正极材料LiFe1-xNixPO4/C的合成及性能

以H3PO4、FeSO4·7H2O和LiOH·H2O为原料,采用水热法以Ni(CH3COO)2·4H2O为镍源、葡萄糖为碳源,合成锂离子电池正极材料LiFe1-xNixPO4/C(x=0,0.02,0.05,0.08).采用X射线衍射、扫描电子显微镜对材料晶体结构和表观形貌进行表征,利用充放电测试技术对其电化学性能进行测定.结果表明:掺杂适量的Ni2+可以减小材料的晶胞体积,提高材料的比电容和循环性能.当Ni2+的掺杂量为5.0％时,LiFe0.95Ni0.05PO4/C材料在0.1C倍率下的首次放电比电容可达到152.8 mA·h/g,经过20次循环后的比电容保持率在97.5％以上.     

用沉淀法制备超细草酸钴粉体

以硫酸钴(CoSO4)和草酸(H2C2O4)为原料,采用直接沉淀法制备超细草酸钴(CoC2O4·2H2O)粉体.用X射线衍射分析、热重-差热分析、激光粒度分析和高倍显微镜对制备的CoC2O4·2H2O粉体进行了表征.讨论了H2C2O4浓度、反应温度、表面活性剂,乙醇脱水和加料速率对CoC2O4·2H2O粉体粒度的影响.结果表明:较高的H2C2O4浓度、较低的反应温度、加入表面活性剂、乙醇脱水、较低的加料速率,都有利于制备较细的CoC2O4·2H2O粉体.     

水热法制备纳米NiO粉体及其应用研究

以Ni(NO3)2·6H2O、CO(NH2)2和乙二醇为原料,采用水热法制备纳米Ni O粉体,并将其应用于固体氧化物燃料电池阳极中,采用XRD、激光粒度仪、TEM和电化学工作站分别对粉体的物相、粒度分布、形貌和单电池的电性能进行了表征。研究结果表明,利用水热法制备了纯度高、分散性好的纳米Ni O粉体。将其用于固体氧化物燃料电池的阳极中,该单电池以氢气为燃料,空气为氧化气,在750℃的最大功率密度0.66W/cm2。     

改性海藻酸钠／壳聚糖双极膜成对电解制备乙醛酸

以镍网电极-改性海藻酸钠/壳聚糖双极膜(Ni-mSA/mCS BM)作为阴阳两室间的隔膜,利用双极膜的中间界面层水解离特性成对电解制备乙醛酸.水解离特性分析结果表明,双极膜中水解离后生成的H 透过mSA阳离子膜进入阴极室中,可及时补充草酸电还原生成乙醛酸过程中的H 消耗;OH(透过mCS阴离子膜进入阳极室中,与乙二醛电氧化生成乙醛酸过程中产生的H 结合生成H2O,可促进正向反应的速度.以饱和草酸和盐酸的混合液作阴极液,以10%乙二醛和10%KBr的混合液作阳极液,镍网为阴极,二氧化铅为阳极,在电流密度为20 mA·cm-2常温下电解,阴极电流效率达82.9%,阳极电流效率达75.7%,电解电压低于2.7 V.     

五氧化二钒电解制备全钒液流电池V3+电解液

电解液的质量直接决定了全钒液流电池的储电能力。为了降低全钒液流电池的生产成本,在国内首次采用流动型电解槽电解还原法,研究了采用相对廉价的五氧化二钒(V2O5)代替价格昂贵的硫酸氧钒(VOSO4)为原料制备全钒液流电池电解液的制备技术;研究了阳极电极材料、电解电流密度等对制备电解液的影响因素;并通过循环伏安、交流阻抗和充放电测试分析和比较由两种原料制备的电解液的电化学性能。实验结果表明:以Ru Ir/Ti为阳极,多孔铅板为阴极,3 mol·L-1 H2SO4为阳极电解液,1.5 mol·L-1 V2O5+3 mol·L-1 H2SO4粉末混合溶液为阴极电解液,40 m A·cm-2恒流电解得到的电解液不但具有良好的电化学活性和可逆性,且电流效率高和电能损耗低,完全可以满足全钒液流电池的工作需求。     

熔盐法制备钛酸镍及其电化学性能

采用熔盐法制备钛酸镍,探讨了煅烧过程中不同熔盐比例以及不同保温时间对钛酸镍晶体结构的影响。结果表明,Ni(OH)2、Ti O2和混合熔盐的摩尔比为1∶1∶4,800℃时通空气保温10 h,可制备黄色钛酸镍,粒径约0. 3～1. 0μm。制备的钛酸镍作为锂离子电池负极材料,表现出良好的电化学性能,充电倍率为0. 1 C时,首次充电比容量为353. 4 m A·h·g-1。在0. 1 C和0. 2 C时循环100次后,容量保持率分别为99. 5%和96. 3%。熔盐法制备钛酸镍是一种简单、廉价、可得到高比能量锂离子电池负极材料的制备工艺。     

氢氧化镍电极的修饰及电化学性能的研究

镍系列二次电池的正极活性物质Ni（OH）2的晶型和镍电极的制备工艺对电池的性能具有较大的影响。文章以镍-氢电池作为对象,着重研究作为电池正极的氢氧化镍电极。通过不同的方法制备电极的活性物质Ni（OH）2,以Co、Zn和稀土作为掺杂剂对电极进行修饰,并对不同掺杂方式构成的电池进行了测试。用金相显微镜来观察Ni（OH）2的外观、颗粒大小;通过恒电流放电曲线比较各电极的放电性能,并通过XRD谱图了解样品的晶型结构。电池性能测试结果表明：采用配位沉淀法制备的Ni（OH）2晶体为最佳;在添加剂方面,Zn、Co、Sm均对镍电极的电化学性能影响较大。     

改进固相法合成LiNixCoyMn1-x-yO2正极材料及性能研究

采用同相法制备正极材料LiNi1/3Co1/3Mn1/3O2,用X射线衍射仪(XRD)、扫描电子显微镜(SEM)/透射电镜(TEM)分析材料的结构和形貌特征,用LAND电池测试系统测试材料的电化学性能(充放电容量和循环性能等).以LiOH·H2O,H2C2O4·2H2O,Ni(AC)2·4H2O,Co(AC)2·4H2O和Mn(AC)2·4H2O为原料,采用固相法在不同煅烧温度和煅烧时间下制备的层状正极材料LiNi1/3Co1/3Mn1/3O2具有典型的α-NaFeO2型层状结构特征,晶型结构完整.电化学性能测试结果表明,在850℃下保温15 h合成的正极材料电化学性能最优,在电流密度为120 mA/g、充放电电压在2.75～4.5 V时,经30次循环后放电比容量为163.5 mA·h/g,容量保持率为94%;50次循环后为157.2 mA·h/g,容量保持率为90.8%.     

超声场中沉淀法纳米氧化锌的制备与表征

将超声辐射应用于以硫酸锌(ZnSO4·7H2O)和草酸(H2C2O4·2H2O)为原料的沉淀法制备纳米氧化锌粉体的工艺过程,制备了平均晶粒尺寸为26nm的氧化锌粉体。通过XRD,DTA—TG和SEM等技术研究了纳米氧化锌的合成过程及粉体性能。结果表明:超声辐射引入普通沉淀法,超声波的空化作用可使前驱体颗粒细化,抑制其团聚并延缓其向凝胶转变,从而可制备出氧化锌纳米粉体。这种方法所得纳米氧化锌粒子外貌为球形,粒度分布均匀,分散性好。     

纳米多孔Fe_2O_3–Fe_3O_4/Ni复合材料作为锂离子电池负极材料的电化学性能

通过在NH4F+H2O的乙二醇溶液中阳极氧化铁箔,制备了纳米多孔结构的铁氧化物(Fe2O3–Fe3O4),然后在纳米多孔中电沉积镍,再经过400°C退火0.5 h,获得了镍与纳米多孔氧化铁的复合材料(Fe2O3–Fe3O4/Ni)。考察了电流密度和时间对镍沉积的影响。用扫描电镜、能谱仪、X射线衍射仪表征了复合材料的表面形貌、元素组成和物相,测试了其电化学性能并与未经电沉积镍的纳米多孔氧化铁(Fe2O3–Fe3O4)比较。结果表明,氧化铁由Fe2O3和Fe3O4组成。镀镍的最佳电流密度为2.0 m A/dm2,时间30 s。该纳米多孔Fe2O3–Fe3O4/Ni复合材料作为锂离子电池负极材料表现出更好的电化学性能──经过50次充放电循环后的放电比容量仍有438.3 m A·h/g,而Fe2O3–Fe3O4电极的放电比容量仅为110.6 m A·h/g。Fe2O3–Fe3O4/Ni电极的循环稳定性和倍率性能优异。     

Magnetic Ceramics: VI, Evaluation of Some Methods of Nickel Ferrite Formation

The extent of nickel ferrite formation, as affected by four preparatory techniques, was investigated by determining the magnetic moment of the reacted powder with a vibrating-coil magnetometer. The oxide, carbonate, hydroxide, and oxalate methods were used. At low temperatures the hydroxide and oxalate techniques were found to give the greatest yield of ferrospinel. The hydroxide method yielded a magnetic material by precipitation. Weight-loss measurements were correlated to the magnetic data.     

Preparation of Spherical, Solid Barium Titanate Particles with Uniform Composition at High Precursor Concentration by Spray Pyrolysis

Hydrolysis-assisted spray pyrolysis (HASP) using dimethyl oxalate as hydrolyte was found to be applicable to precipitation of solid, spherical BaTiO₃ powder with uniform composition when the stock solution concentration was high (>1.0 M ). Solid, dense powder with uniform composition was successfully obtained because barium titanium oxalate was prepared from partial hydrolysis of dimethyl oxalate and coprecipitation of oxalate with barium and titanium during the hydrolysis–precipitation process, and then the oxalate particles became seeds in the following process. The sintered sample from the as-prepared BaTiO₃ powder led to a higher dielectric constant and lower loss.     

不锈钢老化着色液预还原草酸沉淀除杂过程研究

为实现不锈钢老化着色液杂质离子的分离与回收,采用预还原-草酸沉淀法对老化液中铁、镍、锰沉淀除杂过程进行研究。通过溶液化学计算及条件优化实验,考察铁、镍、锰离子沉淀效率,并使用X射线衍射仪、扫描电子显微镜、X射线光电子能谱仪对草酸沉淀物进行物相及形貌结构的表征。结果表明,通过控制溶液pH及草酸用量可有效实现溶液中铁离子、锰离子、镍离子与草酸根络合,形成草酸盐沉淀,实现杂质离子与溶液铬离子分离,杂质离子沉淀顺序依次为锰离子、镍离子、铁离子。老化液预还原后,在草酸过量系数为1.2、溶液pH为2、反应温度为25℃的条件下沉淀反应2 h,铁、锰、镍离子沉淀率分别可达98.12%、99.35%、87.26%,沉淀物主要为二水草酸亚铁及少量草酸镍、草酸锰。     

Preparation of cobalt oxalate powders with the presence of a pulsed electromagnetic field

The size and morphology of cobalt oxalate powders are the keys to metal cobalt powder production. Spheroidic and fine cobalt oxalate powders were prepared by conventional precipitation when a pulsed electromagnetic field (PEMF) was introduced. The phase structures of the produces were characterized by means of X-ray powder diffraction (XRD). Scanning electron microscopy (SEM) images were used to observe the morphologies of the cobalt oxalate powders. Thermal analyses were performed using TG–DSC thermogravimetric analyzer. Meanwhile, a possible mechanism was proposed based on the interaction between pulsed electromagnetic field and cobalt oxalate cluster.     

草酸铵沉淀法制备纳米氧化钕研究

以硝酸钕、草酸铵为原料,六偏磷酸钠为分散剂,采用沉淀法制备纳米氧化钕前驱体,将前驱体在空气中焙烧制备纳米氧化钕粉体。研究了反应温度、物料浓度等因素对粉体的影响,用激光粒度仪测得样品的粒度分布,用X射线衍射和扫描电镜对样品进行表征。实验表明,在最佳条件下可以制得平均粒径为100 nm的片状氧化钕粉体。     

多孔镍/白云石颗粒对生物质气化焦油裂解的催化性能

通过添加镍的方法,改善多孔白云石颗粒对生物质气化焦油裂解的催化能力。采用配位沉淀法制备Ni/白云石粉末,再以Ni/白云石粉末为原料,制备多孔Ni/白云石颗粒。以苯为生物质气化焦油的模型成分,在Ni/白云石颗粒固定床对苯进行蒸汽重整,考察了多孔Ni/白云石颗粒制备过程中,焙烧温度和氧化镍含量等条件对其催化能力的影响。结果表明,多孔Ni/白云石颗粒的催化能力随焙烧温度和氧化镍含量而变化,在焙烧温度750 ℃和氧化镍质量分数13.5%的条件下,Ni/白云石颗粒上苯蒸汽重整的气体收率达到最大值83.0%。在焙烧温度（450～900） ℃和氧化镍质量分数0～22.5%时,积炭率基本保持在4.5%。900 ℃焙烧2 h,对积炭失活的多孔Ni/白云石颗粒进行再生,再生的多孔Ni/白云石颗粒对苯蒸汽重整的催化能力与新鲜多孔Ni/白云石颗粒相同。     

Impregnation of porous nickel plates by cathodic polarization

The influence of cathodic polarization during the precipitation of Ni(OH)₂ in porous plates prepared from sintered nickel powder has been studied and the influence of the preparation method on the properties of the electrodes examined under conditions which do not lead to the dissolution of the sintered nickel plate. An increase of electrode capacity is recorded for electrodes produced by cyclic polarization between treatment of the plates by immersion in KOH solution.     

副产硫酸亚铁制备电池级草酸亚铁的研究

以钛白副产硫酸亚铁为原料制备出电池级草酸亚铁。研究了除杂、沉淀、转化反应过程中反应温度、反应时间、硫酸亚铁浓度以及反应pH等因素对产品质量的影响,并得到了优惠工艺条件。结果表明：在反应温度为 95 ℃、反应时间为6 h的条件下用铁粉对硫酸亚铁溶液除杂,得到纯净硫酸亚铁溶液;在反应温度为40 ℃、铁（Ⅱ）质量浓度为90 g/L的条件下用氨水沉淀,再用草酸于反应时间为60 min、pH=2.0条件下将氢氧化亚铁转化成草酸亚铁,制备出了纯度大于99.5%、粒径小于3.0 μm、杂质含量低的电池级草酸亚铁。为解决钛白副产硫酸亚铁的综合利用提供了一条有效的途径。     

Synthesis and characteristics of nanocrystalline 3Y-TZP and CuO powders for ceramic composites

A weakly agglomerated 3Y-TZP powder with 100% tetragonal crystal structure and a primary crystallite diameter of 8 nm was prepared by co-precipitation of metal chlorides in an ammonia solution, followed by extensive washing with ethanol, drying and calcining at 550 °C. Powder characteristics as function of thermal treatment are discussed. A copper oxalate precipitation for the preparation of nanocrystalline CuO powders was optimised in order to minimise aggregation and agglomeration. The influence of calcination procedure and synthesis medium on several powder characteristics of the CuO powders were investigated in detail. Oxalate precipitation in ethanol followed by sequential drying and calcination in air at 250 °C in an open tubular furnace with proper air-powder contact area was found to be the optimal procedure for producing nanocrystalline single-phase CuO powder with small aggregates and weak agglomerates. With this optimal procedure a CuO powder with crystallite diameter and BET equivalent particle diameter of respectively 12 and 20 nm was obtained.     

Fabrication and characterization of NiO nanoparticles by precipitation from aqueous solution

Present work involves synthesis of NiO nanoparticles using chemical homogeneous precipitation (CHP) method as a facile procedure. Ammonia as a complex agent was used in this method. Effects of different types of complexation-precipitation methods on the crystallinity and morphology of nanoparticles were investigated. NiO particles were prepared by direct precipitation method from NiSO₄ solution to compare crystallinity and morphology of NiO particles with particles obtained via complexation-precipitation methods. Our major intent was to investigate the effect of complex agent on the crystallization and growth of NiO nanoparticles. Results showed that the best condition for synthesizing spherical NiO shape was using NaOH as decomposing agent, of which the consequence was more uniformity and spherical nanoparticles with a diameter in the range of 40–60 nm. The size of the nickel oxide and nickel hydroxide nanoparticles was estimated by X-ray powder diffraction (XRD) pattern. The chemical structure information of the particles was studied by Fourier transform infrared (FT-IR) spectroscopy. Spherical, elliptical, sheet or flowerlike shapes were detected by field emission scanning electron microscopy (FESEM) analysis. Results showed that by the use of ammonia as complex agent, crystalline state and particles size distribution of NiO nanoparticles improved.