氟硼酸镀液二氧化铅电沉积

研究了在氟硼酸或其掺杂镀液中于Pt基底电沉积PbO2镀层的电化学和结构性质.循环伏安测试、XRD分析和SEM形貌观察表明,BF4-可提高二氧化铅电沉积速率;电沉积的PbO2晶型为β-PbO2;F-、Fe3+共掺杂影响晶体生长的择优取向及镀层形貌,电沉积的FB/F-Fe-PbO2镀层整齐致密;电沉积过程增大电流密度可改变生长晶面取向.     

添加剂对离子液体中电沉积金属钴的影响

在含有氯化钴的室温离子液体氯化1-甲基-3-乙基咪唑(EMIC)和乙二醇(EG)体系中,采用扫描电子显微镜(FE-SEM）、阴极极化曲线、循环伏安及X射线衍射等方法研究了添加剂对电沉积金属钴的影响。结果表明,在EMIC-EG-CoCl₂熔盐中加入丁炔二醇能够有效地改善钴镀层的外观质量,丁炔二醇的加入量在0.3～0.7 g·L^-1范围内,能够得到银灰色、具有金属光泽的良好镀层。从FE-SEM照片可以看出,在EMIC-EG-CoCl₂熔盐中加入丁炔二醇后,使金属钴的结晶变得更加细致;阴极极化曲线表明,丁炔二醇的加入不仅增大了阴极极化,而且还消除了钴的欠电势沉积;循环伏安测试证明,添加剂的加入对阴极沉积过程有阻化作用;XRD分析证实,丁炔二醇的加入使金属钴的衍射峰变宽,晶粒尺寸为纳米级。     

镍钨硼合金电沉积机理及镀层微晶尺寸

应用循环伏安、恒电位阶跃和X射线衍射 (XRD)等方法研究了Ni_W_B合金电沉积特点和镀层微晶尺寸 .结果表明 ,在以柠檬酸铵为络合剂的溶液中 ,Ni_W_B合金沉积层较Ni_W合金有较低的电化学活性 .电位阶跃i～t曲线分析表明 ,在玻碳电极上Ni_W_B合金电结晶过程遵循扩散控制瞬时成核三维成长模式 ,且随过电位的增加 ,电极表面晶核数增多 .XRD测试结果表明 ,随沉积电流密度提高 ,合金镀层微晶尺寸逐渐增大 ,说明电流密度提高将更加有利于Ni_W_B合金电结晶过程中的晶核生长 .     

(110)晶面全择优取向Cu镀层的制备及其条件优化

研究了添加剂聚乙二醇(PEG)、氯离子(Cl－)和电流密度对Cu的电沉积过程的影响, 着重探讨了制备(110)晶面全择优取向Cu镀层的电沉积条件及其形成机理. 循环伏安(CV)结果表明, PEG阻化Cu的电沉积, Cl－加快Cu的电沉积速率. XRD实验结果表明, PEG和Cl－在一定浓度范围有利于(110)晶面择优取向; 这两种不同特性的添加剂的协同作用可以制得(110)晶面全择优取向的较薄的Cu镀层; 所制备的全择优Cu镀层较稳定. 全择优取向Cu镀层形成的机理在于PEG和Cl－吸附过程联合起作用, 在不同晶粒的不同晶面进行选择吸附, 改变了晶面的生长速率及晶粒的快生长方向.     

2,2′-联吡啶在化学镀铜中的作用研究

研究了以次磷酸钠作还原剂的化学镀铜体系,添加剂2,2′-联吡啶对化学镀铜沉积速率、次磷酸钠阳极氧化和铜离子阴极还原、以及镀层形貌、结构和组分存在状态的影响.结果表明,2,2′-联吡啶对化学沉积起阻化作用.电化学线性伏安扫描实验显示,镀液中加入2,2′-联吡啶,次磷酸钠的氧化峰电势有所负移,但峰电流减小;铜离子的还原峰电势负移,但峰电流逐渐增大.扫描电子显微镜(SEM)、能量色散谱(EDS)、X射线衍射(XRD)及X射线光电子能谱(XPS)等实验分别表明,添加剂使镀层致密和光亮、镍含量降低;镀层为Cu-Ni合金,呈面心立方结构,无明显晶面择优取向现象;镀层中铜和镍以金属态存在,磷的质量含量小于0.05%.     

非晶/米晶Ni-Mo-Ce合金镀层结构及其催化析氢性能

在Ni-Mo合金镀液中添加适量的CeCl3溶液,获得了非晶+纳米晶混合结构的Ni-Mo-Ce合金镀层。用X射线衍射(XRD)和扫描电镜(SEM)测试技术研究镀层结构及其表面形貌。实验结果表明,随着Ce含量的增加,镀层中Mo元素含量有所提高,而Ni元素含量有所降低;镀层的显微硬度先增加后降低,当Ce加入量为2 g.L-1时,显微硬度最高。电解实验表明,Ni-Mo-Ce合金具有比Ni-Mo合金更优异的耐蚀性能和良好的催化析氢性能。     

非晶态Ni-Ce-P合金的共沉积与耐蚀性能

采用恒电位沉积、循环状安等方法研究了在水溶液中电沉积稀土合金的可能性 ,首次在含有CeCl3的弱酸性NaH2 PO2 镀液中获得了不同铈含量的Ni Ce P合金镀层 ,XPS、AES、XRD和SEM等实验技术表征了镀层的组成和结构 ,极化电阻和腐蚀电位的测试数据表明此镀层与Ni P无定形合金相比 ,具有更强的耐腐蚀能力 ,同时 ,讨论了沉积条件与镀层耐蚀性能的关系 ,结论是 :镀层中铈含量越高 ,其耐腐蚀性能越好 ,此外还对Ni Ce P的共沉积机理进行了初步探讨 ,指出在所研究的电沉积条件下 ,Ni Ce P合金共沉积可以用“诱导共沉积理论”合理解释     

钇对Zn-Fe合金镀层耐蚀性的影响

电镀液中加入钇盐,在A3钢表面电镀Zn-Fe合金薄膜,研究了钇对Zn-Fe合金镀层耐蚀性能的影响.用线性扫描伏安法和交流阻抗法,研究Zn-Fe合金镀层在30℃0.20 mol·L-1H2SO4溶液中的腐蚀行为.用XRD和SEM研究zn-Fe合金镀层在腐蚀前后的微观结构和形貌的变化.结果表明:加入钇盐,能改变Zn-Fe合金镀层的晶面择优取向和织构系数,使结晶粒度变小,且低晶面指数的晶面耐蚀性较好;当加入钇盐量为0.60 g·L-1时,镀层变得均匀、致密,电结晶生长形态变为层状;镀层的致钝电流密度(ipp)和维钝电流密度(ip)降低显著,极化电阻Rp增大,获得的Zn-Fe合金镀层的耐蚀性能最好.     

主盐浓度和工艺条件对Sn-Ag-Cu合金镀层组成和形貌的影响

在弱酸性镀液中电沉积得到无铅Sn-Ag-Cu可焊性合金镀层。采用X射线荧光光谱仪(XRF)和扫描电子显微镜(SEM)研究了镀液中主盐浓度和电镀工艺条件对镀层的组成和形貌的影响。研究表明,Sn-Ag-Cu合金的电沉积是正则共沉积。镀液中Sn²⁺和Ag⁺浓度改变对镀层晶粒大小影响较大,Cu²⁺浓度的改变对镀层的平整度影响较大。电流密度增加、pH值下降、温度降低,都能使镀层结晶细致。     

CO3^2-对羟基乙叉二膦酸镀铜液的影响

研究羟基乙叉二膦酸（HEDPA）镀铜液中CO3^2-含量对电沉积时阴、阳极过程及镀层的择优取向的影响.通过分析阴、阳极的动电位极化曲线,发现镀液中逐渐加入的CO23-提高了阴极的极化,使电结晶晶粒细化,直至达到稳定;同时促进了铜阳极的溶解.而X射线衍射（XRD）结果表明,铜镀层的晶面择优取向从（222）逐渐向（111）转变.通过镀液中固体络合物的红外光谱分析表明,CO3^2-的加入以第二配体的方式进入该镀液的放电络合离子结构中,参与Cu2＋的络合,形成更稳定的络合物,从而导致铜沉积电位负移,镀层（111）晶面取向增强.     

双金属Ag-Cu枝晶的制备及应用

通过铜箔基体上电沉积泡沫铜结合伽尔瓦尼置换反应制备出了银-铜(Ag-Cu)纳米枝晶, 利用X射线衍射(XRD)和场发射扫描电子显微镜(FE-SEM)对枝晶的成分及形貌进行研究发现, 随着沉积过电位的增加, 铜的前驱体形貌由棒状到枝晶状, 最后发展为泡沫状, 但泡沫状的前驱体制备的Ag-Cu 枝晶却是最规整和致密的. 另外, 银离子的浓度也会影响枝晶的形貌, 一定范围内浓度的增加有利于枝晶的形成. 通过线性扫描伏安和电流-时间曲线对制备的Ag-Cu 枝晶催化性能进行表征, 在电解质溶液中, -0.25 V(相对于饱和甘汞电极(SCE))时有一个明显的双氧水(H₂O₂)还原峰, 这意味着Ag-Cu枝晶对H₂O₂的电还原具有较好的催化活性, 当该电极被用于双氧水传感器时, 电流响应快, 能在3 s 内达到稳态电流, 线性测量范围为0.1-12 mmol·L^-1, 灵敏度可以达到330.36 μA·(mmol·L^-1)^-1·cm^-2, 这点对于提高传感器的准确性非常重要.     

Coulometric Determination of Trace Silver in Surfactant-Containing Solutions

The voltammetric behavior of silver in redox reactions [Ag(I) Ag(0)] on a platinum-gauze electrode was studied to select the optimum conditions for the potentiostatic coulometric determination of silver in 10^–6–10^–5 M solutions in the presence of surfactants using the oxidation of silver electrochemically predeposited on the electrode. The determination error and the relative standard deviation varied from 0.5 to 6%, depending on the concentration of silver. The inhibiting effect of surfactants on the rates of silver deposition and dissolution decreased as their concentration was decreased by the repeated dilution of the initial solution and by their removal at the sample preparation stage and as the potentials and times of silver electrodeposition and electrodissolution were changed. The mode of alternating cathodic and anodic polarization of the electrode provided the complete deposition and dissolution of silver; in this mode, silver(I) could be determined from a single portion of the solution many times. The procedure was applied to the determination of silver in drugs and cosmetic and photographic materials.     

离子液体中电沉积制备钴纳米线阵列

Porous anodic alumina (PAA) was used as a template to prepare Co nanowires array from 1-ethyl-3-methylimidazolium chloride ionic liquid by direct current method. The surface morphology of porous anodic alumina template was observed by field emission-scanning tunneling microscopy (FE-SEM) before and after the electrodeposition of Co nanowires. The electrodeposition of Co nanowires was characterized by transmission electron microscopy (TEM) and X-ray powder diffraction (XRD). TEM results indicate that the Co nanowire surface is coarse and porous when aqueous solution was used as electrolyte， and the Co nanowire deposited from the ionic liquid is uniform and smooth. XRD results show that the electrodeposition of Co is a mixture of crystal and microcrystal phase.     

Membrane extraction and electrodeposition of silver(I) in systems with di(2-ethylhexyl) hydrogen phosphate

Extraction of silver(I) from nitric acid solution by electrodialysis with liquid membranes containing di(2-ethylhexyl) hydrogen phosphate with addition of tri-n-octylamine in 1,2-dichloroethane is studied. The effects of the composition of aqueous solutions and liquid membranes as well as of the basic parameters of electrodialysis on the Ag(I) transport and electrodeposition rates are examined, and the process conditions are optimized.     

Microstructure and corrosion behavior of electroless deposited Ni-P/CeO2 coating

Electroless Ni-P/nano-CeO2 composite coating was prepared in acidic condition, and its microstructure and corrosive property were compared with its CeO2-free counterpart. Scanning electronic microscopy （SEM） and X-ray diffraction （XRD） spectrometer were used to examine surface morphology and structure of the as-plated coating. Differential scanning calorimeter （DSC） and transmission electronic microscopy （TEM） were used to study the coating＇s phase change at high temperature. The coating＇s corrosive behavior in 3%NaCl ＋ 5%H2SO4 solution was also investigated. The results showed that Ni-P coating had partial amorphous structure mixed with nano-crystals, while the Ni-P/CeO2 coating had perfect amorphous structure. In high-temperature condition, Ni3P precipitation and Ni crystallization took place in both coatings but at different temperatures, while the Ni-P/CeO2 coating had sintered phase of NiCe2O4 spinels. The anti-corrosion property was better in the CeO2-containing coating, and this was due to its less liability to undergo local-cell corrosion than its CeO2-free counterpart. Ni-P/CeO2 coating＇s pure amorphous structure was the result of Ni＇s hindered crystal-typed deposition and P＇s promoted deposition.     

Effect of hydrodynamic conditions on the silver electrodeposition from water-ethanol solutions of electrolytes

Effect of hydrodynamic conditions on the silver electrodeposition from the aqueous and water-ethanol solutions of silver nitrate is studied with the purpose of the establishing the process limiting step nature. In the investigated systems of the silver electrodeposition in the potentiodynamic regime the current strength depends on the intensity of stirring and is changed due to the change in the limiting step and the surface morphology. Adding of nonaqueous solvent to the larger extent influences the electrolytic rather than diffusion stage of the process.     

Nanostructured polyamic acid membranes as novel electrode materials

This paper describes a new approach for the preparation of polyamic acid (PAA) composites containing Ag and Au nanoparticles. The composite film of PAA and metal particles were obtained upon electrodeposition of a PAA solution containing gold or silver salts with subsequent thermal treatment, while imidization to polyimide is prevented. The structural characterization of the films is provided by 1H NMR and Fourier transform infrared spectroscopy (FTIR), while the presence of metallic nanoparticles within the polymeric matrix was confirmed by scanning electron microscopy (SEM), cyclic voltammetry (CV), energy-dispersive X-ray analysis (EDX), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). This approach utilizes the unique reactivity of PAA by preventing the cyclization of the reactive soluble intermediate into polyimides at low temperature to design polymer-assisted nanostructured materials. The ability to prevent the cyclization process should enable the design of a new class of electrode materials by use of thermal reduction and/or electrodeposition.     

A facile and simple method for the preparation of copoly(TEAMPS/VP)/silver nanocomposites for the humidity-sensing membranes

We developed a simple method for the preparation of polyelectrolyte/silver nanocomposites, where silver nanoparticles were dispersed in a polyelectrolyte. Copoly(TEAMPS/VP)/silver (w/w=100/0, 100/1, 100/2, 100/3 and 100/4) nanocomposites were obtained by a thermal decomposition reaction of silver carbamate complex at 130 degrees C, and well-dispersed silver colloids were stabilized by copolymer of tetraethylammonium 2-acrylamido-2-methyl-1-propanesulfonate (TEAMPS) and N-vinylpyrrolidone (VP). A dark brown solution in its UV-vis absorption spectrum showed surface plasmon resonance absorption bands at 420 nm in solution. The silver precursor and the resulting polyelectrolyte/Ag nanocomposite was characterized by differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), X-ray diffraction (XRD), infrared (IR), transmission electron microscopy (TEM). In addition the humidity-sensing properties using copoly(TEAMPS/VP)/Ag nanocomposite films were examined.     

316L钢表面纳米银镀层的制备、性质及血液相容性

采用恒电位电沉积方法在316L不锈钢表面沉积银纳米镀层, 并将钢板置于全氟硅烷溶液中浸泡, 通过动态凝血实验、 抗凝血时间测定、 血小板黏附实验、 溶血实验和蛋白吸附实验等手段, 测试材料的血液相容性. 结果表明, 通过上述方法可明显改善316L不锈钢的血液相容性, 而抗凝血性能、 溶血率及纤维蛋白吸附量不亚于裸钢板. 与316L裸不锈钢相比, 银镀膜全氟硅烷浸泡316L不锈钢具有良好的血液相容性, 是一种比较理想的冠状动脉支架材料, 具有良好的应用前景.     

Ag／TiO2复合纳米催化剂的制备和表征及其光催化活性

 采用光还原沉积贵金属法，制备了Ag／TiO2复合纳米催化剂．通过调节溶液的pH值控制TiO2表面负载银的形貌，利用AAS，XRD，TEM和XPS等手段对样品进行了表征．以苯胺氧化为模型反应，考察了Ag／TiO2复合纳米催化剂样品的光催化活性以及银沉积量和沉积形貌对催化剂活性的影响．结果表明，通过调控光还原沉积条件，可在平均粒径为24nm左右的TiO2颗粒上获得3nm左右均匀分散的银粒子；在TiO2上沉积适量的具有较高分散度的金属Ag，能有效提高TiO2对苯胺氧化反应的光催化活性．