Synthesis and characterization of Co<Subscript>3</Subscript>O<Subscript>4</Subscript> prepared from atmospheric pressure acid leach liquors of nickel laterite ores

A chemical precipitation-thermal decomposition method was developed to synthesize Co₃O₄ nanoparticles using cobalt liquor obtained from the atmospheric pressure acid leaching process of nickel laterite ores. The effects of the precursor reaction temperature, the concentration of Co2+, and the calcination temperature on the specific surface area, morphology, and the electrochemical behavior of the obtained Co₃O₄ particles were investigated. The precursor basic cobaltous carbonate and cobaltosic oxide products were characterized and analyzed by Fourier transform infrared spectroscopy, thermogravimetric differential thermal analysis, X-ray diffraction, field-emission scanning electron microscopy, specific surface area analysis, and electrochemical analysis. The results indicate that the specific surface area of the Co₃O₄ particles with a diameter of 30 nm, which were obtained under the optimum conditions of a precursor reaction temperature of 30℃, 0.25 mol/L Co2+, and a calcination temperature of 350℃, was 48.89 m2/g. Electrodes fabricated using Co₃O₄ nanoparticles exhibited good electrochemical properties, with a specific capacitance of 216.3 F/g at a scan rate of 100 mV/s.     

球形多孔氧化钴/碳复合材料的制备及电容性能研究

采用水热合成和煅烧制备氧化钴/碳(Co3O4/C)复合材料,通过SEM、XRD、N2吸附实验等对该材料进行表征.制备的Co3O4/C复合材料为5μm大小,孔径约为30nm的多孔球形结构.在6mol/L的氢氧化钾溶液中进行电化学测试.结果表明,Co3O4/C复合材料具有良好的电容性能.在电流密度为1A/g时,比电容为143F/g.此外,Co3O4/C复合材料还表现出良好的循环稳定性,在1A/g的电流密度下,充放电循环1000次后,比电容保持率为77.8%.     

Preparation and electrochemical performance of double perovskite La<Subscript>2</Subscript>CoMnO<Subscript>6</Subscript> nanofibers

Through electrospinning, La₂CoMnO₆ nanofibers were prepared from a polyvinylpyrrolidone/lanthanum nitrate–cobalt acetate–manganese acetate (PVP/LCM) precursor and were used as electrode materials. The morphologies and structures of the samples were characterized by field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and Brunauer-Emmett-Teller (BET) specific surface area analysis. The results show that the prepared La₂CoMnO₆ nanofibers are stable, one-dimensional structures formed from interconnected La₂CoMnO₆ nanoparticles with a diamond-like crystal structure. The specific surface area of the fibers is 79.407 m2·g-1. Electrochemical performance tests with a three-electrode system reveal the specific capacitance of the La₂CoMnO₆ nanofibers as 109.7 F·g-1 at a current density of 0.5 A·g-1. After 1000 charge-discharge cycles at a current density of 1 A·g-1, the specific capacitance maintains 90.9% of its initial value, demonstrating a promising performance of the constraint capacitance and good cyclic stability.     

Preparation and luminescence properties of YeO3：Er^3＋/TiO2 with high specific surface area

The three composites Y2O3 :Er3+ , Y2O3 :Er3+ /Yb 3+ andY2O3 :Er3+ /TiO2 were prepared using coprecipitation and sol-gel techniques. Their morphology, specific surface area, porosity, UV-vis. absorption spectra and fluorescence spectra were measured using SEM, TEM, surface analysis, UV-vis. absorption and photoluminescence spectrophotometry. SEM and TEM showed that samples prepared using coprecipitation were dispersed, while Y2O3 :Er3+ /TiO2 particles possessed a mesoporous surface and average diameter of ab...     

聚苯胺纳米纤维的界面聚合法合成及电化学电容行为

利用盐酸和四氯化碳的水/油两相界面,通过界面聚合法合成具有良好纳米纤维结构的聚苯胺,用这种聚苯胺纳米纤维为活性物质制备电极,以1 mol/L H2SO4水溶液为电解液组装超级电容器,通过恒电流充放电、循环伏安、交流阻抗等技术研究其电化学电容行为。研究结果表明,合成的聚苯胺的直径为50～100 nm,长度为500nm至几微米不等,且纤维之间相互交织缠绕,形成网状形貌;聚苯胺纳米纤维电极材料的功率特性与循环性能优于用传统化学氧化法合成的颗粒状聚苯胺材料的性能,在5 mA放电电流下,其比电容可达317 F/g,20mA放电电流下比电容仍维持300 F/g左右,500次循环容量衰减在4%以内。     

无模板法制备多孔聚苯胺及其电化学性能

通过以极慢的速率滴加氧化剂水溶液方式,构建了受限的油水反应界面,在无模板条件下制备了多孔聚苯胺,并研究了产物的结构和用作超级电容器电极材料的电化学性能.结果表明:产物为银耳状多孔结构,富含小于10 nm的中介孔.在电流密度为1 A/g时,充放电时间近似对称,比电容高达441 F/g,经2 000次充放电循环后,比电容损失率为27.3%,该聚苯胺表现出良好的电化学性能.     

Immobilization of hemoglobin on platinum nanoparticles-modified glassy carbon electrode for H<Subscript>2</Subscript>O<Subscript>2</Subscript> sensing

This work described an amperometric hydrogen peroxide (H2O2) biosensor based on immobilization of hemoglobin (Hb) on a glassy carbon (GC) electrode modified by platinum nanoparticles, which was prepared by an in situ chemical reductive growth method. The electrochemical impedance measurements confirmed that the Hb was immobilized on the platinum nanoparticles-modified glassy carbon surface and has a synergistic effect with platinum nanoparti-cles in improving the catalytic reduction of H2O2. The Hb immobili...     

A new PAA Sol-gel method to synthesis the spinel LiMn<Subscript>2</Subscript>O<Subscript>4</Subscript> Material for Li-ion battery

A PAA sol-gel method, which is based on the chelate effect of PAA polymer, was developed for the synthesis of the spinel LiMn₂O₄ material. The pyrolysis process of the PAA-nitrate mixture precursor was investigated by TG and DTA analysis. It is found that the structure and electrochemical properties of the material are sensitive to the atmosphere employed in the synthesis process. Preliminary results show that the material thus prepared has a good electrochemical performance even at high charge and discharge current. Foundation item: Supported by the National Science Foundation of China (No. 29833090) Biography: Zhan Hui (1973-), female, Ph.D. research direction relectrochemistry.     

Graphene-immobilized flower-like Ni<Subscript>3</Subscript>S<Subscript>2</Subscript> nanoflakes as a stable binder-free anode material for sodium-ion batteries

A binder-free Ni₃S₂ electrode was prepared directly on a graphene-coated Ni foam (G/Ni) substrate through surface sulfiding of substrate using thiourea as the sulfur source in this work. The Ni₃S₂ showed a flower-like morphology and was uniformly distributed on the G/Ni surface. The flower-like Ni₃S₂ was composed of cross-arrayed nanoflakes with a diameter and a thickness of 1-2 μm and~50 nm, respectively. The free space in the flowers and the thin feature of Ni₃S₂ buffered the volume changes and relieved mechanical strain during repeated cycling. The intimate contact with the Ni substrate and the fixing effect of graphene maintained the structural stability of the Ni₃S₂ electrode during cycling. The G/Ni-supported Ni₃S₂ maintained a reversible capacity of 250 mAh·g-1 after 100 cycles at 50 mA·g-1, demonstrating the good cycling stability as a result of the unique microstructure of this electrode material.     

Synthesis and characterization of Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>@SiO<Subscript>2</Subscript> magnetic composite nanoparticles by a one-pot process

Fe₃O₄@SiO₂ core–shell composite nanoparticles were successfully prepared by a one-pot process. Tetraethyl-orthosilicate was used as a surfactant to synthesize Fe₃O₄@SiO₂ core–shell structures from prepared Fe₃O₄ nanoparticles. The properties of the Fe₃O₄ and Fe₃O₄@SiO₂ composite nanoparticles were studied by X-ray diffraction, transmission electron microscopy, energy dispersive spectroscopy, and Fourier transform infrared spectroscopy. The prepared Fe₃O₄ particles were approximately 12 nm in size, and the thickness of the SiO₂ coating was approximately 4 nm. The magnetic properties were studied by vibrating sample magnetometry. The results show that the maximum saturation magnetization of the Fe₃O₄@SiO₂ powder (34.85 A·m2·kg–1) was markedly lower than that of the Fe₃O₄ powder (79.55 A·m2·kg–1), which demonstrates that Fe₃O₄ was successfully wrapped by SiO₂. The Fe₃O₄@SiO₂ composite nanoparticles have broad prospects in biomedical applications; thus, our next study will apply them in magnetic resonance imaging.     

Synthesis and modification of well-ordered layered cathode oxide LiNi<Subscript>2/3</Subscript>Mn<Subscript>1/3</Subscript>O<Subscript>2</Subscript>

Oxalic-acid-based co-precipitation method was employed to prepare LiNi_2/3Mn_1/3O₂ sample with a high-ordered structure. Li⁺, Ni²⁺ and Mn²⁺ acetates were used as starting materials. The influence of the amount of lithium source in the starting materials on Li⁺ content, disorder of Li⁺-Ni²⁺ ions, and electrochemical performance has been investigated. Rietveld refinement shows that the sample prepared with 20% excess Li-source in the starting materials exhibits a perfect ordered structure. A specific discharge capacity is as high as 172 mAh/g at C/20 in the voltage range of 4.35–2.7 V. However, the cyclability is not satisfactory: about 25.3% fade in capacity was observed over 50 cycles. Chemically stable SiO2 was coated on the surface of LiNi_2/3Mn_1/3O₂ particles. A significant improvement in cyclability was attained with 3 wt% SiO2 coating, which is ascribable to the protection of LiNi_2/3Mn_1/3O₂ particles from being dissolved into the electrolyte.     

A study on nano-sized NiO electrodes doping with C and Co prepared by electrochemical deposition-sintering processes and their capacitance performance

In the present work, it was studied that nanoosized NiO electrodes doping with C and Co were prepared by electrochemical deposition in an ethanol solution containing nickel nitrate and cobalt nitrate and sintering processes. The capacitance performance of such electrodes was also studied. The results reveal that samples obtained by electrochemical deposition first on a porous nickel cathode in an ethanol solution contain 0.5 mol/L nitrates, in which Ni(NO3)2 and Co(NO3)2 were mixed in a molar proportion of 8 : 2. After sintering at 300℃ for 2 h, they exhibited the best performance. XRD analysis illustrates that the essential phase of the product is NiO doping with certain content of C and Co. The particles of product imaged a spherical morphology with sizes of 20---30 nm in diameter, and with an average crystal size of 4--5 nm. The capacitance measurement of the simulating C/NiO capacitors indicates that a single electrode can reach as high as 410.0 F/g, and still maintain the value of 323 F/g after 30 recycles showed as a stabilized value with increasing recycles, when it was discharged at a current of 5 mA.     

Electrochemical properties of LiNi<Subscript>0.5</Subscript>Mn<Subscript>1.3</Subscript>Ti<Subscript>0.2</Subscript>O<Subscript>4</Subscript>/Li<Subscript>4</Subscript>Ti<Subscript>5</Subscript>O<Subscript>12</Subscript> cells

Spinel compounds LiNi_0.5Mn_1.3Ti_0.2O₄ (LNMTO) and Li₄Ti₅O₁₂ (LTO) were synthesized by different methods. The particle sizes of LNMTO and LTO are 0.5–2 and 0.5–0.8 μm, respectively. The LNMTO/LTO cell exhibits better electrochemical properties at both a low current rate of 0.2C and a high current rate of 1C. When the specific capacity was determined based on the mass of the LNMTO cathode, the LNMTO/LTO cell delivered 137 mA·h·g⁻¹ at 0.2C and 118.2 mA·h·g⁻¹ at 1C, and the corresponding capacity retentions after 30 cycles are 88.5% and 92.4%, respectively.     

Electro-deoxidation of V<Subscript>2</Subscript>O<Subscript>3</Subscript> in molten CaCl<Subscript>2</Subscript>-NaCl-CaO

The electro-deoxidation of V₂O₃ precursors was studied. Experiments were carried out with a two-terminal electrochemical cell, which was comprised of a molten electrolyte of CaCl₂ and NaCl with additions of CaO, a cathode of compact V₂O₃, and a graphite anode under the potential of 3.0 V at 1173 K. The phase constitution and composition as well as the morphology of the samples were studied by X-ray diffraction (XRD) and scanning electron microscopy (SEM). 3 g of V₂O₃ could be converted to vanadium metal powder within the processing time of 8 h. The kinetic pathway was investigated by analyzing the product phase in samples prepared at different reduction stages. CaO added in the reduction path of V₂O₃ formed the intermediate product CaV₂O₄.     

聚苯胺/活性炭复合材料电容性能研究

以商品化活性炭为原料，在1mol／L盐酸环境下采用原位聚合法制备了聚苯胺／活性炭复合材料（PANI／C），复合材料中聚苯胺的质量分数为46．4％．用循环伏安、交流阻抗、恒流充放电测试等方法考察比较了新材料与原活性炭在1mol／L H2SO4溶液中的电容性能．结果表明，新材料的比容量和大电流充放电性能均优于碳材料．3．0mA／cm^2电流密度下，复合材料电极比容量高达448．7F／g，比原碳材料提高60％．     

花状Co5（O9．48H8．52）NO3的简易制备及其超级电容性能

采用简单沉淀方法制备出花状结构的Co5(O9.48H8.52)NO3,运用XRD、SEM、TEM、BET等方法对反应产物进行表征.结果表明,Co5(O9.48H8.52)NO3具有低结晶度的花状结构,孔径主要分布在4~40 nm,比表面积为77.22 m2/g.循环伏安、恒流充放电、交流阻抗和循环寿命测试均表明该材料具有良好的超级电容特性,单电极比容量可达368 F/g.     

Mn_7C_3@C核壳型纳米粒子制备及其超级电容器电极特性

以甲烷作为碳源气体,块体锰作为原料,采用一种简单的直流电弧等离子体法成功制备了Mn_7C_3@C核壳型纳米粒子,用于高性能超级电容器的电极材料.所制备的Mn_7C_3@C核壳型纳米粒子平均直径为30~35nm.拉曼光谱结果显示石墨碳壳具有良好的导电性.通过循环伏安、恒电流充放电及电化学交流阻抗谱对Mn_7C_3@C核壳型纳米粒子电极材料进行电化学性能分析,结果表明其具有高比电容、快速充放电等优异的电化学性能.在扫描速率为1mV/s时,比电容最高可达185.8F/g.同时具有良好的循环稳定性,在100mV/s扫描速率下1 000次循环伏安测试后,比电容仍保持为最初的88%,与单纯Mn_7C_3(79%)相比,有明显提高.Mn_7C_3@C核壳型纳米粒子电极材料优异的电化学性能归因于其良好的核壳结构,富缺陷碳层具有良好的导电性,有助于离子的传输和结构的稳定,而内核Mn_7C_3主要产生赝电容,在C和Mn_7C_3的协同作用下产生双电层和赝电容双模式储能机制.     

高比表面积椰壳活性炭的制备及其应用

以活性炭AC为原料,采用CO2活化法制备高比表面积活性炭,通过控制尾气中CO2含量间接控制活化反应速率,测试了以产品活性炭为电极材料的双电层电容器的充放电性能及循环伏安特性,并测定了以产品活性炭为吸附剂的CO2、CH4、N2、O2和H2的298K吸附等温线．实验结果表明,在控制尾气中C02含量小于10％,活化28h,所得活性炭（AC-28）比表面积为2587m^2／g,总孔容为1．47cm^3／g,较原料活性炭AC的相应数值分别提高33％和62％,以AC-28为电极材料的双电层电容器具有良好的充放电性能,电极比电容达171F／g,作为吸附剂,活陛炭AC-28对CO2的吸附量远远大于CH4、O2、N2和H2,具有吸附分离COJN2、CO2／O2及CO2／空气气体混合物中CO2的潜力。     

RGO/NiCo_2O_4复合电极材料制备及电化学性能研究

采用层-层自组装法制备了前驱体RGO/Ni-Co@Ni-foam(泡沫镍负载石墨烯/镍-钴金属化合物),并在高温下煅烧得到RGO/NiCo_2O_4@Ni-foam复合电极材料。运用X射线衍射仪、扫描电子显微镜以及能谱仪对多孔RGO/NiCo_2O_4@Ni-foam复合材料进行结构表征,并通过循环伏安、恒流充放电等测试方法考察了其作为电极材料的电化学性能。结果表明,制备的多孔RGO/NiCo_2O_4@Ni-foam复合电极材料的比电容在电流密度为0.5A/g时可达到444F/g,并且在经过1 000次循环实验后,比电容仍有342F/g。这表明多孔RGO/NiCo_2O_4@Ni-foam复合材料在超级电容器领域具有广阔的应用前景。     

Adsorption and catalytic combustion of ARB on CuO-Fe<Subscript>2</Subscript>O<Subscript>3</Subscript>

CuO-Fe2O3 composite material with strong magnetism and a large surface area is prepared by the co-precipitate method. Its adsorption properties towards Acid Red B (ARB) and the regeneration by catalytic combastion of organic compounds have been studied. The results show that the prepared CuO-Fe2O3 composite is an excellent adsorbent for ARB adsorption at acid condition. The presence of Cl^- has no effect on ARB adsorption. But the SO4^2- can inhibit ARB adsorption. After being recovered by the magnetic separation method, the adsorbent can be regenerated by catalytic oxidation of absorbate at 300℃ in air atmosphere. The combustion reactions of ARB in the presence or absence of CuO-Fe2O3 are studied by in situ diffuse refieclion FTIR. The results indicate that, in the presence of CuO-Fe2O3, the degradation temperature is significantly lowered by the catalysis of CuO-Fe2O3, and ARB can be oxidized completely without volatile organic compound by-product; in comparison, in the absence of CuO-Fe2O3, the temperature needed for oxidation of ARB is higher and the reaction is incomplete with some N-containing harmful compounds produced. The reusability of CuO-Fe2O3 is also studied in successive seven adsorption-regeneration cycles.