Name: fabrication of thin film silver/silver chloride electrodes with finely controlled single layer silver chloride
Uploaded: 2020-07-01T13:00:00
Description: Watch this Scientific Journal Video about Fabrication of Thin Film Silver/Silver Chloride Electrodes with Finely Controlled Single Layer Silver Chloride at JoVE.com

这项工作得到香港研究资助理事会赞助的RGC-NSFC联合基金的资助（项目号N_HKUST615/14） 的支持。我们感谢科大纳米系统制造设施（NFF）的设备/系统制造。

1. 使用升降制造 Cr/Au 粘附层
<ol><li>旋转涂层 HPR504 正光处理器厚度为 1.2 μm，使用 1，000 rpm 的扩散速度为 5 秒，旋转速度为 4，000 rpm，为 30 s。</li>
	<li>在 110°C 下将石英晶圆上的光敏材料软烤5分钟。</li>
	<li>使用掩膜对齐器，公开晶圆，使 Cr/Au 沉积的位置暴露在紫外线 （UV） 光下。曝光功率密度和时间分别是 16 mW/cm2 和7.5 s（曝光能量密度 = 120 mJ/cm2）。</li>
	<li>通过将晶圆淹没?...

<ol>
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J., Stelzenmuller, A., Mijares, G., MacCrehan, W., Gaitan, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Ag/AgCl+microelectrodes+with+improved+stability+for+microfluidics.">Ag/AgCl microelectrodes with improved stability for microfluidics.</a> Sensors and Actuators B: Chemical. 114 (1), 239-247 (2006).</li><li>Mechaour, S. S., Derardja, A., Oulmi, K., Deen, M. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Effect+of+the+wire+diameter+on+the+stability+of+micro-scale+Ag/AgCl+reference+electrode.">Effect of the wire diameter on the stability of micro-scale Ag/AgCl reference electrode.</a> Journal of The Electrochemical Society. 164 (14), E560-E564 (2017).</li><li>Brewer, P. J., Leese, R. J., Brown, R. J. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=An+improved+approach+for+fabricating+Ag/AgCl+reference+electrodes.">An improved approach for fabricating Ag/AgCl reference electrodes.</a> Electrochimica Acta. 71, 252-257 (2012).</li><li>Safari, S., Selvaganapathy, P. R., Derardja, A., Deen, M. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrochemical+growth+of+high-aspect+ratio+nanostructured+silver+chloride+on+silver+and+its+application+to+miniaturized+reference+electrodes.">Electrochemical growth of high-aspect ratio nanostructured silver chloride on silver and its application to miniaturized reference electrodes.</a> Nanotechnology. 22 (31), 315601 (2001).</li><li>Tjon, K. C. E., Yuan, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Impedance+characterization+of+silver/silver+chloride+micro-electrodes+for+bio-sensing+applications.">Impedance characterization of silver/silver chloride micro-electrodes for bio-sensing applications.</a> Electrochimica Acta. 320, 134638 (2019).</li><li>Pargar, F., Kolev, H., Koleva, D. A., van Breugel, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Microstructure,+surface+chemistry+and+electrochemical+response+of+Ag+|+AgCl+sensors+in+alkaline+media.">Microstructure, surface chemistry and electrochemical response of Ag | AgCl sensors in alkaline media.</a> Journal of Materials Science. 53 (10), 7527-7550 (2018).</li><li>Hassel, A. 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Ag/AgCl 电极的物理特性由沉积在电极上的 AgCl 的形态和结构控制。本文提出了一个精确控制银电极表面单层AgCl覆盖的协议。协议的一个组成部分是法拉第电解定律的修改形式，用于控制薄膜银电极上的AgCl度。它可以写成：
<img alt="Equation" src="/files/ftp_upload/60820/60820eq1.jpg">
其中 X 是单个 AgCl 层的厚度（厘米（350 nm = 3.5 x 10-5厘米）;P% 是 Ag 电极表面 Ag...

Ag/AgCl电极是电化学领域使用最多的电极之一。它最常用作为电化学系统中的参考电极，因为它易于制造，无毒特性和稳定电极电位1，2，3，4，5，6。2,3,4,5,61
研究人员试图了解Ag/AgCl电极的机理。电极上的氯化盐层是含有电解质的氯化物中Ag/AgCl电极特性氧化还原反应的基本材料。对于氧化路径，电极表面的不完美位点上的银与溶液中的氯化离子结合，形成可溶性AgCl复合物，在复合物中扩散到沉积在电极表面的AgCl边缘，以AgCl的形式进行沉淀。还原路径涉及使用电极上的 AgCl 形成可溶性 AgCl 复合物。复合体扩散到银表面，并减少回元素银7,7，8。
AgCl层的形态学对Ag/AgCl电极的物理属性有着关键的影响。各种工作表明，大表面积是形成参考Ag/AgCl电极的关键，具有高可重复性和稳定的电极电位9,9、10、11、12。10,11,12因此，研究人员研究了创建具有较大表面积的Ag/AgCl电极的方法。Brewer等人发现，使用恒定电压代替恒定电流来制造Ag/AgCl电极将导致高度多孔的AgCl结构，增加AgCl层11的表面面积。Safari等人利用AgCl形成过程中在银电极表面的量传输限制效应，在银电极表面形成AgCl纳米板，显著增加AgCl层表面积12。
为传感应用设计AgCl电极的趋势正在兴起。低接触阻抗对于感应电极至关重要。因此，了解AgCl的表面涂层如何影响其阻抗特性非常重要。我们先前的研究表明，在银电极上的AgCl覆盖程度对电极/电解质接口13的阻抗特性有重要影响。但是，要正确估计薄膜 Ag/AgCl 电极的接触阻抗，形成的 AgCl 层必须平滑且具有良好的覆盖范围。因此，需要一种具有指定 AgCl 覆盖程度的平滑 AgCl 层的方法。已为部分满足这一需要而做了努力。Brewer等人和Pargar等人讨论了一个平滑的AgCl可以实现使用温和的恒定电流，制造AgCl层顶部的银电极11，14。11,卡坦等人在他们的银样品上形成了一层AgCl，并观察了单个AgCl粒子8的大小。他们的研究发现，一层AgCl的厚度在350纳米左右。这项工作的目的是开发一个协议，形成精细和控制良好的AgCl薄膜与预测的阻抗性能在银电极的顶部。

<table border="1" fo:keep-together.within-page="1" fo:keep-with-next.within-page="always">
	<tbody>
		<tr>
			<td>AST Peva-600EI E-Beam Evaporation System</td>
			<td>Advanced System Technology</td>
			<td></td>
			<td>For Cr/Au Deposition</td>
		</tr>
		<tr>
			<td>AZ 5214 E Photoresist</td>
			<td>MicroChemicals</td>
			<td></td>
			<td>Photoresist for pad opening</td>
		</tr>
		<tr>
			<td>AZ P4620 Photoresist</td>
			<td>AZ Electronic Materials</td>
			<td></td>
			<td>Photoresist for Ag liftoff</td>
		</tr>
		<tr>
			<td>Branson/IPC 3000 Plasma Asher</td>
			<td>Branson/IPC</td>
			<td></td>
			<td>Ashing</td>
		</tr>
		<tr>
			<td>Branson 5510R-MT Ultrasonic Cleaner</td>
			<td>Branson Ultrasonics</td>
			<td></td>
			<td>Liftoff</td>
		</tr>
		<tr>
			<td>CHI660D</td>
			<td>CH Instruments, Inc</td>
			<td></td>
			<td>Electrochemical Analyser</td>
		</tr>
		<tr>
			<td>Denton Explorer 14 RF/DC Sputter</td>
			<td>Denton Vacuum</td>
			<td></td>
			<td>For Ag Sputtering</td>
		</tr>
		<tr>
			<td>FHD-5</td>
			<td>Fujifilm</td>
			<td>800768</td>
			<td>Photoresist Development</td>
		</tr>
		<tr>
			<td>HPR 504 Photoresist</td>
			<td>OCG Microelectronic Materials NV</td>
			<td></td>
			<td>Photoresist for Cr/Au liftoff</td>
		</tr>
		<tr>
			<td>Hydrochloric acid fuming 37%</td>
			<td>VMR</td>
			<td>20252.420</td>
			<td>Making diluted HCl for cathodic cleaning</td>
		</tr>
		<tr>
			<td>J.A. Woollam M-2000VI Spectroscopic Elipsometer</td>
			<td>J.A. Woollam</td>
			<td></td>
			<td>Measurement of silicon dioxide passivation layer thickness on dummy</td>
		</tr>
		<tr>
			<td>Multiplex CVD</td>
			<td>Surface Technology Systems</td>
			<td></td>
			<td>Silicon dioxide passivation</td>
		</tr>
		<tr>
			<td>Oxford RIE Etcher</td>
			<td>Oxford Instruments</td>
			<td></td>
			<td>For Pad opening</td>
		</tr>
		<tr>
			<td>Potassium Chloride</td>
			<td>Sigma-Aldrich</td>
			<td>7447-40-7</td>
			<td>Making KCl solutions</td>
		</tr>
		<tr>
			<td>SOLITEC 5110-C/PD Manual Single-Head Coater</td>
			<td>Solitec Wafer Processing, Inc.</td>
			<td></td>
			<td>For spincoating of photoresist</td>
		</tr>
		<tr>
			<td>SUSS MA6</td>
			<td>SUSS MicroTec</td>
			<td></td>
			<td>Mask Aligner</td>
		</tr>
		<tr>
			<td>Sylgard 184 Silicone Elastomer Kit</td>
			<td>Dow Corning</td>
			<td></td>
			<td>Adhesive for container on chip</td>
		</tr>
	</tbody>
</table>

fabrication of thin film silver/silver chloride electrodes with finely controlled single layer silver chloride

本文旨在提出一种协议，在薄膜银电极上指定覆盖，形成光滑、可控的氯化银薄膜（Ag/AgCl）。薄膜银电极大小为 80 μm x 80 μm，160 μm x 160 μm 溅射在石英晶圆上，镀铬/金（Cr/Au）层用于粘附。经过钝化、抛光和阴极清洗过程，电极在考虑法拉第的电解定律后进行了电静氧化，形成AgCl的平滑层，在银电极上具有指定程度的覆盖。通过检查制造Ag/AgCl薄膜电极表面的扫描电子显微镜（SEM）图像来验证该协议，从而突出了协议的功能和性能。非最佳制造的电极也是为了进行比较。该协议可广泛用于制造具有特定阻抗要求的Ag/AgCl电极（例如，探测阻抗传感应用的电极，如阻抗流细胞仪和数字间电极阵列）。

图 1显示了一个 80 μm x 80 μm Ag/AgCl 电极，其设计 AgCl 覆盖范围为 50%。，该电极按照本协议制造。通过观察，AgCl 贴片的面积约为 68 μm x 52 μm，相当于 AgCl 覆盖率的 55% 左右。这表明，该协议可以精细地控制薄膜Ag电极上的AgCl覆盖量。制造出的AgCl层也非常光滑，从相邻的AgCl粒子的聚集就可见一下。此外，AgCl 层只是单个层，没有堆叠的 AgCl 粒子和独特...

Watch this Scientific Journal Video about Fabrication of Thin Film Silver/Silver Chloride Electrodes with Finely Controlled Single Layer Silver Chloride at JoVE.com

Fabrication of Thin Film Silver/Silver Chloride Electrodes with Finely Controlled Single Layer Silver Chloride

本文旨在提出一种在薄膜银电极上具有指定覆盖的光滑、控制良好的氯化银薄膜（AgCl）的方法。

薄膜银/银氯化银电极的制造，具有精细控制的单层氯化银

This paper aims to present a protocol to form smooth and well-controlled films of silver/silver chloride (Ag/AgCl) with designated coverage on top of thin ...

该协议允许在薄膜银电极上指定覆盖的光滑单层氯化银沉积。这是首次引入一种能够精确控制电极薄膜上单层氯化银覆盖的技术。首先，使用异丙醇后用 DI 水冲洗芯片。将0.01摩尔盐酸溶液倒入丙烯酸容器中。使用实验室清洁湿巾，擦干宏银/氯化银参考电极移液器外部和电极。将芯片和微距电极连接到分析仪，使芯片上的薄膜银电极定义为工作电极，将微量银/氯化银参考电极定义为参考电极，将裸微量银/氯化银电极定义为反电极。将宏电极放入容器中。使用蓝光作为容器的盖子来锚定宏电极。将设置放入法拉第笼中。在 CHI660D 软件中，单击窗口左上角的设置选项卡。然后单击技术、安培 IT 曲线和 OK 对电极进行阴极清洁。在弹出式菜单中，修改阴极清洁参数。将初始电压设置为负 1.5，将采样间隔设置为 0.1 秒，运行时间设置为 900 秒，安静时间设置为零秒，运行期间缩放为 1。对于 80 微米由 80 微米电极，将灵敏度设置为 1 e 减 006。按"确定"。通过按菜单栏下的"开始"图标启动该过程。让实验运行并完成。打开法拉第笼，取出宏参考和反电极，然后擦干。将用过的电解质倒入废容器中，并使用 DI 水冲洗丙烯酸容器。将 0.1 摩尔氯化钾溶液倒入丙烯酸容器中。将芯片和微距电极连接到分析仪，使芯片上清洁的薄膜银电极定义为工作电极，将微量银/氯化银参考电极定义为参考电极，将裸微量银/氯化银电极定义为反电极。将宏电极放入容器中。使用蓝光作为容器的盖子来锚定宏电极。将设置放入法拉第笼中。在 CHI660D 软件中，单击窗口左上角的设置选项卡，单击技术、计时位测量和 OK 以在银电极上执行单层氯化银的电静态制造。在弹出式菜单中，修改参数。将阴极电流设置为零安培。设置诺迪克电流，使施加在薄膜电极上的电流密度为每平方厘米 0.5 毫安。保持高端低电压限制，保持默认时间。将阴极时间设置为 10 秒。相应地设置一些时间，以达到所需的氯化银覆盖程度。将初始极性设置为 anodic，数据存储间隔设置为 0.1 秒，将段数设置为 1，将当前交换优先级设置为时间。当采样间隔大于或等于 0.0005 秒时，取消选中辅助信号记录。按"确定"。通过按菜单栏下的"开始"图标启动该过程。让实验运行并完成。打开法拉第笼，取出宏参考和反电极，擦干其表面。将微量电极淹没在 3.5 摩尔氯化钾溶液中进行储存。然后将用过的电解质丢弃在废物容器中，并使用DI水冲洗丙烯酸容器。使用石蜡膜盖住丙烯酸容器的开口，直到准备好使用。此图显示一个80微米×80微米银/氯化银电极，设计为氯化银覆盖率为50%。相邻的氯化银颗粒有一个堆积，但堆积的氯化银颗粒没有观察到。可以看到一个独特的银/氯化银交叉口。此处展示了薄膜银/氯化银电极的更成功示例。80微米由80微米电极，指定氯化银覆盖率为70%和30%，160微米由160微米电极，指定氯化银覆盖率为75%和90%。此处显示的是抛光电极表面和未抛光电极表面。对于未抛光的电极，在表面上观察到手指样的结构，而抛光电极表面光滑，抛光过程造成轻微划痕。这里是一个未抛光的80微米×80微米银/氯化银电极，设计银氯化银覆盖50%，形成的氯化银似乎向内凹陷，而不是向外突出。在不同表面积的电极上形成氯化银层时，必须记住重新调整施加的电流以保持相同的电流密度。该协议使研究人员能够对分配的薄膜银/氯化银电极进行阻抗传感，因为先前的研究表明，银/氯化银电极阻抗取决于氯化银的覆盖范围。

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Profiling the Triacylglyceride Contents in Bat Integumentary Lipids by Preparative Thin Layer Chromatography and MALDI-TOF Mass Spectrometry

用制备薄层色谱和MALDI-TOF质谱分析的三酸甘油酯含量的蝙蝠外皮血脂

The mammalian integument includes sebaceous glands that secrete an oily material onto the skin surface. Sebum production is part of the innate immune ...

科研

化学

Thin-layer Chromatographic (TLC) Separations and Bioassays of Plant Extracts to Identify Antimicrobial Compounds

Thin-layer Chromatographic TLC Separations and Bioassays of Plant Extracts to Identify Antimicrobial Compounds

薄层色谱（TLC）分离和植物提取物的生物测定识别抗菌化合物

A common screen for plant antimicrobial compounds consists of separating plant extracts by paper or thin-layer chromatography (PC or TLC), exposing the ...

Dynamic Electrochemical Measurement of Chloride Ions

氯离子的动态电化学测试

This protocol describes the dynamic measurement of chloride ions using the transition time of a silver silver chloride (Ag/AgCl) electrode. Silver silver ...

Layer-by-layer Synthesis and Transfer of Freestanding Conjugated Microporous Polymer Nanomembranes

层 - 层的合成和独立式共轭微孔聚合物纳米薄膜的转移

CMP as large surface area materials have attracted growing interest recently, due to their high variability in the incorporation of functional groups in ...

Influence of Hybrid Perovskite Fabrication Methods on Film Formation, Electronic Structure, and Solar Cell Performance

上成膜钙钛矿型混合制造方法，电子结构和太阳能电池性能的影响

Hybrid organic/inorganic halide perovskites have lately been a topic of great interest in the field of solar cell applications, with the potential to ...

Fabrication and Testing of Photonic Thermometers

光子温度计的制作与测试

In recent years, a push for developing novel silicon photonic devices for telecommunications has generated a vast knowledge base that is now being ...

Chemical Synthesis of Porous Barium Titanate Thin Film and Thermal Stabilization of Ferroelectric Phase by Porosity-Induced Strain

孔隙诱导应变法合成多孔钛酸钡薄膜及铁电相热稳定性

Barium titanate (BaTiO3, hereafter BT) is an established ferroelectric material first discovered in the 1940s and still widely used because of its ...

The Effect of Ultraviolet Radiation on the Chemical Bath Deposition of Bis(thiourea) Cadmium Chloride Crystals and the Subsequent CdS Obtention

The Effect of Ultraviolet Radiation on the Chemical Bath Deposition of Bisthiourea Cadmium Chloride Crystals and the Subsequent CdS Obtention

紫外辐射对双 (硫脲) 氯化镉晶体化学镀液沉积的影响及随后的 CdS 获得

In this work, the effects on the preparation of bis(thiourea) cadmium chloride crystals when illuminated with ultraviolet (UV) light at a wavelength of ...

Solution-Processed "Silver-Bismuth-Iodine" Ternary Thin Films for Lead-Free Photovoltaic Absorbers

无铅光伏吸收剂的溶液处理 "银铋碘" 三元薄膜

Bismuth-based hybrid perovskites are regarded as promising photo-active semiconductors for environment-friendly and air-stable solar cell applications. ...

Bio-inspired Polydopamine Surface Modification of Nanodiamonds and Its Reduction of Silver Nanoparticles

纳米金刚石的生物激发多巴胺表面改性及其对银纳米粒子的还原

Surface functionalization of nanodiamonds (NDs) is still challenging due to the diversity of functional groups on the ND surfaces. Here, we demonstrate a ...