浮法玻璃下表面渗锡的X射线光电子谱

利用X射线光电子谱仪（X-ray photoelectron spectroscopy,XPS）对国内外浮法玻璃样品（样品A和样品B）下表面渗锡情况进行了对比分析。结果表明：在浮法玻璃下表面900nm范围内,2种样品中的锡离子在渗锡面均以Sn^0,Sn^2＋,Sn^4＋ 3种价态存在,Sn^2＋在整个渗锡量中均占最大比例。在近表面区,渗锡均以Sn^2＋态为主,Sn^0和Sn^2＋含量之和均占到总渗锡量的90％以上,且样品A渗锡量远远高于样品B的渗锡量。样品A的不同锡离子相对含量沿深度变化较大,而样品B的不同锡离子相对含量沿深度变化小于1％。结合扫描电子显微镜形貌观察可知：钢化虹彩现象是由钢化处理中,Sn^2＋转变为Sn^4＋的氧化反应导致的体积膨胀引起的。在该反应过程中单胞体积增大3％。综合XPS与钢化虹彩实验结果可知,XPS分析可以有效而精确地提供浮法玻璃中锡的价态以及含量信息。     

电镀制备铟-锡合金电极及其电还原二氧化碳性能

以腐蚀铜网为基体,在硫酸盐镀液中制备得到用于电还原CO2的铟-锡合金电极。对镀液配方进行了筛选,并通过正交试验对镀液配方进行优化,得到制备铟-锡合金电极的最佳工艺条件为:In2(SO4)350g/L,SnSO430g/L,柠檬酸40g/L,添加剂TSNA4g/L,稳定剂3g/L,电流密度1.5A/dm2,温度25°C,pH约1.5。最佳工艺下制备的In-Sn合金镀层呈均匀的灰白色,结合力良好,In-Sn合金电极上电还原CO2生成甲酸的电流效率达71%,稳定性良好。     

锡镍镀液中Sn^2＋和Ni^2＋离子浓度的伏安测定

采用ＤＺ－１Ｂ型电镀添加剂测定仪测定锡镍合金镀液中主盐的浓度，实验结果表明，应用玻碳电极和汞膜电极可快速测定合金镀液中Ｓｎ＾２＋和Ｎｉ＾２＋离子的浓度，操作简便，适用于电镀车间生产的现场监控。     

碱性铜锡合金镀液中游离氢氧化钾含量的自动电位滴定

研究了碱性铜锡合金镀液中用自动电位滴定法测定游离氢氧化钾的条件和方法。实验结果表明,以pH复合电极为指示电极,设定滴定终点为pH=11.52时,共存的氰化钾和酒石酸钾不干扰测定。方法具有较高的准确度和精密度,而且操作简便快捷,7 m in内能打印出分析结果。     

锡铋合金电镀工艺条件的研究

锡铋合金镀层因具有无晶须、熔点较低、可焊性好等优点,在国外已大量推广应用,在国内的研究和应用则较少。本文通过条件实验和正交试验对硫酸盐锡铋合金电镀液配方进行了改进。研究了镀液中稳定剂、平滑剂、光亮剂、表面活性剂含量及操作条件对镀液及镀层性能的影响。结果表明,该镀液稳定、易操作,且获得的Sn-Bi合金镀层均匀致密、光亮、结合力及钎焊性优良。得到合适的工艺条件为：镀液中稳定剂含量1．5～2ml／L、平滑剂含量0．5～1g／L、光亮剂含量8～10ml／L、表面活性剂含量3g／L、pH值0．9～1．1、阴极电流密度1A／dm^2。     

微电子封装化学镀镍工艺研究及应用

在微细图形上实施化学镀有一定的技术难度,尤其是在批量生产中。通过研究工艺条件对镀层的影响,探索出微电子封装化学镀镍的工艺参数的适宜范围分别为:23～27g/L的镍盐、4～6g/L的还原剂、pH值4 5左右、温度(90±2)℃。经试验筛选出合适的镀液稳定剂Tl2+,使批量生产的封装微细图形不"糊片",无镍粒。用X射线荧光测厚仪及化学分析方法对生产过程中的镀液成分进行测定,确定了维护镀液所用的补充液的组分,从而延长了镀液的使用寿命,满足了微电子封装批量生产的要求。     

化学镀Ni-Sn-P合金镀层的研究与应用

用化学镀的方法获得了Ni-Sn-P非晶态合金镀层。给出了镀层的技术指标和检测方法,并与Ni-P镀层进行了比较。分析得出,该镀层有较高的耐蚀性、焊接性、延展性、结合力、修复性,性能优于Ni-P合金镀层。分析了Sn^2 对Ni-Sn-P合金镀液与镀层性能的影响,给出了Sn^2 与Ni-Sn-P合金镀层非晶态与耐蚀性、延展性、焊接性、压应力、抗氧化性、镀层颜色的关系。介绍了Ni-Sn-P合金镀液的管理与维护,包括技术要求,化学材料和水质的选择,工作温度、pH值、镀液寿命、装载量、镀速和镀层质量的控制,镀液的补充与添加,Ni^2 的分析方法等。Ni-Sn-P合金镀层为钢铁件防腐提供了一种全新的防护技术,在各行业中均有应用,具有广泛的应用前景。     

镀黑色锡镍合金溶液中氯化镍的光度法测定

在较大的pH值范围内,EDTA与镍离子生成稳定的蓝色络合物,利用这一特性,用EDTA分光光度法测定镀黑色锡镍合金溶液中氯化镍的质量浓度。以水作参比液,在波长590 nm处测定吸光度。实验表明,在pH≈4的条件下,镀液中的氨分子对测定无影响,铜离子和铁离子对测定的影响一般可以忽略不计。本法相对平均偏差为0.71%,回收率为100.4%-100.8%。     

镍—铁合金刷镀液性能及工艺参数

一镍-铁合金刷镀液的性能镍-铁合金刷镀液是由镍盐、铁盐、缓冲剂、稳定剂以及光亮整平剂、润湿剂、镀层增韧剂等组成的金属有机络合物的水溶液.1 镍-铁合金刷镀液呈浅绿色、腐蚀性极小,施镀过程中无异味,pH为3.8,使用过程中无需调整pH值,可以一直把镀液消耗完为止.耗电系数C值为0.093A.h/dm~2μm.2 沸点测试方法:将待测镀液置沸点仪中,用小火加热观察沸点,大气压775.8mmHg镍-铁合金刷镀液沸点 100.2℃快速镍刷镀液沸点 99.5℃     

交流示波极谱滴定法测定镀液中铜,锡,镍

介绍了交流示波极谱法测定镀铜－锡－镍合金镀液中铜、锡、镍含量的新方法。该方法采用汞膜电极、钨电极下的配位滴定法，连续测定镀液中的铜、锡、镍离子的含量。方法简便、快速、终点直观，结果准确。     

航空胶片稳定处理的研究

稳定处理是代替黑白航空胶片常规加工中定影和水洗的处理技术。本文以硫氰酸盐为重点 ,研究了稳定剂的种类、浓度、温度、PH值、缓冲溶液等对稳定处理效果的影响。     

XRD studies of the phase composition of the electrodeposited copper-rich Cu-Sn alloys

Studies of the phase and chemical compositions as well as of the surface morphology of Cu-Sn alloys electrodeposited in the sulphate solution containing laprol were carried out using the XRD, SEM, and EDX techniques. The multiphase composition—pure copper, the α-CuSn phase and the intermediate hcp phase were determined to be present in the deposits obtained at cathode potentials positive to that of the reversible of the Sn/Sn²⁺electrode. When the content of Sn in the deposit was higher than 12-13 at.%, the β and/or δ phases were determined to be present along with that mentioned above. The deposit obtained at the potentials negative to that of the reversible of the Sn/Sn²⁺ electrode presented the δ phase with low quantities of the pure Cu and α-CuSn phases. The grain size of deposits increased with the cathode potential until it was positive to that of the reversible of the Sn/Sn²⁺ electrode. The presence of Br⁻ ions in the solution hindered the granular electrocrystallization and reduced the Sn proportion in the alloy. It was assumed that underpotential deposition (UPD) of Sn on copper could be responsible for the formation of the multiphase composition and the intermediate hcp phase. It was concluded that the brightness of the studied Cu-Sn coatings was conditioned by the surface morphology.     

Influence of ethylene glycol,ethanol and formic acid on platinum and ruthenium electrodeposition on carbon support material

Carbon supported Pt–Ru catalysts were prepared by potentiostatic deposition at −0.5 V from H₂PtCl₆ + RuCl₃ in H₂SO₄ solution in the presence of ethylene glycol (EG), ethanol (EtOH) and formic acid (HCOOH) as stabilizing agents. The active surface area of the Pt–Ru catalyst was determined by Cu-UPD. The highest value was obtained with HCOOH added, followed by EtOH, and EG. SEM and AFM images showed that the mean particle size of the Pt–Ru nanoparticles was three or four times smaller in the presence of a stabilizer. Electrocatalytic activity measurements indicated that the most active electrode for methanol electrooxidation was obtained with EtOH as additive, followed by EG. The electrode prepared with HCOOH additive gave lower catalytic activity than that without stabilizing agent.     

Sn~(4+)修饰的PEG-Pd催化氯代硝基苯选择性加氢反应

考察了PEG-Pd(PEG:聚乙二醇,Pd 0.2%)催化剂催化对氯硝基苯的加氢反应中,添加第二金属组分以及Sn4+含量对反应的影响。结果表明,添加一定量的Sn4+对反应选择性有着显著的影响。不添加Sn4+离子,会有严重的脱氯反应发生;加入Sn4+离子后,在Sn与Pd的摩尔比为0.8,温度60℃,氢压1.0 MPa的条件下,经过60 min反应,对氯硝基苯转化率为99.6%,而对氯苯胺选择性由不加Sn4+离子时的68.5%上升到96.1%。对取代位置不同的其它氯代硝基苯,该催化体系同样表现出很高的催化活性和氯代苯胺选择性。     

In(acac)_3和Sn(acac)_2Cl_2的合成及表征

介绍了化学法制备氧化铟锡(ITO)纳米材料的两个重要合成原料In(acac)3和Sn(acac)2Cl2的合成方法。以InCl3·4H2O为原料,在pH值为9.0的柠檬酸溶液中制备In(acac)3;以SnCl4·5H2O与乙酰丙酮为原料,在甲苯溶剂中加热回流制备Sn(acac)2Cl2。通过IR、NMR、XRD检测手段对合成的产物进行表征分析。讨论了各种实验条件对合成反应的影响,总结出In(acac)3的最佳合成条件是:柠檬酸浓度为84 mmol·L-1,pH值为9.0;制取Sn(acac)2Cl2的最佳溶剂是甲苯。     

Oxygen reduction on ultra thin carbon supported polymeric phthalocyanine electrodes in 6 N KOH

Oxygen reduction on carbon supported polymeric iron, manganese and mixed Fe/Sn and Fe/Cu phthalocyanines has been examined in 6 N KOH, using the Vogel Lundquist ultra-thin electrode technique. Activity of samples prepared by gas phase in situ methods is 2–3 times greater than that observed for phthalocyanines precipitated from solution. While a reduced performance of mixed polyphthalocyanines occurs on introduction of Cu, introduction of Sn causes no change in activity up to 50% Sn.Results are examined as a function of support material. Current densities on the untreated supports are higher than on the corresponding supported catalyst in the diffusion region. This effect is interpreted by a superficial distribution of the catalyst.     

ZSM-5沸石分子筛吸附模拟废水中对苯二酚的研究

以正硅酸乙酯为硅源、偏铝酸钠为铝源、四丙基氢氧化铵为模板剂,利用水热合成法制备ZSM-5沸石分子筛并将其应用到吸附水中对苯二酚的研究,考察了吸附时间、对苯二酚溶液pH值、吸附温度、吸附剂用量对吸附效果的影响。结果表明,最佳吸附条件是:吸附温度为35℃,吸附时间为60 min,对苯二酚溶液pH值为6,吸附剂用量为0.4 g。此时,对苯二酚的去除率最高,达到了68.28%。     

Participation of the dissolved O2 in the passive layer formation on Zn surface in neutral media

The composition of the passive layers formed on Zn electrode in naturally aerated and de-aerated 0.1 M KClO₄ solution were studied using X-ray photoelectron spectroscopic measurements (XPS). A correlation between the presence of dissolved O₂ and the formation of an interior passive layer was carried out. Librated Cl⁻ from the perchlorate reduction reaction was detected in its solutions during Zn electrode polarization. The librated Cl⁻ concentration reached its maximum value at −1.4 V. Moreover, in the studied potential range the perchlorate reduction rate increases in absence of dissolved oxygen. Chrono-amperometry and electrochemical impedance spectroscopy (EIS) were performed for the stationary and the rotating disc Zn electrodes in naturally aerated and de-aerated 0.1 M KClO₄ solution. EIS technique showed a change in the electrode impedance with the experimental conditions as a result of changing the reactions occurring in the electrode vicinity. The obtained data were fitted to three different equivalent circuits depending on the electrode potential. The protective nature of the passive layers formed in different experimental conditions was found to decrease with rotating the electrode and de-aerating the solution.     

The effect of the Zn/Sn ratio on the formation of single phase kesterite Cu2ZnSnS4 solar cell material

The effect of the Zn/Sn ratio in the solution on the properties of Cu₂ZnSnS₄ films prepared by sol-gel method has been investigated. As the Zn/Sn ratio in the solution increases to a certain value, a pure single phase kesterite CZTS is obtained and confirmed by XRD, XPS and Raman. Through controlling the Zn/Sn ratio in the solution, secondary phases such as SnO₂ can be avoided and an optimal condition for single phase kesterite CZTS can be achieved. Surface SEM images of the CZTS films are investigated and the optical band gap of the optimized CZTS film is found to be 1.23 eV.     

Advanced structures in electrodeposited tin base anodes for lithium ion batteries

A novel composite anode material consisted of electrodeposited Sn dispersing in a conductive micro-porous carbon membrane, which was directly coated on Cu current collector, was investigated. The composite material was prepared by: (1) casting a polyacrylonitrile (PAN)/dimethylformamide (DMF) solution that contained silica particles on a copper foil, (2) removing the solvent by evaporation, (3) dissolving the silica particles by immersing the copper foil into an alkaline solution, (4) drying the copper foil coated by micro-porous membrane, (5) electrodepositing Sn onto the copper foil through the micro-pores in the micro-porous membrane, and (6) annealing as-obtained composite material. This method provided the composite material with high decentralization of Sn and supporting medium purpose of conductive carbon membrane deriving from pyrolysis of PAN. SEM, XRD and EDS analysis confirmed this structure. The characteristic structure was beneficial to inhibit the aggregation between Sn micro-particles, to relax the volume expansion during cycling, and to improve the cycleability of electrode. Galvanostatic tests indicated the discharge capacity of the composite material remained over 550 mAh g⁻¹ and 71.4% of charge retention after 30 cycles, while that of the electrode prepared by electrodepositing Sn on a bare Cu foil decreased seriously to 82.5 mAh g⁻¹ and 13%. These results show that the composite material is a promising anode material with larger specific capacity and long cycle life for lithium ion batteries.