Fabrication of Low-cost Screen-printed Electrode in Paper Using Conductive Inks of Graphite and Silver/Silver Chloride

The fabrication of the Screen-Printed Electrode (SPE) was performed using the graphite ink to print the working (WE) and counter electrodes (CE), and silver/silver chloride path as reference electrode (RE). All the electrodes are printed in a paper substrate using screen-printing technique. The resulting SPE is characterized using scanning electron microscopy, showing all the ink layer, and subsequently optimized. The paper sample presented the cellulose fibers entanglement, extremely rough, with highly porous network. Then the graphite ink was deposited and the surface became flat, thinner and very smooth. When the silver ink was painted on top of the graphite ink, the spherical silver particles, ranged from 2–3.5 μm in size, were observed. And finally, the silver ink was covered with a AgCl layer and the particle size becomes larger with an irregular sphere-like phase. The images showed that the layers appear to be homogeneously distributed with good coverage. Then fabrication process was optimized concerning type of paper, the sanding process, the hydrophobic barrier, the electrode design and size. In summary, the optimized values included using the previously sanded matte paper with a mineral spirit layer. The design and size of the electrode were also tested to achieve the best electrochemical performance (design 3 with 3.5 cm). The final SPE was a miniaturized and flexible paper-based electrochemical electrode. In order to evaluate the electrical properties, the ohmic resistance of each ink was tested using a multimeter and the obtained values were 2.18 kΩ for the graphite ink, 2.27 Ω for the silver ink and 38.33 kΩ for the silver/silver chloride ink. That can indicate the good conductivity of each ink used in the fabrication of the electrode and the correct deposition of Ag/AgCl. Finally, the electrode was used to measure the electrochemical response of K₄[Fe(CN)₆] in different concentrations. Then a calibration curve was obtained from the voltammograms and a linearity was observed between the current and concentration in the range of 0.50–2.00 mM. That indicates that the SPE has potential to be used as a voltammetric electrode.     

Determination of Amino Acids at a Silver Oxide/Silver Phosphate Electrode and the Analysis of Structure‐Response Relationships

When a silver electrode is conditioned in a solution of 0.5 M sodium hydroxide with added sodium phosphate and using a dual pulse (500 mV/750 mV vs. Ag/AgCl), a stable silver(I)/silver(II) oxide surface is formed. It has been previously shown that various moieties react with the silver(II) oxide in a chemical oxidation at the outer surface of the oxide layer. This is then followed by re‐oxidation of the silver with the generation of current at approximately 500 mV relative to the silver/silver chloride electrode. Previously we found the need to remove carbon dioxide from the base and condition the electrode in a solution containing phosphate ion in order to provide mechanical stability to the oxide layer. We have previously shown this electrode to be applicable to the detection of a variety of carbohydrates. The applicability of the silver oxide/silver phosphate electrode to the post‐chromatographic amperometric detection of amino acids was investigated. Calibration studies of amino acids representative of the various classes demonstrated good sensitivity and linearity in the 1–100 μM range. Responses of amino acids were measured using glucose as an external standard, in order to correct for variability of the oxide layer. Relative responses of the amino acids ranged from 3 down to 0.1. Correlation with structure suggested the importance of absorption in determining the rate of oxidation. Comparison of arginine with n‐benzoyl‐L ‐arginine ethyl ester indicated that side chains as well as the backbone amino group can be oxidized. A Levitch plot of alanine was shown to be linear from approximately 30 to 300 radians per second spin rate at a scan rate of 50 mV per second. Application to post‐chromatographic detection was demonstrated.     

Development of a micro-planar Ag/AgCl quasi-reference electrode with long-term stability for an amperometric glucose sensor

This paper reports a micro-planar Ag/AgCl quasi-reference electrode (QRE) with long-term stability which is characterized by both long-term potential stability and practical immunity to interference species, and which has been applied for use with an amperometric glucose sensor for plasma glucose. For fabrication, we coated a silver/silver chloride (Ag/AgCl) electrode first with γ-aminopropyltriethoxysilane (γ-APTES) and then with perfluorocarbon polymer (PFCP). Tests demonstrate the new electrode’s ability to remain stable over an 82-day period in 150 mM KCl, and also show its imperviousness to the effects of interference species (1 mM KI and 1 mM KBr), pH, and serum. Furthermore, in tests for glucose concentrations in plasma samples, a good correlation coefficient, 0.954 (n=30, Y=1.02X+0.20), was demonstrated between results obtained with a clinical analyzer and those obtained with an amperometric glucose sensor that used the developed Ag/AgCl QRE, showing that the Ag/AgCl QRE functions well as a reference electrode for plasma samples.     

Characterization of Silver Flake Lubricants

There is a thin layer of organic lubricant on commercial silver (Ag) flakes that are widely used as the fillers in electrically conductive adhesives (ECAs). This lubricant layer highly affects the properties such as conductivity of the ECAs. Therefore, understanding the behavior of Ag flake lubricant layer is essential for developing high performance ECAs. This work is aimed at studying the chemical nature of the lubricant layer, interaction between the lubricant layer and Ag flakes, and thermal behavior of the lubricants during heating. A blank Ag powder is ball-milled into Ag flakes with five fatty acids that have different carbon–hydrogen chain length as lubricants. After lubrication, the Ag flakes are studied using scanning electron microscopy (SEM), differential scanning calorimetry (DSC), and thermogravimetry (TG), and diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS). It is found that (i) Ag flakes lubricated with fatty acids of different chain lengths have exothermic DSC peaks and mass losses at different temperatures, (ii) the lubricant layer on the lubricated Ag flake surfaces is a salt formed between the acid and Ag, and (iii) exothermic DSC peaks (in air) of a lubricated Ag flake is probably due to the oxidation of lubricant layer on the Ag flake surface. This revised version was published online in July 2006 with corrections to the Cover Date.     

Improvement of the silver/silver chloride reference electrode and its application to pH measurement

When a silver/silver chloride (Ag AgCl ) reference electrode was used continuously in a low conductivity solution or reductive solution, it was often observed that stability of the liquid junction potential was lost. This phenomenon was remarkable with a Ag AgCl reference electrode compared to a calomel reference electrode. We found that 340 mg l(-1) of silver was dissolved in 3 M potassium chloride (KCl) internal solution as silver complex ions (AgCl(-(x-1))(x)) for x = 2 or 3. However, only 1.93 mg l(-1) of silver chloride (AgCl) can theoretically be dissolved in water. The complex ion that effused into the sample solution through the liquid junction clogged the liquid junction (e.g. porous ceramic) as AgCl, or as metallic silver (Ag) in reducing solution. Therefore, the constant effusion of KCl internal solution was inhibited, and the liquid junction potential became unstable or fluctuating. A new reference electrode was developed, which can eliminate AgCl(-(x-1))(x) in 3 M KCl internal solution by the use of chelating resins. A combination of this reference electrode with a pH electrode made long-term stable pH measurements possible.     

Investigation of a Thin‐film Quasi‐reference Electrode Fabricated by Combined Sputtering‐evaporation Approach

This paper presents the development of a thin‐film quasi‐reference electrode (tQRE), which was fabricated by sputtering silver (Ag) on a conducting gold layer. The Ag layer was subsequently covered by silver chloride (AgCl) with the aid of e‐beam evaporation. The functionality of the tQREs as reliable reference electrodes was confirmed by observing the potential response in solutions with various chloride ion concentrations. The influence of solution pH on the potential change of the tQREs was evaluated. In the solution with controlled ionic strength, the tQREs were able to provide stable and consistent potential outputs. Experimental investigation of the electrochemical sensors with integrated tQREs demonstrated potential applicability of the tQREs to be incorporated into miniaturized and disposable lab‐on‐a‐chip sensors for point‐of‐care/in‐situ measurements.     

Preparation of stable aqueous conductive ink with silver nanoflakes and its application on paper‐based flexible electronics

A new kind of stable aqueous conductive ink with silver nanoflakes was developed, which was also used to fabricate conductive patterns on weighing paper for flexible electronics by direct writing. Silver nanoflakes of different sizes were characterized by transmission electron microscopy. The physical properties of the conductive ink were investigated by a dynamic contact angle system, Ubbelohde viscometer, and a surface tension instrument. Conductive properties of paper‐based conductive patterns were also investigated by 4‐point probe, scanning electron microscopy, X‐ray diffraction and Uscan explorer with a 3D profilometer system. It is demonstrated how the formulation of conductive ink affects the surface morphology, microstructure conductivity, and line width of conductive patterns. It can be obtained that the paper‐based conductive patterns have low resistivity. Especially, when the sintering condition is 200 °C for 20 min, the resistivity can be down to 9.4 μΩ?cm. The application of the ink on an antenna for radio frequency identification was also studied. Copyright © 2011 John Wiley & Sons, Ltd.     

基于原位体积加成制备导电线路的研究

本文提出一种制备导电电路的方法。以纳米铜为导电填料，以光固化树脂为连接剂，制备含铜光固化油墨，利用丝网印刷方法获得含有纳米铜的图案，利用铜与银盐间的置换反应，将铜纳米粒子图案通过原位体积加成转化为导电银图案。研究结果表明，铜图案不具有导电性，而置换反应生成的银图案具有导电性，且导电能力受铜含量、银盐浓度、光照时间、浸泡反应时间等因素影响，本实验中获得的最高电导率为1.25×10⁵ S/m，导电线路具有良好的耐弯曲、耐疲劳性能，同时兼具优异的可修复性能，为导电线路的制备提供了常温下简单有效、成本低廉的实现方法，具有重要的参考价值。     

In-Situ Formation of AgCl Nanocrystallites in Films Prepared by the Sol-Gel and Silver Nanoparticles in Silica Glass Films

We are reporting on a novel preparation of silver chloride in sol-gel silica films as a precursor for nanoparticles of silver. The precipitation of silver chloride particles in-situ was achieved by the reaction of silver nitrate with trichloroacetic acid. The reaction leads to a slow release of chloride leading to a controlled precipitation of AgCl. The existence of an isotropic crystalline AgCl phase in the glass films was demonstrated by X-rays Diffraction Analysis (XRD) and Scanning Electron Microscope and Energy Dispersive Analysis of X-rays (SEM-EDAX). The resulting films are of good optical quality and exhibit a strong coloration upon irradiation with sunlight or heating to 600°C, due to the reduction of AgCl to silver nanoparticles. The absorption spectra of the films before and after irradiation are shown.     

Ink‐Jet Printing of Metallic Nanoparticles and Microemulsions

Summary: Two types of ink‐jet inks are presented: ink containing an aqueous dispersion of silver nanoparticles and an oil‐in‐water microemulsion‐based ink. The metallic ink contains nanoparticles of silver, which are formed in the presence of an ionic polymeric stabilizer. Sintering of the printed image obtained with the use of such silver‐based inks at temperatures as low as 300 °C results in formation of patterns possessing noticeable conductivity. The microemulsion inks are based on a thermodynamically stable microemulsion, in which the dispersed oil phase is a volatile solvent containing a water‐insoluble colorant. After contact of the jetted ink droplets with a substrate, nanodroplets of the microemulsion are converted into nanoparticles of the solubilized colorant. In some cases, it was found that the evaporation of microemulsion ink droplets leads to formation of rings composed of ordered nanoparticles.

Scheme of ink‐jet printing of an oil‐in‐water microemulsion followed by conversion of the nanodroplets into nanoparticles, caused by quick evaporation of the solvent within the microemulsion droplets. Therefore, the ink behaves as a dye‐based ink prior to printing, but after printing it behaves like a pigment‐based ink.     

Polyaniline/Silver Nanoparticle-Doped Multiwalled Carbon Nanotube Composites

A simple method was used to synthesize the hybrid nanocomposites consisting of the functionalized multiwalled carbon nanotube composites (MWCNTs) with the polyaniline incorporated silver nanoparticles (a-MWCNT/PANI-Ag) through an emulsion polymerization at room temperature in order to enhance the electrical conductivity of polyaniline. The electrical conductivity of the composite with the incorporated Ag nanoparticles was 5% higher than the same weight percent for the composite without Ag nanoparticles, and the thermal stability was dramatically increased from 54% for the composite (a-MWCNT/PANI) to 69% through the incorporation of the Ag nanoparticles at 830°C. Additionally, the advantages of the Ag nanoparticles, including the improved electrical and thermal properties without damage to the polyaniline structure, were confirmed using FTIR and Raman spectroscopy.     

银包玻珠核壳复合粒子的表面处理及环氧导电胶的电性能

以化学还原法合成的银包玻珠核壳复合粒子(Ag/GM)为原料, 乙二胺为表面处理剂, 制备了表面吸附有乙二胺的Ag/GM, 并用它作为导电填料组成了导电胶. 与化学还原法直接合成或沸水处理的Ag/GM相比, 乙二胺处理的Ag/GM能更有效地分散在环氧树脂胶黏剂中, 且能与环氧树脂基体产生化学键合, 降低Ag/GM和环氧树脂基体间的界面能, 用其制备的导电胶的导电率较高, 导电渗滤阈值较低. 同时, 结合导电网络理论和等效电路图, 阐明了用乙二胺处理的Ag/GM作填料制备的导电胶具有较低体积电阻率的原因.     

一种全固态扑尔敏电极的研制

制备了以脲醛树脂为框架，以ＫＣｌ粉末为活性组分的Ａｇ／ＡｇＣｌ固体电极。结果表明该电极具有相当好的稳定性并能用于扑尔敏制剂的含量测定。     

Synthesis of Ag_2S nano-sized clusters and their chemical sensitizations in AgCl cubic and {100} tabular microcrystal imaging systems

1 Introduction Since the 1990s, silver chloride {100} tabular grain emulsion has attracted much attention from research-ers working in different enterprises all over the world, such as Eastman Kodak[1―5], Agfa-Gavaert[6,7] and the Lucky Group Company in …     

新型氮杂环卡宾银(I)配合物的合成及其晶体结构

以取代苄氯(1a~1c)为起始原料,与咪唑经氮烷基化反应制得苄基咪唑氯盐(2a~2c); 2a~2c与氧化银经原位去质子化反应合成了3种新型的氮杂环卡宾银配合物--(NHC)AgCl［NHC: 1,3-二(4-甲氧基苄基)咪唑-2-亚基(3a), 1,3-二(3-甲氧基苄基)咪唑-2-亚基(3b)］和［(NHC)AgCl]₂［NHC=1,3-二(4-氯苄基)咪唑-2-亚基(3c)］,其结构经¹H NMR, ¹³C NMR, IR,元素分析和X-射线单晶衍射表征。3a~3c单晶结构均属单斜晶系,3a为P2₁/n空间群,3b和3c为P2₁/c空间群,3a和3b为单核银配合物,3c为双核银配合物。     

Solid Contact Nitrate Ion‐Selective Electrode Based on Ionic Liquid with Stable and Reproducible Potential

A simple, fast and cheap method of preparation of solid contact nitrate ion‐selective electrode is proposed. The electrode membrane phase consist of only three components: PVC, plasticizer and ionic liquid (IL).The ionic liquid trihexyltetradecylphosphonium chloride is used in triple function as ionophore, as lipophilic ionic component in order to reduce membrane resistance, and as transducer media in order to stabilize the potential of internal Ag/AgCl electrode. The electrical properties of the membrane were studied by electrochemical impedance spectroscopy and the influence of the interfacial water film was evaluated by potentiometric water layer test.     

银纳米线的制备及电催化还原氧性能研究

分别以聚乙烯基吡咯烷酮(PVP),乙二醇作为软模板和还原剂,采用不同晶种(AgCl、Ag)快速合成了银纳米线.通过SEM和TEM表征,证明合成银纳米线材料形貌均一,颗粒含量很少.并且发现以AgCl为晶种合成的银纳米线长径比为200左右(SNWH),而以Ag为晶种合成的长径比为30左右(SNWL).以银纳米线作为电催化氧...     

硫化银/凹凸棒的Ag+选择电极

以硝酸银、凹凸棒石和硫代乙酰胺为原料制得硫化银/凹凸棒-Ag₂S/ATT电极,并探讨了硫代乙酰胺配比、增塑剂用量、膜厚度以及溶液pH值等因素对电极性能的影响. 结果表明,新型银离子选择电极有较好的能斯特响应,其响应斜率48.0 mV·decade^-1,Ag⁺浓度线性响应范围1.0×10^-1 ~ 1.0×10^-6 mol·L^-1. 在pH = 2.0 ~ 8.0溶液中该电极电势可稳定72 h,对常见阳离子如Na⁺、Ca²⁺、Fe²⁺、Cu²⁺等呈现较强的抗干扰能力.     

核酸对氯化银胶体溶液共振光散射的猝灭作用及其应用

报道了一种测定水溶液中核酸的方法,该法基于核酸对氯化银溶胶共振射光的猝灭作用。在理想测定条件下,散射光的猝灭程度正比于核酸的浓度,三种核酸（ｃａｌｆ ｔｈｙｍｕｓ ＤＮＡ,ｈｅｒｒｉｎｇ ＤＮＡ ａｎｄ ＹｅａｓｔＲＮＡ）的线性范围分别为０－２０μｇ／Ｌ,０－６０μｇ／Ｌ和０－８０μｇ／Ｌ,检测限分别为０．６５μｇ／Ｌ,１．１μｇ／Ｌ和１．９μｇ／Ｌ。６种合成样品的测定结果令人满意,机理研究结果表明,核酸中的碱基（尤其是嘌呤碱）同银离子具有很强的结合能力,这种结合影响了氯化银的沉淀平衡,导致了氯化银溶胶共振散射光的猝灭。     

Ag纳米粒子在TiO2四棱柱阵列上的可控生长及其SERS效应

采用水热法在导电玻璃FTO导电面上沉积TiO₂四棱柱阵列; 并以其为基体, 分别采用聚乙烯基吡咯 烷酮(PVP)还原Tollens试剂以及柠檬酸三钠(TSC)还原硝酸银溶液, 将Ag纳米粒子(AgNPs)沉积在TiO₂四棱柱阵列上形成TiO₂@AgNPs-PVP和TiO₂@AgNPs-TSC微纳结构作为表面增强拉曼散射(SERS)基底. 实验结果表明, Ag纳米粒子在TiO₂四棱柱阵列上的尺寸和分布可通过改变Tollens试剂的浓度和TSC还原硝酸银溶液的反应时间来调控, 进而优化基底的SERS灵敏度. TiO₂@AgNPs-PVP微纳结构对罗丹明6G(R6G)的检出限为10^-12 mol/L, 对低活性小分子三聚氰胺的检出限为0.01 mg/mL; TiO₂@AgNPs-TSC微纳结构对R6G的检出限为10^-10 mol/L, 对三聚氰胺的检出限为0.01 mg/mL. TiO₂@AgNPs-PVP和TiO₂@AgNPs-TSC微纳结构基底的SERS活性、 循环可回收性与还原剂种类紧密相关: 包覆在Ag纳米粒子上的PVP可以作为隔离层避免Ag纳米粒子直接接触, 防止电磁场耦合作用减弱, 增强基底的SERS活性; 同时, PVP是一种水性聚合物, 有较强的亲水性, 作为循环可回收SERS基底使用时, 吸附小分子物质清洗难度较大.