Amperometric Determination of Sugars at Activated Barrel Plating Nickel Electrodes

We report amperometric determination of sugars by using a disposable barrel plating nickel electrode (Ni‐BPE) in this study. The activated Ni‐BPE possesses good reproducibility in flow injection analysis of sugars with a relative standard deviation of 3.16% for 10 consecutive injections of glucose. The electrocatalytic mechanism for the detection of sugars as well as the use as a detector in high‐performance liquid chromatography (HPLC) is investigated. We achieve a good separation of four sugars (glucose, fructose, sucrose, and maltose) in HPLC with favorable sensitivity at a detection potential of +0.55 V vs. Ag/AgCl. The results of wide linear calibration ranges and detection limits in the μM range meet the need of real sample analysis. This detection method is successfully used for quantitative determination of sugars in honey to identify its authentication.     

玻璃表面的无钯活化化学镀镍

在非金属基体上化学镀镍 ,一般要先在基体上形成一层化学镀的催化剂 ,传统工艺是采用PdCl2 SnCl2 活化 敏化法[1 ] 。该工艺处理过程复杂 ,而且使用有毒的PdCl2 ,其价格昂贵。因此无钯活化法将带来巨大的经济效益和社会效益。我们曾在这方面进行了有益的尝试 ,如将玻璃表面经喷雾热解形成ZnO ,然后吸附银盐 ,活化还原 ,再化学镀[2 ] 。李兵等[3] 研究了非金属材料无钯催化活化工艺。研究了活化时间及温度对覆盖度的影响 ,但未给出具体活化液配方。本文提出了玻璃表面的一种无钯活化镀镍液配方 ,该配方由醋酸镍、甲醇、柠檬酸钠和氨组…     

化学镀镍法制备碳纳米管

以PdCl2为活化液,用化学镀镍法制备了具有活性中心的镀镍硅模板,通过催化裂解在镀镍硅模板上制备了碳纳米管。讨论了化学镀工艺参数对镀镍硅模板表面活性中心的尺寸和分布的影响。最佳的工艺条件为:在0.17mol·L-1的SnCl2中敏化10min,0.4g·L-1PdCl2中活化2min,50℃施镀3min所得的镍粒子活性中心的粒径为200nm~300nm。用扫描电镜观察到碳纳米管为竹节形状,直径为100nm~110nm。     

碳纳米管表面的无钯活化化学镀镍研究

本文提出碳纳米管表面无钯活化的化学镀镍方法.碳纳米管经硝酸氧化和碱中和后表面生成羧基,利用羧基吸附镍离子,之后吸附的镍离子被化学还原为镍的纳米微粒并成为化学镀镍的催化活性中心.红外吸收光谱和电子显微镜观察等证实了上述活化过程的机理.实验表明,新的活化方法对碳纳米管表面化学镀是切实可行的,文中同时对化学沉积层的不同形貌进行讨论.     

Electroless Nickel Plating and Electroplating on FBG Temperature Sensor

Metal-coated fiber Bragg grating（FBG）temperature sensors were prepared via electroless nickel（EN）plating and tin electroplating methods on the surface of normal bare FBG.The surface morphologies of the metal-coated layers were observed under a metallographic microscope.The effects of pretreatment sequence,pH value of EN plating solution and current density of electroplating on the performance of the metal-coated layers were analyzed.Meanwhile, the Bragg wavelength shift induced by temperature was monitored by an optical spectrum analyzer.Sensitivity of the metal-coated FBG（MFBG）sensor was almost two times that of normal bare FBG sensor.The measuring temperature of the MFBG sensor could be up to 280℃,which was much better than that of conventional FBG sensor.     

What Does the Chemical Industry Expect from Physical and Industrial Chemistry?

Process innovation—the systematic optimization of raw materials, energy consumption and product yields—is a constant challenge for those operating plants producing vital basic and intermediate chemicals. The production processes, rather than the products themselves, exhibit life cycles and determine the profitability of downstream manufacturing. The ongoing task of interdisciplinary teams of experts is not just to develop new process routes, but, more commonly, to improve individual process steps. The impulse for this innovation arises from changes in the price and availability of raw materials, economic and environmental considerations and, last but not least, scientific and technological progress. This paper illustrates the opportunities available using examples which have already been put into practice as well as problems not yet resolved. Questions such as the use of alternative feedstocks and the switch to catalytic processes arc addressed and used to suggest novel ideals for basic research. Worthwhile projects are identified in the area of industrial oxidation, both catalytic and non-catalytic. A highly developed, systematic, computer-based method for optimizing the integration of energy flows within a plant is presented and novel measurement techniques for efficient production control and product quality are. discussed. The successful realization of such concepts requires the ability and the willingness to think in terms of new approaches to problem solving, making this an important objective for university education geared to future needs.     

镀液中金属杂质离子对电镀镍层性能的影响

向镍电镀原液中引入2 g/L的Co~(2+),Cr3+,Mn~(2+),Fe~(2+),Cd~(2+),Zn~(2+)等离子,通过电镀得到不同的镀层.X射线衍射(XRD)、X射线光电子能谱(XPS)及扫描电子显微镜(SEM)的结果表明,不同金属离子对镍沉积影响不同,金属杂质离子的存在会使镀层中晶粒尺寸变小,影响镍镀层的均匀性和致密度.通过阴极极化曲线、计时电位和交流阻抗等方法探讨了含有不同金属杂质的镀液在电镀过程中电化学行为的规律性.通过镀液的浓度梯度、耐腐蚀、耐热循环及耐高温等实验获得了不同条件下金属杂质在镀液中所允许的浓度范围.     

化学镀镍磷镀层及其耐蚀性研究

针对工业实际对提高防护层防腐、耐磨性能的要求,对化学镀镍磷镀层的方法,镀敷液配方等进行了分析,对其腐蚀率进行了测定,并对镀层性能进行了表征;讨论了影响腐蚀率的若干重要因素;对有关工艺进行了优化,从而在多种基质上获得了抗腐蚀性较好的镍磷镀层,初步研究证明,其性能优于电镀方法所获得的镀层.     

化学镀镍液中次磷酸钠在线检测仪的设计

基于次磷酸钠的化学性质和碘溶液的光谱吸收特征，将现有的分光光度计进行改造，采用流动注射光度分析法测定镀液中次磷酸钠的含量，借助于计算机控制，实现次磷酸钠的在线检测，能满足生产工艺分析的要求。     

化学镀镍过程中丙酸作用的机理研究

利用循环伏安法和红外漫反射光谱法研究化学镀镍过程中丙酸的作用机理. 不同丙酸浓度下的循环伏安曲线表明,丙酸能同时促进Ni^2＋的还原和H₂PO^-₂的氧化.根据丙酸分别与NaH₂PO₂和NiSO₄共存时镍基体上吸附物的红外漫反射光谱变化,推断丙酸是通过与NaH₂PO₂和Ni^2＋形成表面络合物来促进化学沉积的. 丙酸能与NaH₂PO₂形成分子间氢键,促使P-H键断裂并生成·PHO^-₂中间物,从而提高H₂PO^-₂的氧化速度; 同时,丙酸以其-OCO-官能团与Ni^2＋生成桥式配合物,有利于加速Ni^2＋的沉积. H₂PO^-₂氧化速度的提高有助于磷的沉积,从而增大了化学镀层中的磷含量.     

聚苯胺微管表面化学镀镍与电磁特性研究

刘建华,周新楣,李松梅. 聚苯胺微管表面化学镀镍与电磁特性研究[J]. 化学学报, 2006, 64(2): 163-168.     

以硼氢化钠为还原剂化学镀镍的电化学研究

采用线性电位扫描伏安法研究了以硼氢化钠为还原剂的化学镀镍体系, 考查了镀液组成及工艺条件对化学镀镍硼阴、阳极过程的影响, 结果表明: 乙酸镍和硼氢化钠含量的提高分别促进了Ni²⁺的还原反应和BH₄^-的氧化反应; 乙二胺、氢氧化钠以及添加剂硫脲、糖精钠对阴、阳极反应均有不同程度的抑制作用, 同时添加剂中的硫元素加速了镍的氧化; 升高温度有利于阴、阳极反应的进行.     

铝表面前处理及化学沉积镍初期行为

利用开路电位-时间(EOCP-t)曲线,研究铝表面经浸镍和化学预镀镍前处理后,化学沉积镍的初期行为;通过扫描电子显微镜(SEM)观察铝表面经前处理后的表面形貌.结果表明:未经及经前处理的铝表面,化学沉积镍的初期行为都经历去氧化膜、活化、混合控制以及化学沉积过程.经过浸镍和化学预镀镍前处理后的铝表面附着细小的镍颗粒.依据EOCP-t和SEM的最佳实验结果,在含有络合剂和还原剂的碱性预镀镍溶液中,经二次化学预镀镍前处理,成功实现铝基底弱酸性化学镀镍.所获得的化学镀镍层与铝基底结合牢固,呈团颗粒状形貌和非晶态结构.     

镍表面三维微图形的复制加工

运用约束刻蚀剂层技术(CELT)在金属镍(Ni)表面实现三维微图形加工,以规整的三维齿状微结构作模板,获得可有效CELT加工的化学刻蚀和捕捉体系,在Ni表面得到了与齿状结构互补的三维微结构并应用扫描电子显微镜(SEM)和原子力显微镜(AFM)表征刻蚀图案,证实CELT可用于金属表面Ni的三维微图形刻蚀加工．     

Molecular Thermodynamics for Chemical Process Design

Thermodynamic properties are essential for quantitative process design to produce chemical products. Caloric properties are required for heat balances, but these properties are usually available or estimated easily. More important—and often much more difficult to estimate—are the chemical potentials of components in mixtures; it is these potentials which determine phase equilibria, as required for separation operations, and chemical equilibria, as required for chemical reactors and for separation operations based on chemical reactions. Molecular thermodynamics is an engineering-oriented science for calculating the desired chemical potentials from a minimum of experimental data. This applied science, based on classical and statistical thermodynamics, yields chemical potentials through models that are based on molecular physics and physical chemistry. Selected examples are cited to illustrate the applicability of molecular thermodynamics: group-contribution methods for obtaining chemical potentials in highly nonideal mixtures as required for distillation-column and process-safety design; equation of state for precipitation of uniform-sized crystals from supercritical fluids; molecular-orbital calculations to guide process development for alternatives to environmentally dangerous chlorofluorohydrocarbons; molecular-simulation calculations for separation of gas mixtures with porous adsorbents; equilibria in two-phase aqueous systems for separation of protein mixtures; and, finally, extended polymer-solution thermodynamics to guide synthesis of hydrogels suitable for protein recovery from soybeans and for novel drug-delivery devices.     

化学镀钴和超级化学镀填充的研究进展

随着半导体集成度的不断提高,铜互连线的电阻率迅速提高。当互连线宽度接近7 nm时,铜互连线的电阻率与钴接近。IBM和美国半导体公司（ASE）已经使用金属钴取代铜作为下一代互连线材料。然而,钴种子层的形成和超级电镀钴填充7 nm微孔的技术工艺仍是一个很大的挑战。化学镀是在绝缘体表面形成金属种子层的一种非常简单的方法, 通过超级化学镀填充方式, 直径为几纳米的盲孔可以无空洞和无缝隙的方式完全填充。本文综述了化学镀钴的研究进展,并分析了还原剂种类对化学镀钴沉积速率和镀膜质量的影响。同时, 在长期从事超级化学填充研究的基础上, 作者提出了通过超级化学镀钴技术填充7 nm以及一下微盲孔的钴互连线工艺。     

介绍一种能使制备出的氢氧化亚铁长时间保持白色不变的方法

取100ml蒸馏水煮沸5分钟,趁热将其中50ml倒入盛有5gNaOH的锥形瓶中,并用移液管小心地加入15ml煤油或苯。再另取一支移液管向剩余的水中缓缓加入5ml浓H2SO4,趁热转入滴液漏斗中,并向其中加入5g无锈铁丝或还原铁粉,再慢慢加入15ml煤油或苯。实验装置见图示。待Fe与H2SO4反应完毕,打开滴液漏斗活塞,立即会看到锥形瓶中有白色絮状的Fe（OH）2生成,该白色Fe（OH）2能在数小时,乃至更长的时间里保持白色不变。     

Pentanuclear Nickel(II) Complex with two Vertex-Shared Triaminoguanidine Fragments and Symmetric Capping Ligand

The pentanuclear nickel(II) complex [Ni₅(saltag^Br)₂(tptz)₄] ( Ni5 ) with the tritopic triaminoguanidine-derived Schiff-base ligand H₅saltag^Br (1,2,3-tris[(5-bromosalicylidene)amino]guanidine) and tptz (2,4,6-tris(2-pyridyl)-1,3,5-triazine) as capping ligands is reported. Ni5 crystallizes in the triclinic space group P1 with the central nickel(II) ion linking two triangular arrangements of nickel(II) ions supported by two tritopic triaminoguanidine ligands. The octahedral coordination of the four peripheral nickel(II) ions is complemented by capping tridentate tptz ligands. By variation of the synthesis also the corresponding trinuclear nickel(II) complex [Ni₃(saltag^Br)(tptz)₃]NO₃ ( Ni3 ) is accessible. Magnetic measurements for Ni3 and Ni5 reveal a singlet ground state with antiferromagnetic coupling between the nickel(II) ions, which in the case of Ni5 can only be simulated assuming a two-J exchange coupled spin topology. For both complexes significant zero-field splitting for the nickel(II) ions is evident from the measured magnetic data, which can be verified by theoretical studies revealing a magnetic anisotropy with strong rhombic distortion due to the presence of the tptz co-ligands in both compounds.     

溶胶-凝胶技术在织物化学镀活化预处理中的应用

以γ-氨丙基三乙氧基硅烷(KH-550)为先驱体,应用溶胶-凝胶技术在织物表面形成一层凝胶薄膜.由于该薄膜含有氨基和羟基等活性基团,能与钯离子起配位络合作用,阻止钯粒子的团聚,使钯以较高的活性完成织物化学镀.扫描探针显微镜(SPM)及扫描电子显微镜(SEM)观察了施镀前后织物的表面形态.与传统的前处理相比,无需SnCl2敏化,减少污染,缩短工艺流程,降低钯盐用量.     

First Isolation and Structural Characterization of a Nickel(III) Complex Containing Aliphatic Thiolate Donors

Long overdue were syntheses of nickel(III ) complexes containing aliphatic thiolate ligands. The complex anion [Ni(phmi)]⁻ (phmi is the tetraanion of N,N′-1,2-phenylenebis(2-methyl-2-sulfanylpropionamide) has now been isolated—as PPh₄ salt—and structurally characterized. The stability of the nickel(III ) complex is attributed to the special properties of the ligand, which abolish or at least retard possible decomposition pathways.