Electrodeposition of Pb-free Sn alloys in pulsed current

A pulsed electrodeposition method is applied to the preparation of Pb-free Sn alloys solder bumps for flip-chip bonding with the aid of a photolithography. Sn-Ag alloy films with near eutectic compositions (Sn-3.5% Ag) were obtained using a pyrophosphate-iodide plating baths regardless under direct or pulsed current. The composition and the morphology of electrodeposits were examinated by SEM and X-ray photoelectron spectroscopy (XPS). The main results revealed that the organic additives affect the electrochemical reduction of tin-silver and the direct consequence on making Sn-Ag alloy is a decreased deposition rate. However, the addition of additives in the plating bath suppressed the dendritic tin-silver growth by adsorption on the deposited surface. Pulsed electrodeposition is shown to be an interesting approach to elaborate bumps with smooth and homogeneous surfaces.     

Metabolite characterisation in peritoneal dialysis effluent using high‐resolution 1H and 1H–13C NMR spectroscopy

Metabolite analysis of peritoneal dialysis (PD) effluent may provide information regarding onset and progression of complications associated with prolonged PD therapy. In this context, the nuclear magnetic resonance detectable small metabolites of PD effluent samples were characterised using high‐resolution ¹H and ¹H–¹³C NMR spectroscopy. The various spectra were recorded (at 800 MHz proton frequency) on PD effluent samples obtained after 4‐h (intraperitoneal) dwell time from patients with end‐stage renal failure and continuing normally on PD therapy. In spite of devastating spectral feature of PD effluent due to the presence of intense resonances from glucose and lactate, we were able to identify 53 small endogenous metabolites (including many complex coupled spin systems) and more than 90% of the total CH cross peaks of ¹H–¹³C heteronuclear single‐quantum correlation spectrum specific to various metabolites of PD effluent. We foresee that the characteristic fingerprints of various metabolites of control PD effluent samples will be used to identify and distinguish metabolic differences from PD‐related complications. Copyright © 2014 John Wiley & Sons, Ltd.     

Electrochemical impedance spectroscopy and X-ray photoelectron spectroscopy study of the corrosion behaviour of galvanized steel and electroplating steel

The efficiency of a formula containing 2-{(2-hydroxyethyl)[(4-methyl-1H-1,2,3-benzotriazol-1-yl)methyl]amino}ethanol (tolyltriazole) and decanoic acid as corrosion inhibitor for galvanized steel and electroplating steel in aqueous solution have been determined by electrochemical impedance spectroscopy (EIS) techniques. The experimental data obtained from this method show a frequency distribution and therefore a modelling element with frequency dispersion behaviour, a constant phase element (CPE) has been used. The corrosion behaviour in the presence of different concentration of decanoic acid (DA) in the formula was also investigated by EIS. Results obtained reveal that, the formula is a good inhibitor for galvanized steel and electroplating steel in aqueous solution, the better performance was obtained in the case of galvanized steel. The ability of the inhibitor to be adsorbed on the surface was dependent on the nature of metal. X-ray photoelectron spectroscopy surface analysis with inhibitor shows that it's chemisorbed at the galvanized and electroplating steel/aqueous solution interface.     

Determination of cyclophosphamide and ifosfamide in sewage effluent by stable isotope-dilution liquid chromatography-tandem mass spectrometry

A reliable and specific method was developed for the determination of the cytotoxic drugs cyclophosphamide and ifosfamide in sewage effluent. The most successful combination was found to be Strata-X solid-phase extraction followed by Florisil^® clean-up with analysis by liquid chromatography–tandem mass spectrometry. Quantification by internal standardisation was achieved using custom synthesised d4-cyclophophosphamide. The mass spectrometer was operated in highly selective reaction monitoring (HSRM) mode, which significantly reduced matrix noise and improved sensitivity. Although it suffered from some ionisation suppression, electrospray ionisation (ESI) was found to give an order of magnitude better sensitivity in terms of limit of detection than atmospheric pressure chemical ionisation (APCI). Using final effluent from two different sewage treatment plants, the method was validated following official European guidelines and shown to be a high performance tool for routine analysis at the sub-nanogram per litre level. Depending on the matrix, the limit of detection for cyclophosphamide was between 0.03 ng/L and 0.12 ng/L and for ifosfamide between 0.05 ng/L and 0.09 ng/L. For cyclophosphamide the accuracy and precision, tested at 1.7 ng/L, were 98–109% and ≤13%, CV respectively. For ifosfamide the accuracy and precision, tested at 1.1 ng/L, were 98–113% and ≤15% CV, respectively. Depending on the sample matrix the absolute recovery of the internal standard was between 57% and 70%. The method was tested by analysis of spot samples taken from the final effluent discharges of two sewage treatment plants; the first using a conventional trickling filter treatment process and second employing activated sludge followed by ultra violet treatment. Cyclophosphamide was detected at 0.19 ng/L at the first plant and at the second detected at 3.7 ng/L and 3.5 ng/L, before and after the UV treatment process; ifosfamide was not detectable at either plant.     

Comparison of Chemometric and Chromatographic Methods to Obtain Kinetic Parameters for Textile Dyes during a Biodegradation Process

The concentrations of three industrial-grade textile dyes were determined in a mixture after degradation by the fungus Ganoderma sp, by using the methods of UV-Vis spectrophotometry associated with Partial Least Squares regression and HPLC and comparing the results obtained from both methods. Using the concentrations calculated from the two methods, a kinetic study of the biodegradation mediated by the fungus was performed. The rate constants and the activation energies for this transformation were obtained for each dye in the mixture. The concentration of Remazol Blue R ESP could be determined by the HPLC method, and the value obtained was comparable with the result using the Partial Least Squares regression method. The Partial Least Squares regression method offers advantages over the HPLC method for the quantification of dyes in textile effluents, as it provides the kinetic parameters of the biodegradation reaction.     

基于应力分析的电镀保护光纤布喇格光栅传感性能分析(英文)

为保护光纤光栅,提出了一种镀层和光纤光栅结合良好的无粗化过程的化学镀和电镀保护方法.基于应力分析法,得到镀镍光纤光栅的温度灵敏度公式,采用ANSYS有限元软件分析了电镀后光纤光栅应力随温度变化关系,并进行了实验证实.结果表明:光纤光栅电镀后温度灵敏度理论和实验值分别为20.6951pm/℃、22.076pm/℃.理论分析和实验、仿真结果基本一致.相比裸光纤光栅,温度灵敏度增加到原来的2.2倍.该方法不仅可以获得厚度理想的保护层,还可以提高光纤光栅的温度灵敏度.     

Multisyringe flow injection analysis system for automation of standard addition calibration method

In the present work, the multi-channel features of multisyringe flow injection analysis (MSFIA) were exploited for the first time to implement calibration based on standard addition method (SAM). For this, standard solutions containing different concentrations of target analyte were placed in each syringe of the multisyringe and connected to a flow network where in-line mixing of sample and standard through a merging zone approach was established prior to detection of analyte. Using this strategy, artifacts reported before in SAM using flow injection analysis were avoided as the concentration of the analyte in the resulting mixture was related to the dilution of sample and added standard within the system, and the concentration of all matrix components was kept constant during all measurements. The feasibility of the proposed MSFIA system was assessed through application to potentiometric determination of chloride ion in electroplating bath and milk samples. Results obtained for samples (n = 15) were not statistically different from those provided by titrimetric procedures, with an excellent throughput (20–31 samples h^{− 1}), comprising four-level addition of chloride ion.     

Preparation of Sn films deposited on carbon nanotubes

In this work carbon nanotubes were first grown on copper substrate by chemical vapor deposition method. The Sn deposits were then deposited on the surface of as-grown carbon nanotubes by three different methods: electroplating, electroless plating and displacing methods. The Sn deposits on CNTs surface were characterized by both scanning electron microscope and field emission scanning electron microscope. The compositions of Sn deposits were analyzed by energy dispersive X-ray spectroscope. The results showed that both electroless plating and displacing deposits can but the electroplating deposits cannot cover on the surface of CNTs. Besides C, Sn, Ni and Pd, the electroless deposits also contain element of oxygen and the displacing deposits also contain elements of copper and oxygen.     

Adsorption of cadmium and lead from palm oil mill effluent using bone-composite: optimisation and isotherm studies

The adsorption of Cd and Pb ions from palm oil mill effluent on a mesoporous-activated cow bone composite powder has been investigated. Adsorbent was developed from cow bones, coconut shells and zeolite. The composite examined in the present work has a BET surface area of 248.398 m²/g. The optimisation of the removal efficiency of the heavy metals was investigated using central composite design and analysed using response surface methodology. The analysis of variance of the quadratic model signified that the model suitably predicted the uptake of the heavy metal ions at a 95% confidence level. The optimal operating condition was recorded at pH 4, 50 rpm, within 24 h and 1 mm of particle size and 12.5 gL^?1 of adsorbent dosage. The characteristics of the composite were investigated using the Fourier transform irradiation. The morphology and chemical composition of composite was examined using the scanning electron microscopy equipped with energy dispersive x-ray. Characterisation study was conducted before and after the adsorption process. The results obtained illustrated that the removal of cadmium and lead from POME was influenced by the functional groups available on the surface of the composite. The carboxyl and hydroxyl groups are mainly responsible for the removal of cadmium and lead through chelating process. The point of zero charge (pH_pzc) revealed that the adsorbent contained acidic sites with negatively charge surface which influenced the adsorption process. The experimental data of the heavy metals of Cd and Pb investigated were fitted to the Langmuir and Freundlich models. The result revealed that the adsorption equilibrium data fitted better to the Langmuir model for the adsorption Cd and to the Freundlich model for the adsorption of Pb.     

新型三维网状锡-钴合金负极材料的结构与性能

应用电沉积技术制备了三维网状结构的Sn-Co合金负极材料, 采用XRD、SEM和电化学方法考察了该负极材料的结构和性能. XRD分析表明, 该三维网状结构的Sn-Co合金镀层为六方固溶体结构. 其电化学性能测试表明: 三维网状结构Sn-Co合金微晶电极的性能稳定, 其首次放电容量高达493.4 mAh•g−1, 首次库仑效率达80.03％, 而平面结构Sn-Co合金电极的首次库仑效率为63.47％. 经50周充放电循环后, 三维网状结构Sn-Co合金电极的放电容量为329.6 mAh•g−1, 放电容量保持率为66.8％；SEM分析表明: 三维网状Sn-Co合金电极表面是由大小不一、高低不同的“岛”紧密排列在一起；“岛”和多孔结构的存在, 缓冲了锂嵌入时体积的膨胀, 部分抑制了材料结构的变化, 减缓了电极容量的衰减, 改善了电极的循环性能.