite confirmed the cubic crystal structure of NiO and elemental composition (i.e., Ni, O, and C) of NiO/GF composite. The results reveal that the incorporation of graphene into NiO nanosheets not only improved the surface area of NiO/GF composite, but also enhanced the performance of the composite on CO sensing by improving its conductivity. These results indicate that NiO/GF has potential as electrode material for CO gas sensor.     

Combustion synthesis of CuFe2O4

Metallic ferrites are investigated as prospective materials for different applications especially as anodes in extractive metallurgy. CuFe₂O₄, one of the important ferrites, is envisaged for substituting the carbon anode in Hall-Heroult cells. A single step combustion process has been used for the synthesis of CuFe₂O₄ powder from cupric nitrate, ferric nitrate and urea. The experimental conditions for maximum conversion efficiency of the precursor powders have been optimized. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM) have confirmed the formation, structure and homogeneity of the as-prepared powders. The detailed physical, electrical and structural characterization of the materials have been carried out for the specimens obtained on sintering at different temperatures up to 1000 °C.     

Characterization and temperature-dependent conductivity of polyaniline nanocomposites encapsulating gold nanoparticles on the surface of carboxymethyl cellulose

Polyaniline nanocomposites encapsulating gold nanoparticles on carboxymethyl cellulose surface were prepared via the polymerization of aniline hydrochloride with different carboxymethyl cellulose (CMC) concentrations (wt.%) using HAuCl₄ as oxidant. The synthesized composites were characterized by Fourier transform infrared (FTIR) spectroscopy. Surface morphology was studied by electron diffraction scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The embedded crystallinity of the composites was investigated by X-ray diffraction (XRD) analyses. The electrical property of the composites was examined by temperature-dependent DC conductivity in the range of 300–500 K. The composites exhibited higher electrical conductivities with increased CMC concentration under equivalent conditions. Activation energy for electron transport was also calculated based on the conductivity data.     

Polyaniline–CdS nanocomposites: effect of camphor sulfonic acid doping on structural, microstructural, optical and electrical properties

Nanocomposites of CdS nanocrystals with conducting polyaniline doped with camphor sulfonic acid (CSA) have been prepared by spin coating technique and investigated by X-ray diffraction, field emission scanning electron microscopy (FESEM), fourier transform infra red spectroscopy (FTIR), UV–visible spectroscopy and electrical transport method. The X-ray diffraction patterns showed broad peaks due to formation of nanoparticles of CdS in polyaniline matrix. FESEM showed that the transformation of morphology from agglomeration to nanopetals. The FTIR spectra confirmed the interaction between CSA and polyaniline (PANi)–CdS nanocomposite. The UV–visible spectrums revealed the enhancement of doping level for the PANi–CdS nanocomposites which is assigned to the existence of greater number of charges on the polymer backbone. DC electrical conductivity studies showed an increase in conductivity of PANi–CdS nanocomposites from 6.9?×?10^?6 to 3.14?×?10^?4 due to addition of CSA (10–50?%).     

Temperature dependent electrical properties of co-precipitated magnesium doped lithium nanoferrites

Due to a number of unique properties, nanoferrites are considered among the most emerging materials for the manufacturing of microwave devices. In past few years, different elemental compositions of nanoferrites were fabricated for this purpose. In our work, magnesium-doped lithium ferrites (Li_2?xMg_xFe₂O_4.5?δ, where x = 0.0 to 1.0) were synthesized by using co-precipitation method in optimized conditions. Structural analysis was done by using X-ray diffraction (XRD); this data was further used to calculate the porosity, phase purity and crystallite size. The XRD results confirmed the formation of spinel structure for all the samples. The surface morphology of the prepared samples was examined by using scanning electron microscope that showed particle like morphology. Thermogravimetric analysis and differential scanning calorimetry were used to investigate the phase transition and melting point of the prepared samples respectively. The analysis showed the phase transitions at two temperature ranges and the melting point of the all the samples was above 900 °C except for composition x = 0.4. Dielectric loss, dielectric constant, AC electrical conductivity and DC electrical resistivity were studied as a function of temperature. Curie temperature was also estimated from the temperature dependent conductivity data and that were observed to be decreased with increase in Mg concentration. The result obtained from the electrical analysis of the prepared samples confirmed that they could be used in frequency dependent devices.     

Synthesis and characterization of CdS doped TiO2 nanocrystalline powder: A spectroscopic study

This report aimed to study the effect of CdS doping in TiO₂ on the phase transformation of TiO₂ from anatase to rutile using X-ray diffraction (XRD) and Raman spectroscopy. CdS-doped TiO₂ nanocomposites have been prepared and characterized using Fourier transform infrared spectroscopy (FTIR) and transmission electron microscopy (TEM). We have observed that contrary to bare TiO₂, phase transformation of TiO₂ from anatase to rutile is hindered when doped with CdS at high temperature. Raman spectroscopy is found to be more sensitive for detection of the surface of TiO₂ as compared to XRD.     

Structural,optical and morphological studies of undoped and Zn-doped CdSe QDs via aqueous route synthesis

Undoped and Zn-doped CdSe quantum dots (QDs) were successfully synthesized by the chemical precipitation method. The structural, optical and morphological properties of the synthesized undoped and Zn-doped CdSe QDs were studied by X-ray diffraction (XRD), UV–visible absorption spectroscopy, photoluminescence (PL) spectroscopy, fluorescence lifetime spectroscopy, scanning electron microscopy (SEM), field emission transmission electron microscopy (FE-TEM) and FTIR. The synthesized undoped and Zn-doped CdSe QDs were in cubic crystalline phase, which was confirmed by the XRD technique. From the UV–visible absorption spectral analysis, the absorption wavelengths of both undoped and Zn-doped CdSe QDs show blue-shift with respect to their bulk counterpart as a result of quantum confinement effect. The highest luminescence intensity was observed for CdSe QDs doped with 4% Zn by PL studies. TEM analysis shows that the prepared QDs are spherical in shape.     

水热条件下氮化硼枝蔓晶的形成

利用水热方法合成了氮化硼枝蔓晶,根据X射线衍射(XRD),傅立叶红外吸收(FTIR)测试确定了产物的物相组成,X射线能谱仪(XPS)也证明了枝蔓晶的立方氮化硼成分,同时,利用透射电镜(TEM)和选取电子衍射(SAED)的测试结果分析了枝蔓晶的形貌和表面特征,另外,本文结合负离子配位多面体理论探讨了枝蔓晶的形成机理.     

Electrocatalytic behavior of calcium doped LaFeO3 as cathode material for solid oxide fuel cell

La(1-x)Ca(x)FeO3 (X = 0.0, 0.2, 0.4, abbreviated as LCF) as cathode material for intermediate temperature solid oxide fuel cells (IT-SOFC) was synthesized by new route of glycine nitrate method. LCF materials were characterized by X-ray diffraction (XRD), scanning electron microscopy-energy-dispersive X-ray spectroscopy (SEM-EDX), transmission electron microscopy (TEM), electrical and electrochemical impedance spectroscopy (EIS). The powder LCFs exhibited single phase with orthorhombic structure, highly porous and small nanoparticles with average size of 200-300 nm. The electrical conductivities of LCFs increased as increasing the Ca content and achieved the maximum electrical conductivity of 148 Scm(-1) for La0.6Ca0.4FeO3 (X = 0.4) at 550 degrees C. The improved conductivity of LCFs could be a promising cathode material for IT-SOFCs. In the impedance analysis of fabricated symmetry cell with the optimized La0.6Ca0.4FeO3 cathode and Ce0.8Sm0.2O3 (SDC) electrolyte, the minimum area specific resistance (ASR) of 0.15 omegacm2 was observed at 850 degrees C, which may due to the lowest activation energy (1.55 eV), resulting from the reduction of oxygen molecules into oxygen ions. It was found that calcium doping was essential to increase the charge carrier concentration of lanthanum iron oxide materials, resulting in the high conductivity at intermediate temperature.     

Synthesis of cadmium titanate powders by a sol-gel-hydrothermal method

Cadmium titanate (CdTiO₃) powders have been synthesized by a sol-gel-hydrothermal method at 200°C. The as-synthesized powders were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), Raman spectroscopy, and thermo-gravimetric and differential thermal analysis (TG-DTA). The results indicate that the as-obtained powders are ilmenite phase CdTiO₃ with rhombohedral structure. This phase changes to orthorhombic perovskite phase upon annealing at about 1050°C.     

球状纳米二氧化钛/石墨烯复合材料的合成及导电性能

采用改进的水热法制备二氧化钛/石墨烯(TiO2/G)复合导电材料,并研究水热温度以及石墨烯用量对TiO2/G复合材料导电性的影响。利用傅里叶变换红外(FTIR)光谱、X射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)和电化学阻抗谱等测试手段对复合材料的结构,微观形貌以及导电性能进行表征,并确定最佳的水热温度以及石墨烯的最佳添加量。结果表明:石墨烯添加量为5%(质量分数),水热温度为160℃,TiO2/G复合材料的导电性最佳,其电阻率为13.46Ω·cm。复合材料中TiO2纳米颗粒为球状的锐钛矿相,直径为100~200nm左右,且均匀生长在石墨烯片层表面。其中,TiO2纳米颗粒生长于石墨烯片层上,有效地阻止石墨烯片层的聚集,有利于石墨烯片层间形成导电网络,提高电子迁移效率,赋予二氧化钛复合材料优异的导电性能。     

Transparent conductive film fabrication using intercalating silver nanoparticles within carbon nanotube layers

Carbon nanotubes have received attention as alternative materials to indium tin oxide for application in transparent conductive films. Their electrical conductivity, however, still has to be improved. In this study, a layer-by-layer self-assembly process was demonstrated using nano-silver-coated carbon nanotubes, which help improve electrical conductivity. The method was based on the pi-pi interaction between the side walls of the carbon nanotubes and nano-silver clusters that were functionalized with benzyl mercaptan. The self-assembled nano-silver cluster monolayer on the surface of the nanotubes can reduce the interfacial contact resistance, thereby leading to high conductivity at a high transparency. The compound was characterized via scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), Raman spectroscopy, and the four-point probe method.     

Structural,electrical, and magnetic properties of erbium (Er3+) substituted Cu–Cd nano-ferrites

In the present work, we reported the structural, electrical, and magnetic properties of erbium Er³⁺-substituted Cu–Cd nano-ferrites with generalized formula Cu_0.8Cd_0.2Er_xFe_2?xO₄ (where x?=?0.000, 0.0010, 0.0015, 0.002, 0.0025, 0.003), as synthesized by the Citrate-Gel Auto-Combustion. The X-ray diffraction (XRD) and scanning electron microscopy (SEM) studies were carried out to investigate their microstructural and surface morphology. The XRD measurements confirm pure cubic spinel phase composition of these nanoparticles. The crystallite size ranges over 9.22–19.22 nm and it reduces with the increase in erbium Er³⁺ concentration from 0.000 to 0.003. The vibration properties were carried out by using FTIR spectrometer. The two probe measurements were used to determine DC resistivity, Curie temperature, and DC conductivity. The plot between DC electrical resistivity and temperature indicates the semiconductor behavior. At room temperature, the vibrating sample magnetometer (VSM) was used to investigate magnetic properties, and the observed values revealed the ferrimagnetic behavior with high saturation magnetization (34.24 emu/g) and high coercivity (1121.70 Oe).

     

Synthesis of tin oxide-coated gold nanostars and evaluation of their surface-enhanced Raman scattering activities

Tin oxide-coated gold nanostar hybrid nanostructures are prepared by first synthesizing gold nanostars (ca. 400 nm), then introducing Na₂SnO₃ precursor followed by its hydrolysis and formation of a tin oxide layer on nanoparticle surface. The synthesized hybrid structures have been characterized by combination of UV–Vis spectroscopy, transmission electron microscope (TEM), energy-dispersive X-ray studies, scanning electron microscope (SEM), X-Ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy. The TEM and SEM analyses showed that gold nanostars have a coating with an approximate thickness of 15 nm. The tin (IV) oxide coating on the gold nanostars was identified by XRD and XPS analyses and confirmed by FTIR spectroscopy. Surface-enhanced Raman scattering (SERS) spectroscopy was performed on tin oxide-coated and uncoated gold nanostars with crystal violet as a probe molecule. The SERS studies revealed field enhancement properties of Au nanostars, thus their strong SERS activity remained after tin oxide coating.     

pH-dependant structural and morphology evolution of Ni(OH)2 nanostructures and their morphology retention upon thermal annealing to NiO

Nickel hydroxide nanosheets, nanobelts and nanorods were prepared by hydrothermal treatment of the precipitates obtained at different pH values. The morphology and crystal structure of the products could be controlled simply by adjusting the pH value at precipitation. Interconnected nanosheets of hexagonal β-Ni(OH)₂ with thickness around 10–20 nm were formed at pH ∼ 11, whereas nanobelts with typical widths around 40–80 nm, and nanorods with diameters around 50–60 nm of phase pure α-Ni(OH)₂ containing intercalated sulphate ions were obtained in the pH range ∼9.5–8.5. Thermal annealing of the hydroxides at 500 °C yielded cubic phase NiO with morphologies similar to their hydroxide precursors. X-ray powder diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), and energy dispersive X-ray (EDX) analysis were used to characterize the as-prepared products. The role of pH in controlling the phase and morphology of the products was discussed.     

Novel Nanostructured MnO_2 Prepared by Pulse Electrodeposition:Characterization and Electrokinetics

Pulse current technique was applied for the preparation of novel electroactive manganese dioxide and possible influences of different electrokinetic phenomena on material characteristics were discussed. The characterizations of pulse deposited sample （pcMD） were carried out by different techniques： Fourier transform infrared spectroscopy （FTIR）, scanning electron microscopy （SEM）, X-ray diffraction （XRD）, Brunauer-Emmett-Teller （BET） method, Raman spectroscopy, and atomic force microscopy （AFM）. SEM image revealed that pulse current could improve the current distribution. This was confirmed by AFM images showing a decrease in surface roughness of pcMDs in comparison to amorphous samples, which were deposited by direct current （dcMD）. Higher distortion of MnO6 octahedral environment of dcMD was detected by FTJR and Raman spectroscopy. Cyclic voltammetric （CV） measurements showed a generally higher energy level drained from the second electron discharge of pcMD. This is mainly attributed to a higher surface area and a lower diffusion pass of electrons and protons arisen via a rather unique nanostructural arrangement of pcMD grains. Results indicate a higher surface area available for the non homogenous second electron discharge of pcMD grains.     

Electrical properties of NiO films obtained by high-temperature oxidation of nickel

Nickel oxide thin films are formed by high-temperature oxidation of nickel foils at 973 K, and are characterized using X-ray diffraction and scanning electron microscopy indicating the formation of a single NiO phase whose thickness grows following a parabolic law. The electrical properties of the formed films are examined by impedance spectroscopy at room temperature; and by measuring direct current (DC) and alternating current (AC) conductivities and dielectric properties at different temperatures. At room temperature, the conductivity is about 4 orders of magnitude higher than that of NiO single crystals. Below 200 K, DC conductivity displays a slight increase with increasing temperature indicating conduction by thermal activation hopping of small polarons. Above 250 K, large polaron conduction associated with holes in the 2p band of O²⁻ with activation energy of about 0.4 eV is observed. Frequency as well as temperature dependencies of the AC conductivity and dielectric constant exhibit trends usually observed in carrier dominated dielectrics.