硬币状氧化镍的制备及其电化学性能研究

通过均匀沉淀法,以氨水作为络合剂,制备了β-氢氧化镍,经450℃煅烧处理得到纳米氧化镍,通过充放电测试和循环伏安测试研究了该产物作为锂离子电池负极材料的电化学性能.XRD、IR表明,反应产物为纯相,SEM和TEM表明,产物形貌为硬币状的特殊形貌.在放电电位区间0.01～3.0 V vs Li/Li＋,0.2C倍率下充放电,初始容量1 050 mAh/g,第2次容量损失35.8％,50次循环后,质量比容量为355 mAh/g,硬币状纳米氧化镍其特殊的形貌具有较大的比表面积,增加了电化学活性点,降低了界面反应的极化,从而提高了NiO电极的电化学性能.     

Morphological variations in cadmium sulfide nanocrystals without phase transformation

A very novel phenomenon of morphological variations of cadmium sulfide (CdS) nanorods under the transmission electron microscopy (TEM) beam was observed without structural phase transformation. Environmentally stable and highly crystalline CdS nanorods have been obtained via a chemical bath method. The energy of the TEM beam is believed to have a significant influence on CdS nanorods and may melt and transform them into smaller nanowires. Morphological variations without structural phase transformation are confirmed by recording selected area electron diffraction at various stages. The prepared CdS nanorods have been characterized by X-ray powder diffraction, TEM, UV-Vis spectroscopy, and photoluminescence spectroscopy. The importance of this phenomenon is vital for the potential application for CdS such as smart materials.     

Sonochemical preparation of palygorskite nanoparticles

Palygorskite nanoparticles were prepared by sonochemical reaction. The products were characterized by X-ray fluorescence analysis (XRF), X-ray powder diffraction (XRD), thermal gravimetry analysis (TGA), differential thermal analysis (DTA) and infrared spectroscopy. The morphology and size of the nanorods were observed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM).     

Preparation and properties of Co<Subscript>3</Subscript>O<Subscript>4</Subscript> nanorods as supercapacitor material

Co₃O₄ nanorods have been successfully synthesized by thermal decomposition of the precursor prepared via a facile and efficient microwave-assisted hydrothermal method, using cetyltrimethylammonium bromide (CTAB) with ordered chain structures as soft template for the first time. The obtained Co₃O₄ was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and electrochemical measurements. The results demonstrate that the as-synthesized nanorods are single crystalline with an average diameter of about 20 to 50 nm and length up to several micrometers. Preliminary electrochemical studies, including cyclic voltammetry (CV), galvanostatic charge–discharge, and electrochemical impedance spectroscopy (EIS) measurements, are carried out in 6 M KOH electrolyte. Specific capacitance of 456 F g⁻¹ for a single electrode could be achieved even after 500 cycles, suggesting its potential application in electrochemical capacitors. This promising method could provide a universal green chemistry approach to synthesize other low-cost and environmentally friendly transition metal hydroxide or oxide.     

水热法制备氧化钴/泡沫镍材料及电容性能分析

利用简单的水热法制备出不同反应液浓度、不同反应时间以及不同反应温度氧化钴/泡沫镍（CoO/NF）电极，旨在改善氧化钴材料的比电容及稳定性。通过XRD、SEM、TEM、EDS Mapping和BET对其结构和形貌进行了表征，同时在1mol/L氢氧化钾（KOH）电解液中采用循环伏安曲线（CV）、充放电曲线（CP）、循环性能测试、大电流充放电测试以及交流阻抗（EIS）测试研究了其电化学性能。表征结果显示氧化钴均匀地分布在泡沫镍载体表面，且片状结构CoO-8h/NF具有较大的比表面积和多孔特性。在三电极体系中，电化学测试结果显示CoO-8h/NF在1mA/cm²电流密度下表现出最好的电容性能，比电容可以达到930mF/cm²。在10mA/cm²电流密度下对CoO-8h/NF电极进行10000次恒电流充放电测试，循环测试后电极的比电容几乎没有衰减，具有较好的稳定性，是超级电容器比较理想的正极材料。     

Expanded graphite as a support for Ni/carbon composites

Expanded graphite decorated with nickel oxide particles (EG_NiO) has been synthesized through electrochemical oxidation of natural graphite in an aqueous nickel nitrate solution followed by a heat treatment. EG_NiO was used to prepare nickel/carbon composites using two techniques: (a) hydrogen reduction of nickel oxide particles loaded on the expanded graphite surface and (b) pyrolysis of coal tar pitch-impregnated EG_NiO blocks. The EG_NiO as well as the nickel/carbon composites have been characterized by X-ray diffraction, scanning and transmission electron microscopy, energy dispersive X-ray spectroscopy and selected area electron diffraction.     

Hot pressing sintering of zinc sulfide microsphere decorated with nanorods synthesized by the simple refluxing method

A zinc sulfide microsphere decorated with nanorods was synthesized using the refluxing method. Then, the as-obtained ZnS nanostructures were consolidated via the hot pressing (HP) technique. X-ray diffraction, Fourier transforms infrared spectroscopy, high-resolution transmission electron microscopy, field emission scanning electron microscopy (FESEM), diffuse reflectance spectroscopy, and X-ray mapping analyzes were used to characterize the ZnS sample. The effects of various factors such as pH, temperature, and reaction time were investigated on the morphology and particle size of ZnS nanostructures. The formation of sphalerite phase of ZnS nanoparticles was confirmed by the XRD analysis. FESEM also revealed that ZnS nanostructures with the molar ratio 1:1.3 (zinc: sulfur) had a spherical morphology decorated with sulfur nanorods. The ZnS nanostructures were consolidated by hot pressing technique at 860 °C for 2h under vacuum atmosphere. XRD analysis indicated that the sintered ceramic had a sphalerite phase. FESEM study demonstrated that ZnS ceramic had a grain size diameter within the range of 1–3 μm.     

Tungsten Oxide Nanorods Array and Nanobundle Prepared by Using Chemical Vapor Deposition Technique

Tungsten oxide (WO₃) nanorods array prepared using chemical vapor deposition techniques was studied. The influence of oxygen gas concentration on the nanoscale tungsten oxide structure was observed; it was responsible for the stoichiometric and morphology variation from nanoscale particle to nanorods array. Experimental results also indicated that the deposition temperature was highly related to the morphology; the chemical structure, however, was stable. The evolution of the crystalline structure and surface morphology was analyzed by scanning electron microscopy, Raman spectra and X-ray diffraction approaches. The stoichiometric variation was indicated by energy dispersive X-ray spectroscopy and X-ray photoelectron spectroscopy.     

Acceleration and quantitative evaluation of degradation for corrosion protective coatings on buried pipeline: Part II. Application to the evaluation of polyethylene and coal-tar enamel coatings

The pulsed potentiostatic polarization technique proposed previously has been applied to evaluate the electrochemical degradation of polyethylene and coal-tar enamel coated SS400 for buried pipeline. The degradation of coated systems was accelerated and evaluated using electrochemical techniques (pulsed potentiostatic polarization test, electrochemical impedance spectroscopy) and surface analyses (scanning electron microscopy and energy dispersive X-ray spectroscopy). It was found that polyethylene coating had better protective performance than coal-tar enamel coating due to its low porosity. It was confirmed that the electrochemically accelerated test is an effective technique in the evaluation of coating performance.     

Synthesis and optical property of one-dimensional spinel ZnMn<Subscript>2</Subscript>O<Subscript>4</Subscript> nanorods

Spinel zinc manganese oxide (ZnMn₂O₄) nanorods were successfully prepared using the previously synthesized α-MnO₂ nanorods by a hydrothermal method as template. The nanorods were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, UV-Vis absorption, X-ray photoelectron spectroscopy, surface photovoltage spectroscopy, and Fourier transform infrared spectroscopy. The ZnMn₂O₄ nanorods in well-formed crystallinity and phase purity appeared with the width in 50-100 nm and the length in 1.5-2 μm. They exhibited strong absorption below 500 nm with the threshold edges around 700 nm. A significant photovoltage response in the region below 400 nm could be observed for the nanorods calcined at 650 and 800°C.     

Hierarchical NiO nanoflake coated CuO flower core–shell nanostructures for supercapacitor

In this work, we developed a simple and cost-effective approach to prepare the hierarchical NiO/CuO nanocomposite without any surfactant. The morphology and structure of the hybrid nanostructure was examined by focus ion beam scanning electron microscopy (FIB/SEM), X-ray diffraction spectroscopy (XRD) and high-resolution transmission electron microscopy (HRTEM). Furthermore, the electrochemical properties of the hierarchical NiO/CuO nanocomposite electrodes were elucidated by cyclic voltammograms, galvanostatic charge/discharge tests and electrochemical impedance spectroscopy in 6 M KOH electrolyte. The electrochemical results demonstrated that this unique NiO/CuO nanostructure exhibited a specific capacitance of 280 F g⁻¹ and excellent cycling stability (91.4% retention after 3000 cycles). The remarkable electrochemical performance coupled with the facile synthesis of the hierarchical NiO/CuO nanocomposite indicated the great application potential in supercapacitors.     

Controllable electrochemical synthesis of La/ZnO hierarchical nanostructures and their optical and magnetic properties

Here we presented a facile electrochemical deposition route for the controllable preparation of La³⁺/ZnO hierarchical nanostructures, such as flower-like nanostructures consisted of nanorods, flower bundles, and hexagonal nanorods with nests at the top. These prepared La³⁺/ZnO deposits were characterized by scanning electron microscopy, transmission electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, UV-vis spectrophotometer, and photoluminescence spectroscopy. The formation process of La³⁺-doped ZnO and the growth mechanisms of La³⁺/ZnO hierarchical nanostructures were discussed. The UV and PL spectra measurements show that the surface morphologies of La³⁺/ZnO deposits have an obvious effect on their optical properties and we can easily adjust their optical properties as well as La³⁺/ZnO nanostructures by changing electrochemical deposition parameters. In addition, the magnetic properties of La³⁺/ZnO deposits were also investigated.     

Graphene nanoplate-MnO2 composites for supercapacitors: a controllable oxidation approach

Graphene nanoplate-MnO(2) composites have been synthesized by oxidising part of the carbon atoms in the framework of graphene nanoplates at ambient temperature. The composites were characterized by means of X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and cyclic voltammetry (CV). It was found that the oxidation extent of the carbon atoms in the graphene framework in these composites was dependent on the reaction time, which also influenced their microstructure, morphology and electrochemical properties. Compared with MnO(2) nanolamellas, the nanocomposite prepared with a reaction time of 3 h reveals better electrochemical properties as a supercapacitor electrode material.     

石墨烯/二氧化锰复合材料的制备与电化学性能

通过改性二氧化锰和氧化石墨烯片之间的静电自组装制备了层状的rGO/MnO2复合纳米材料。通过XRD分析材料的晶体结构,用扫描电镜观察材料的微观表面形貌。这种材料用来研究其电化学电容性能,结果表明这种纳米复合材料显示出很好的电容性能(在0.2 A/g的电流密度下可达246 F/g)。此外,在2 A/g的电流密度下循环1000次后容量保持率为91%。材料的性能提升是因为复合材料中二氧化锰纳米棒和石墨烯片层很好的贴合,而石墨烯片的加入也大大提高了材料的导电性。     

Synthesis and characterization studies of NiO nanorods for enhancing solar cell efficiency using photon upconversion materials

We report the effect of calcination on the structural and optical properties of nanocrystalline NiO nanoparticles were successfully synthesized by virtue of a single source precursor method at mild reaction conditions between nickel nitrate and sodium hydroxide. Composition, structure and morphology of the products were analyzed and characterized by X-ray powder diffraction (XRD). The ultra-violet visible (UV–vis) absorption peaks of NiO exhibited a large blue shift and the luminescent spectra had a strong and broad emission band centered at 328 nm. The intense band gap was also observed, with some spectral tuning, to give a range of absorption energies from 2.60 to 3.41 eV. The various functional groups present in the NiO nanorods were identified by FTIR analysis. High resolution transmission electron microscopy (HRTEM) and the chemical composition of the samples the valence states of elements were determined by X-ray photoelectron spectroscopy (XPS) in detail. The electrochemical response of NiO proved that the nano-nickel has a high level of functionality due to its small size and higher electrochemical activity without any modifications. The above studies demonstrate the potential for the utilization of NiO nanoparticles as a promising material for opto-electronics applications.     

Microwave combustion synthesis,magneto-optical and electrochemical properties of NiMoO4 nanoparticles for supercapacitor application

Nickel molybdate (NiMoO₄) nanoparticles (NPs) were synthesized by a simplistic one-pot microwave combustion method using urea as the fuel. The produced NPs have been examined by powder X-ray diffraction (XRD), Fourier transform infrared (FT-IR) analysis, scanning electron microscope (SEM), energy dispersive X-ray (EDX), high-resolution transmission electron microscopy (HR-TEM) analysis. Further, optical and electronic properties were determined by UV-Visible and Photoluminescence (PL) analysis, respectively. The magnetic performance of the NiMoO₄ NPs was investigated by vibrating sample magnetometer (VSM) and the surface chemical composition was identified by X-ray photoelectron spectroscopy (XPS). The electrochemical activities of the NiMoO₄ NPs were studied by cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and galvanostatic charge/discharge (GCD) analysis. From the results, the CV curves indicated the occurrence of redox couples and besides with the EIS data (Nyquist plot), confirmed the supercapacitor nature of the synthesized NiMoO₄. The prepared NiMoO₄ exhibits a high specific capacitance and rateability. This electrode grants a high specific capacitance of 450?F?g^?1 at 2?mA?cm^?2 and the well permanency with a cycling proficiency of 94% after 1000 cycles. These results clearly showed that the synthesized NiMoO₄ NPs have potential application for the forthcoming flexible and lightweight energy storage.     

CuInSe2 films prepared by three step pulsed electrodeposition. Deposition mechanisms, optical and photoelectrochemical studies

p-Type semiconducting copper indium diselenide thin films have been prepared onto In₂O₃:Sn substrates by a recently developed pulse electrodeposition method that consists in repeated cycles of three potential application steps. The Cu–In–Se electrochemical system and the related single component electrolytes were studied by cyclic voltammetry to identify the electrode processes and study the deposition processes. In situ atomic force microscopy measurements during the first 100 deposition cycles denote a continuous nucleation and growth mechanism. Particles removed by film sonication from some of the films were characterized by transmission electron microscopy and determined to consist in nanoscopic and crystalline CuInSe₂. The remaining film is still crystalline CuInSe₂, as assessed by X-ray diffraction.The chemical characterization by combined X-ray photoelectron spectroscopy, X-ray fluorescence and inductively coupled plasma optical emission spectroscopy, showed that films were Cu-poor and Se-poor. Raman characterization of the as-grown films showed that film composition varies with film thickness; thinner films are Se-rich, while thicker ones have an increased Cu–Se content. Different optical absorption bands were identified by the analysis of the UV–NIR transmittance spectra that were related with the presence of CuInSe₂, ordered vacancy compounds, Se, Cu_2−xSe and In₂Se₃. The photoelectrochemical activity confirmed the p-type character and showed a better response for the films prepared with the pulse method.     

ZnSe纳米棒的水热法合成及发光性能研究

以氢氧化钠、单质硒粉与4种不同锌盐为起始原料、EDTA为软模板剂,在190℃水热条件下合成了ZnSe半导体材料。采用X-射线粉末衍射(XRD)、扫描电镜(SEM)、X-射线光电子能谱(XPS)、荧光光谱(FS)、紫外可见吸收光谱(UV-Vis)等测试手段对所得样品的物相结构、化学组成、形貌和性能进行了测试。结果表明,所得ZnSe为立方闪锌矿型结构且纯度较高;锌源对产物的形貌具有一定的影响;合成的粉体在紫外区有强的吸收峰,具有良好的光学性能。     

Effect of nickel content on the electrochemical behavior of Cu-Al-Ni alloys in chloride free neutral solutions

The electrochemical behavior of Cu-Al-Ni alloys in chloride free neutral solutions was investigated. The effect of Ni content on the corrosion resistance of the alloys was examined and evaluated. Conventional electrochemical techniques and electrochemical impedance spectroscopy, EIS, have been used. Potentiodynamic measurements revealed that the increase in the Ni content decreases the stability of the Cu-Al-Ni alloys. The polarization measurements were confirmed by EIS experiments. The morphology of the alloy surface was investigated by scanning electron microscopy, SEM, and surface analysis was made by energy dispersive X-ray technique. The experimental impedance data were fitted to theoretical data according to a proposed equivalent circuit model representing the electrode/electrolyte interface. The results of these experiments are discussed in reference to the potential-pH (Pourbaix) diagrams of the alloying elements.     

Design and synthesis of three-dimensional needle-like CoNi2S4/CNT/graphene nanocomposite with improved electrochemical properties

In this paper, we described a simple two–step method for preparing needle-like CoNi₂S₄/CNT/graphene nanocomposite with robust connection among its ternary components. The prepared CoNi₂S₄/CNT/graphene nanocomposite has been thoroughly characterized by spectroscopic (Fourier-transform infrared spectroscopy, Raman spectroscopy, X-ray photoelectron spectroscopy), X-ray diffraction and thermogravimetric analysis. Microscopy techniques (scanning electron microscopy–energy dispersive spectroscopy and transmission electron microscopy) were employed to probe the morphological structures. The electrochemical properties of the as-prepared 3D architectures were investigated with three and two-electrode systems. In addition to its high specific capacitance (710 F g⁻¹ at 20 A g⁻¹), after charging–discharging for 2000 cycles, the electrode still maintained the capacity retention of about 82%. When used as the active electrode material for supercapacitors, the fabricated CoNi₂S₄–g–CNT nanostructure exhibited excellent specific capacitance and good rate capability, making it a promising candidate for next-generation supercapacitors.