电感耦合等离子体质谱法(ICP-MS)测定镍钴锰三元氢氧化物中铅

研究了用电感耦合等离子体质谱法（ICP-MS）测定镍钴锰三元素氢氧化物中铅含量的测定方法。选择了仪器的最佳测量条件、元素测定的质量数,进行了基体元素的干扰等实验。方法测定结果准确、可靠,测定下限小于0.00005%,样品加标回收率在99.2%~101.0%。方法的建立为控制镍钴锰三元素氢氧化物中铅提供了检测依据。     

电感耦合等离子体质谱法(ICP-MS)测定镍钴锰三元素氢氧化物中铅

研究了用电感耦合等离子体质谱法(ICP-MS)测定镍钴锰三元素氢氧化物中铅含量的测定方法。选择了仪器的最佳测量条件、元素测定的质量数,进行了基体元素的干扰等实验。方法测定结果准确、可靠,测定下限小于0.00005%,样品加标回收率在99.2%~101.0%。方法的建立为控制镍钴锰三元素氢氧化物中铅提供了检测依据。     

氯化银比浊法测定镍钴锰三元素氢氧化物中氯离子

建立了氯化银比浊法测定镍钴锰三元素氢氧化物中氯离子含量的测定方法。选择了合适的测定波长,并对硝酸用量、沉淀剂用量、稳定时间对测定结果的影响进行了试验,确定了较优的分析条件。样品加标回收率在95%~103.3%,氯离子浓度在0~4μg/mL与浊度值有良好线性关系。方法为控制镍钴锰三元素氢氧化物中氯离子提供了检测依据。     

电导滴定法测定镍的含量

由电导滴定法确定终点，在氨性介质中用丁二酮肟乙醇溶液滴定镍的含量，采用硫脲掩蔽Cu(Ⅱ），用H2O2将Mn（Ⅱ），Co(Ⅱ）氧化成Mn(Ⅳ）和Co(Ⅲ）消除干扰，其它金属离子对测定没有干扰，此法的测定结果与丁二酮肟重量法接近，且不受溶液的颜色、浊度的影响，具有准确、快速、干扰少的特点，适用于化学镀镍溶液，电镀镍和镍合金中镍的测定。     

氯化银比浊法测定镍钴锰三元素氢氧化物中氯离子含量

研究了氯化银比浊法测定镍钴锰三元素氢氧化物中氯离子含量的测定方法。选择了合适的测定波长,并对硝酸用量、沉淀剂用量、稳定时间的影响进行了试验,确定了较优的分析条件。样品加标回收率在95%-103.3%,氯离子浓度在0-4μg/mL与浊度值有良好线性关系。方法为控制镍钴锰三元素氢氧化物中氯离子提供了检测依据。     

Na2EDTA返滴定法测定铜镍合金中的镍含量

采用Na₂EDTA返滴定法测定铜镍合金中的镍含量,用柠檬酸钠、硫代硫酸钠和酒石酸作掩蔽剂,丁二酮肟沉淀分离,以二甲酚橙为指示剂,加入过量的Na2EDTA,用氯化锌标准溶液返滴定,能很好地分离铜及其他杂质的干扰。方法用于测定铜镍合金中的镍含量,测定结果的相对标准偏差(RSD,n=9)为0.046%~0.24%,加标回收率为99.3%~101%。能够满足日常样品的检测要求。     

CAS-CPB胶束增溶光度法直接测定金红石单矿物中铝

一般矿石中微量铝采用CAS光度法测定,用酒石酸或苦杏仁酸掩蔽钛的干扰,TiO_2的允许量最多达250微克。金红石含TiO_295%左右,所以直接测定其中的铝是困难的。CAS-CPB胶束增溶光度法测定铝比CAS的灵敏度高,但钛的干扰严重,经试验用酒石酸掩蔽钛,存在0.5毫克TiO_2就有明显正干扰,1毫克TiO_2使吸光度增加1倍;采用酒石酸—苦杏仁酸联合掩蔽效果较好,1.5毫克TiO_2基本无影响,但灵敏度有所降低,摩尔吸光系数为8.5×10~4,仍比CAS灵敏度高,可不经分离直接光度法测定金红石单矿物中的微量铝。     

以α型氢氧化物前驱体制备LiNi_(0.8)Co_(0.15)Al_(0.05)O_2及其电化学性能

本文采用球形Al/Co部分取代α型Ni(OH)2为前驱体成功制备了锂离子电池正极材料LiNi0.8Co0.15Al0.05O2。首先采用氢氧化钠与碳酸钠为沉淀剂合成出Al/Co部分取代α型Ni(OH)2,然后将之与LiOH·H2O混合,最后在氧气气氛中不同温度下热处理8h,即可得到球形LiNi0.8Co0.15Al0.05O2材料。X射线衍射结果表明,LiNi0.8Co0.15Al0.05O2材料为α-NaFeO2相。扫描电镜结果表明,材料颗粒形貌为球形。热重分析结果表明合成LiNi0.8Co0.15Al0.05O2的主反应温度在700～750℃之间。振实密度测试结果表明,750℃下制备的LiNi0.8Co0.15Al0.05O2材料可达2.2g·cm-3。恒流充放电结果表明,该材料在0.5mA·cm-2电流密度下,在3.0～4.3V间的首次充电容量可达210.3mAh·g-1,首次放电容量为179.7mAh·g-1,充放电效率为85.4%。与采用以β-Ni0.85Co0.15(OH)2为前驱体合成的LiNi0.85Co0.15O2和Al掺杂的LiNi0.8Co0.15Al0.05O2相比,尽管其首次放电容量与放电效率都有所降低,但循环性能有所提高,50周期后容量仍为初始容量的89.5%。研究表明,以球形Al/Co部分取代α型Ni(OH)2作为前驱体为球形氧化镍钴铝锂材料的制备提供了一条新的途径。     

共沉积铝镍氢氧化物的结构及电化学特性

为了改善Ni(OH)2的电化学性质,提高锌镍电池的充放电性能,用化学共沉淀法合成了混合铝镍氢氧化物Ni/Al(OH)x.用XRD和FTIR表征了Ni/Al(OH)x样品的晶体结构及IR光谱特征;测试了用Ni/Al(OH)x为正极活性物质的Zn/Ni实验电池的充放电性能.研究结果表明:所合成的Ni/Al(OH)x具有α-Ni(OH)2的晶体结构;Ni/Al(OH)x活性物质在充放电过程中主要为γ/α循环,以Ni/Al(OH)x作为正极活性物质的Zn/Ni试验电池具有优良的循环性能,其最高放电比容量为379mA·h/g.     

镍氢电池正极大电流充放电性能及最佳配方

采用化学共沉淀法制备了镍铝和钴铝2种层状氢氧化物[ Ni4Al(OH)10]OH和[Co4Al(OH)10]NO3.将前者作为电极活性材料,后者及石墨作为正极导电添加剂,通过单纯形重心设计研究了正极中3种物质的最佳配比,使其大电流充放电性能得到有效地提高.结果表明,电极的性能与电极配方密切相关.当[ Ni4Al(OH)...     

Selective decoration of nickel and nickel oxide nanocrystals on multiwalled carbon nanotubes

A simple route to selective decoration of nickel and nickel oxide nanocrystals on multiwalled carbon nanotubes (MWCNTs) using nickel acetylacetonate (NAA) was successfully achieved for the first time. The homogeneously decorated nanocrystals on MWCNTs were investigated for their structure and morphology by various techniques, such as powder X-ray diffraction, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, transmission electron microscopy, field emission scanning electron microscopy and thermogravimetric analysis. It was found that the size distributions of the nanocrystals on MWCNTs ranged from 8 to 15 nm and they were well resolved. The precursor, NAA, was effectively employed to impregnate the MWCNTs, which on calcination at suitable temperatures and in the presence of hydrogen and nitrogen atmosphere gave rise to nickel and nickel oxide nanocrystals, respectively.     

Characterizations of nickel mesh and nickel foam current collectors for supercapacitor application

Nickel (Ni) current collectors having a three-dimensional and porous structure are considered attractive contestants for high-efficiency supercapacitors. Therefore, Ni current collectors have a unique architecture and outstanding electrochemical properties. This study reports the effect of electrochemical characterizations on the electrochemical behavior and physical properties of Ni mesh and Ni foam. Cyclic voltammetry (CV) and galvanostatic charge discharge (GCD) are used to examine the electrochemical properties and life span of the Ni mesh and Ni foam as a current collector in a supercapacitor application. Structural and microstructural characterizations are performed to verify the formation of an oxide layer after 1000 cycles of CV analysis. Results show that Ni foam can increase the yield electrochemical performance of the supercapacitor. Ni foam present better efficiency (35 F g⁻¹) compared to the Ni mesh (12 F g⁻¹) at 10 mV s⁻¹ scan rate by using 2 mg imaginary mass of active material. This result shows that Ni foam has good electrochemical performance and reversibility, higher pseudocapacitance, weaker polarization, and enhance rotating performance as to Ni mesh. The porous structure of Ni foam is in control for improving of the electrochemical properties, therefore, the electrochemical region was increased and shortened ion diffusion. Structural analysis shows that Ni mesh and Ni foam are oxidized after the electrochemical analysis and transformed to nickel oxide hydroxide (NiOOH). Higher specific surface area between the electrode and electrolyte leads to excellent electrochemical and pseudocapacitive performance of the Ni foam compared to the Ni mesh, even if the materials of current collectors are the same. Hence, the physical structure of the current collectors have a critical part in improving the energy density of the supercapacitor.     

A quartz crystal microbalance study on a metallic nickel electrode

Electrochemical processes taking place on a Ni electrode have been investigated with the electrochemical quartz crystal microbalance. At potentials negative of ca. –500 mV vs. SCE, a closed frequency loop is observed without irreversible changes in the mass of the electrode. The phase transition - -Ni(OH)₂, taking place at potentials positive to –500 mV vs. SCE, is accompanied by an irreversible increase in the mass of the electrode. When Ni(OH)₂ is further oxidized, the frequency increase is followed by a decrease, indicating the transport of various species in both directions, i.e. from and into the electrode. During the Ni(OH)₂ oxidation reaction the transport of species responsible for the mass increase is slower than the charge transfer process.Contribution to the 3rd Baltic Conference on Electrochemistry, GDASK-SOBIESZEWO, 23–26 April 2003. Dedicated to the memory of Harry B. Mark, Jr. (February 28, 1934–March 3rd, 2003)     

Spectrophotometric determination of aluminium and nickel

A simple spectrophotometric method, based on the complexes with xylenol orange (XO) and EDTA, is presented for the rapid determination of aluminium and nickel, respectively, in synthetic samples of hydrotalcite. The method only requires the solubilization in sulphuric acid of the inorganic material before the ligand addition. Under optimum conditions, the complexes Al-XO and Ni-EDTA showed maximum absorption at 554 nm and 380 nm, respectively. The method obeyed Beer's law in the concentration range 0.14-1.8 microg mL(-1) of aluminium, and 30-2730 microg mL(-1) of nickel. Molar absorptivities were 2.45 x 10(4) and 14.85 L mol(-1) cm(-1) while Sandell's sensitivities were 1.1 x 10(-3) and 3.9 microg cm(-2) for aluminium and nickel, respectively. The standard addition technique was used and the recoveries obtained revealed that the proposed procedure shows good accuracy.     

Study of the decomposition of supported nickel acetylacetonate by thermal techniques

The decomposition of supported nickel acetylacetonate (AcacNi) was studied by using thermal techniques to evaluate the nature of the calcination products. Thermogravimetric techniques used in this work indicated transformations occurring during preparation and calcination steps. Results demonstrated the important influence of support modifications upon the catalyst nature finally obtained.     

Hydrothermal synthesis of nickel hydroxide nanostructures in mixed solvents of water and alcohol

Nickel hydroxide nanosheets and flowers have been hydrothermally synthesized using Ni(CH₃COO)₂·4H₂O in mixed solvents of ethylene glycol (EG) or ethanol and deionized water at 200 °C for different time. The phase and morphology of the obtained products can be controlled by adjusting the experimental parameters, including the hydrothermal time and the volume ratio of water to EG or ethanol. The possible reaction mechanism and growth of the nanosheets and nanoflowers are discussed based on the experimental results. Porous nickel oxide nanosheets are obtained by heating nickel hydroxide nanosheets in air at 400 °C. The products were characterized by using various methods including X-ray diffraction (XRD), fourier transform infrared (FTIR), transmission electron microscopy (TEM), selected-area electron diffraction (SAED), field emission scanning electron microscopy (FESEM). The electrochemical property of β-Ni(OH)₂ nanosheets was investigated through the cyclic voltammogram (CV) measurement.     

泡沫镍及负载型镍催化剂制备纳米碳纤维层的研究

纳米碳纤维可用在催化材料、储氢材料、及纳米电子器件等方面。本文对用泡沫镍及负载型镍催化剂催化分解乙烯或丙烯制备纳米碳纤维进行了研究。利用X射线衍射仪、物理吸附仪、扫描电镜进行了分析表征,并考察了催化剂、碳源、生长温度对纳米碳纤维生长量、形貌、结构的影响。结果表明:在生长温度450℃,乙烯流率30mL/m in的条件下,负载型镍催化剂纳米碳纤维的生长量要高出泡沫镍3~6倍,负载型镍催化剂制备的纳米碳纤维直径为40~60纳米,小于泡沫镍的情况。泡沫镍催化分解乙烯制备纳米碳纤维时,纳米碳纤维的生长量和平均直径随温度的降低而逐渐减小。纳米碳纤维在泡沫镍上的最低生长温度为420℃,在低于480℃生长纳米碳纤维时泡沫镍的骨架结构不会被破坏,由此制备的纳米碳纤维在新型结构催化材料中有很好的的应用前景。     

Arylcyanation of alkynes catalyzed by nickel

A nickel catalyst prepared from Ni(cod)₂ and PMe₃ is found to effect arylcyanation reaction of alkynes, namely, cleavage of a C-CN bond of an aryl cyanide followed by addition of each fragment across an alkyne. A wide range of functional groups in aryl cyanides tolerated the catalysis, giving variously functionalized β-arylalkenenitriles stereoselectively.     

Tris(triphenylphosphan)nickel(0)-Komplexe mit Nitril-Liganden

Tris(triphenylphosphane)nickel(0) Complexes with Nitrile Ligands . Synthesis, properties and reaction behaviour of (Ph₃P)₃Ni(η¹-NCR) (R = PhCH₂, 2-MeC₆H₄, Me₃Si) complexes as well as the X-ray structure of (Ph₃P)₃Ni(η¹-NCSiMe₃) are described. With NC(CH₂)_nBr (n = 1, 2) instead of the analogous nitrile complexes (Ph₃P)₂NiBr₂ and CH₃CN or C₂H₅CN respectively are formed.     

Surfactant-assisted polyol preparation of nickel powders with different morphologies

Sub-micrometer nickel powders of controlled size and morphology were produced by a surfactant-assisted polyol method, using ethylene glycol (EG) as solvent and reductant in the presence of sodium dodecyl sulfate (SDS) surfactant and NaOH. The resultant Ni powders were characterized by XRD, SEM, EDS, and FTIR. Spherical, hexagonal, and triangular fcc Ni powders from 0.30 to 0.60 μm were obtained in the presence of SDS; irregular spherical fcc Ni powders were obtained in its absence. The concentrations of SDS, NaOH and Ni(CH₃COO)₂·4H₂O greatly influence the product morphology and size.