电感耦合等离子体原子发射光谱法测定人造金刚石中铁、钴、锰、镍

1引言近年来,我国人造金刚石的产量和应用有了很大的发展。以现有的人造金刚石合成技术,通常以Fe,Ni,Co,Mn等元素组成的合金作为触媒,这使人造金刚石中极易残留这些金属组成的包裹体。诸多研究表明,包裹体含量和分布情况对人造金刚石的性能有着重要影响[1]。经查阅文献,已有使用X射线荧光光谱法对人造金刚石中杂质元素含量进行半定量分析的报道[2]。电感耦合等离子体发射光谱法(ICP-AES)被广泛应用于岩矿、土壤样品中多元素分析[3]。本实验以在大气气氛中高温灰化和混合酸对样品进行前处理,采用ICP-AES测定人造金刚石中Fe,Co,Ni和Mn。本方法操作简便,处理效果良好。     

表面活性剂辅助共沉淀法制备Ni-Mg-Al固体碱催化剂用于CH_4-CO_2重整反应

采用表面活性剂辅助共沉淀法制备了Ni-Mg-Al固体碱催化剂并用于CH4-CO2重整反应,探讨了表面活性剂对Ni(111),Ni(200)晶面的择优取向作用,在800℃下比较了不同表面活性剂制备的催化剂的催化性能,详细考察了CTAB制备的催化剂CB-LDO在不同反应温度下的催化活性和稳定性.采用红外光谱、X射线衍射、程序升温还原、X射线光电子能谱、高分辨透射电镜和程序升温氧化等表征手段分析了催化剂的活性、稳定性和失活原因.结果表明,四丙基氢氧化铵(TPAOH)促进Ni(200)的生长,而聚氧乙烯-聚氧丙烯-聚氧乙烯(P123)、聚乙烯吡咯烷酮(PVP)和十六烷基三甲基溴化铵(CTAB)抑制Ni(200)晶面的生长;Ni(200)的结晶程度对CH4的活化起到关键的作用,催化剂CB-LDO在高温下反应会发生晶型的转化,Ni(200)晶面由于反应过程中生成NiAl2O4尖晶石而得到缓慢释放,使催化剂的活性得以维持较高的水平.     

Nd,Ce和La改性对Ni/SBA-15催化剂在CH4/CO2重整反应中性能的影响

以稀土金属Nd,Ce或La的氧化物为助剂,采用β-环糊精浸渍法对Ni/SBA-15催化剂进行了改性,并运用X射线衍射、N₂吸附-脱附、程序升温还原和热重等手段考察了改性的催化剂在CO₂重整CH₄制合成气反应中的催化性能. 结果表明,Nd等稀土金属氧化物的添加对催化剂孔结构和晶相结构等性质影响不大,但可影响NiO的还原; Nd的添加使NiO与载体之间以Ni-Nd-O形式相互作用,促进了活性组分NiO的还原. 其中,Nd的添加量为5-10 wt%时所制备的催化剂在重整反应中的催化活性最高,且具有很强的抗积碳性能. La和Ce氧化物促进的Ni催化剂也表现出类似的性质和催化性能.     

A novel bimediator amperometric sensor for electrocatalytic oxidation of gallic acid and reduction of hydrogen peroxide

A novel bimediator amperometric sensor is fabricated for the first time by surface modification of graphite electrode with thionine (TH) and nickel hexacyanoferrate (NiHCF). The electrochemical behavior of the TH/NiHCF bimediator modified electrode was characterized by cyclic voltammetry, differential pulse voltammetry and chronoamperometry. The TH/NiHCF bimediator modified electrode exhibited a pair of distinct redox peaks for NiHCF and TH with formal potentials of 0.33 V and −0.27 V vs. SCE at a scan rate of 50 mV s⁻¹ in 0.1 M NaNO₃ and 0.1 M NH₄NO₃ respectively. The electrocatalytic activity of the bimediator modified electrode towards oxidation of gallic acid with NiHCF and reduction of hydrogen peroxide with TH was evaluated and it was observed that the modified electrode showed an electrocatalytic activity towards the oxidation of gallic acid in the concentration range of 4.99 × 10⁻⁶–1.20 × 10⁻³ M with a detection limit of 1.66 × 10⁻⁶ M (S/N = 3) and reduction of H₂O₂ in the concentration range of 1.67 × 10⁻⁶–1.11 × 10⁻³ M with a detection limit of 5.57 × 10⁻⁷ M (S/N = 3). The bimediator modified electrode was found to exhibit good stability and reproducibility.     

Hierarchical porous nanofibers of carbon@nickel oxide nanoparticles derived from polymer/block copolymer system

The triblock copolymer (PAA-b-PAN-b-PAA) is prepared by reversible addition-fragmentation chain-transfer polymerization, and then blended with polymer (PAN) and metal hydroxide (Ni(OH)₂) as a precursor for heat-treatment. A composite material of hierarchical porous nanofibers and nickel oxide nanoparticles (HPCF@NiO) is prepared by electrospinning combined with high-temperature carbonization. The effects of the ratio of PAA and PAA-b-PAN-b-PAA on the internal structure of nanofibers and their electrochemical properties as positive electrode materials are investigated. The experimental results show that when the ratio of PAA to PAA-b-PAN-b-PAA is 1.3 to 0.4, it has good pore structure and excellent electrochemical performance. At the current density of 1 A/g, the specific capacitance is 188.7 F/g and the potential window is −1 V to 0.37 V. The asymmetric supercapacitor assembled with activated carbon as the negative electrode materials has a specific capacitance of 21.2 F/g in 2 mol/L KOH and a capacitance retention of 85.7% after 12,500 cycles at different current density.     

Synthesis,structure and electrocatalytic H2-evoluting activity of a dinickel model complex related to the active site of [NiFe]-hydrogenases

Structural and functional biomimicking of the active site of [NiFe]-hydrogenases can provide helpful hints for designing bioinspired catalysts to replace the expensive noble metal catalysts for H₂ generation and uptake. Treatment of dianion [Ni(phma)]²⁻ [H₄phma = N,N'-1,2-phenylenebis(2-mercaptoacetamide)] with [NiCl₂(dppp)] (dppp = bis(diphenylphosphino)propane) yielded a dinickel product [Ni(phma)(μ-S,S')Ni(dppp)] (1) as the model complex relevant to the active site of [NiFe]-H₂ases. The structure of complex 1 has been characterized by single-crystal X-ray analysis. From cyclic voltammetry and controlled potential electrolysis studies, complex 1 was found to be a moderate electrocatalyst for the H₂-evoluting reaction using ClCH₂COOH as the proton source.     

Thermal and dielectric studies of nickel malonate dihydrate single crystals

Single crystals of nickel malonate dihydrate were grown by the gel technique, employing the single diffusion method. Thermal dehydration of the crystal was investigated by thermogravimetric and differential thermal analyses. The title compound exhibits a steady thermal behaviour at higher temperature range of 350-800 °C. The dielectric properties of the prepared sample were analyzed as a function of frequency in the range of 1 kHz-1 MHz and at temperatures between 40 and 140 °C.     

Ni原子双飞秒脉冲激光诱导击穿光谱的信号增强研究

在大气环境下采用波长为800nm,脉宽为30fs的飞秒激光研究了Ni的双脉冲激光诱导击穿光谱,与单飞秒脉冲激光诱导击穿光谱相比,双飞秒脉冲在最优的双脉冲相对延时下,其信号强度增强接近10倍,实验研究了双脉冲相对延时在0-1300ps范围内不同延时对激光诱导击穿光谱信号强度增强因子的影响。整个相对延时区域可以分为三个阶段：在0-50ps区域内信号增强因子是一个持续增大的过程,在50ps左右,达到一个最大值;在50-300ps区域内,信号增强因子呈现出一个先下降后上升的过程;在300-1300ps,信号增强因子基本保持不变。     

Microstructure and surface mechanical properties of pulse electrodeposited nickel

The surface of carbon steel was modified by electrochemical deposition of Ni in a standard Watt's bath using dc and pulse plating electrodeposition. The aim was to compare the microstructure and surface mechanical properties of the deposit obtained by both techniques. Materials characterization was conducted using field emission scanning electron microscope fitted with scanning transmission electron detector, atomic force microscope and X-ray diffractometer. Nanoindentation hardness, elastic modulus, adhesion, coefficients of friction and wear rates were determined for both dc and pulse electrodeposits. Experimental results indicate that pulse electrodeposition produced finer Ni grains compared to dc plating. Size of Ni grains increased with deposition. Both dc and pulse deposition resulted in grain growth in preferred (2 0 0) orientation. However, presence of Ni (1 1 1) grains increased in deposits produced by pulse deposition. Pulse plated Ni exhibited higher hardness, creep and coefficient of friction and lower modulus of elasticity compared to dc plated Ni.     

Epitaxial growth of uniform NiSi2 layers with atomically flat silicide/Si interface by solid-phase reaction in Ni-P/Si(1 0 0) systems

As metal-oxide-semiconductor field-effect transistor (MOSFET) devices are shrunk to the nanometer scale, flat shallow metal/Si electrical contacts must be formed in the source/drain region. This work demonstrates a method for the formation of epitaxial NiSi₂ layers by a solid-phase reaction in Ni-P(8 nm)/Si(1 0 0) samples. The results show that the sheet resistance remained low when the samples were annealed at temperatures from 400 to 700 °C. P atoms can be regarded as diffusion barriers against the supply of Ni to the Si substrate, which caused the formation of Si-rich silicide (NiSi₂) at low temperature. Furthermore, elemental P formed a stable capping layer with O, Ni and Si during the annealing process. A uniform NiSi₂ layer with an atomically flat interface was formed by annealing at 700 °C because of the formation of a Si-Ni-P-O capping layer and a reduction in the total interface area.