Name: electrochemical roughening of thin-film platinum macro and microelectrodes
Uploaded: 2019-06-30T12:30:00
Description: Watch this Scientific Journal Video about Electrochemical Roughening of Thin-Film Platinum Macro and Microelectrodes at JoVE.com

作者感谢劳伦斯·利弗莫尔国家实验室生物工程中心在编写本手稿期间给予的支持。Loren Frank 教授因与团队合作,使上述工作中讨论的薄膜 Pt 微阵列的制造和设计得以进行,这一合作令人欣然接受。这项工作由美国能源部主持,由劳伦斯利弗莫尔国家实验室根据DE-AC52-07NA27344合同进行,并由实验室定向研发奖16-ERD-035资助。LLNL IM 版本 LLNL-JRNL-762701。

注意:请在使用前查阅所有相关的安全数据表 (SDS)。本议定书中使用的几种化学品在高浓度下使用时具有剧毒、致癌、氧化和爆炸性。与散装材料相比,纳米材料可能具有额外的危害。执行此协议时,请使用所有适当的安全实践,包括使用工程控制(烟罩)和个人防护设备(安全眼镜、手套、实验室外套、全长裤子、闭趾鞋)。
1. 在初始表征和表面粗加工之前清洁 Pt 电极
<ol><li>用实验...

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薄膜大电极和微电极的电化学粗加工可以通过氧化还原脉冲进行。这种简单的方法确实需要几个关键元素来无损粗糙薄膜电极。与铝箔不同,如果参数没有正确选择,薄膜的粗加工可能导致样品破坏。粗加工过程的关键参数是脉冲振幅、持续时间和频率。此外,确保电极清洁度和在手术前的高氯酸纯度对于防止电极损坏至关重要。微加工过程中存在有机物或污染物,会通过腐蚀或分层造成电极的破坏。...

近五十年前,首次观测到表面增强拉曼光谱(SERS)发生在电化学粗化银1。金属箔的电化学粗加工今天仍然具有吸引力,因为它比其他粗加工方法2,3的简单性,它在许多应用中的有用性,如改进aptamer传感器4,改善神经探针5,提高金属基板6的附着力。许多散装金属的电化学粗加工方法存在1、5、7、8、9、10。然而,直到最近,还没有关于电化学粗加工应用于薄(百纳米厚)金属薄膜的报告,尽管微制薄膜金属电极在很多领域普遍存在。
建立的方法粗糙厚铂(Pt)电极5,8分层薄膜Pt电极6。通过调节粗加工过程的频率和用于粗加工的电解质,Ivanovskaya 等人演示了 Pt 薄膜粗加工,无需分层。该出版物侧重于使用这种新方法增加微制神经探头上铂记录和刺激电极的表面面积。该电极的粗加工性能提高了记录和刺激性能,提高了电化学沉积膜的附着力,提高了生物传感器的灵敏度6.但是,这种方法还可能改进微制电极阵列的表面清洁,并增强薄膜电极用于其他传感器应用(例如 aptasensor)的能力。
在以下协议中描述了粗制薄膜宏电极(1.2 mm直径)和微电极(20μm直径)的方法。这包括为粗加工而制备电极表面,以及如何描述电极的粗糙度。介绍了这些步骤,并介绍了如何针对其他电极几何形状优化粗加工过程以及确保电极无损粗加工的最重要因素。

<table border="0" cellpadding="0" cellspacing="0" style="width:648px;" width="646">
	<tbody>
		<tr height="62">
			<td height="62" style="height:62px;width:223px;">Acetone</td>
			<td style="width:131px;">Fisher Scientific, Sigma Aldrich or similar</td>
			<td style="width:123px;">n/a</td>
			<td style="width:172px;">Laboratory grade</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:223px;">EC-Lab Software</td>
			<td style="width:131px;">Bio-Logic Science Instruments</td>
			<td style="width:123px;">n/a</td>
			<td style="width:172px;">For instrument control and data analysis</td>
		</tr>
		<tr height="125">
			<td height="125" style="height:125px;width:223px;">Leakless Silver/Silver Chloride Reference</td>
			<td style="width:131px;">eDAQ Company, Australia</td>
			<td style="width:123px;">ET069-1</td>
			<td style="width:172px;">Free from chloride anion contamination 
			(or other type of chloride free electrode e.g. Mercury sulfate electrode)</td>
		</tr>
		<tr height="62">
			<td height="62" style="height:62px;width:223px;">Mercury Sulfate &#38; Acid Electrode Kit&#160;</td>
			<td style="width:131px;">Koslow, Scientific Testing Instruments</td>
			<td style="width:123px;">5100A</td>
			<td style="width:172px;">glass, 9mm version</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:223px;">Milipore DI water</td>
			<td style="width:131px;">MilliporeSigma</td>
			<td style="width:123px;">n/a</td>
			<td style="width:172px;">Certified resistivity of 18.2 M&#937;.cm (at 25&#176;C)&#160;</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:223px;">Perchloric acid, 99.9985%</td>
			<td style="width:131px;">Sigma Aldrich</td>
			<td style="width:123px;">311421</td>
			<td style="width:172px;">High Purity</td>
		</tr>
		<tr height="83">
			<td height="83" style="height:83px;width:223px;">Phosphate-buffered saline</td>
			<td style="width:131px;">Teknova</td>
			<td style="width:123px;">P4007</td>
			<td style="width:172px;">10mM PBS with 100mM NaCl, pH 7 
			or similar product from elsewhere</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:223px;">Platinum Wire Auxiliary Electrode (7.5 cm)</td>
			<td style="width:131px;">BASi</td>
			<td style="width:123px;">MW-1032</td>
			<td style="width:172px;">Counter electrode</td>
		</tr>
		<tr height="125">
			<td height="125" style="height:125px;width:223px;">Pt macroelectrodes</td>
			<td style="width:131px;">Lawrence Livermore National Laboratory</td>
			<td style="width:123px;">n/a</td>
			<td style="width:172px;">1.2 mm diameter, 250 nm thick Pt disc electrodes insulated in polyimide. More information in Reference 9.</td>
		</tr>
		<tr height="104">
			<td height="104" style="height:104px;width:223px;">Pt microelectrode arrays</td>
			<td style="width:131px;">Lawrence Livermore National Laboratory</td>
			<td style="width:123px;">n/a</td>
			<td style="width:172px;">20 &#181;m diameter 250 nM thick Pt disc electrodes insulated in polyimide. More information in Reference 9.</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:223px;">Sulfuric acid, 99.999%</td>
			<td style="width:131px;">Sigma Aldrich</td>
			<td style="width:123px;">339741</td>
			<td style="width:172px;">High Purity</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:223px;">UV &#38; Ozone Dry Stripper</td>
			<td style="width:131px;">Samco</td>
			<td style="width:123px;">UV-1</td>
			<td style="width:172px;">for cleaning electrodes</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:223px;">VersaSTAT 4 Potentiostat</td>
			<td style="width:131px;">AMETEK, Inc.</td>
			<td style="width:123px;">n/a</td>
			<td style="width:172px;">Good time resolution for pulsing tests</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:223px;">VersaStudio Software</td>
			<td style="width:131px;">AMETEK, Inc.</td>
			<td style="width:123px;">n/a</td>
			<td style="width:172px;">For instrument control</td>
		</tr>
		<tr height="104">
			<td height="104" style="height:104px;width:223px;">VMP-200 Potentiostat&#160;</td>
			<td style="width:131px;">Bio-Logic Science Instruments</td>
			<td style="width:123px;">n/a</td>
			<td style="width:172px;">Low current resolution&#160;option is preferable for measurements with microelectrodes</td>
		</tr>
	</tbody>
</table>

electrochemical roughening of thin-film platinum macro and microelectrodes

该协议演示了一种在金属晶粒边界上不优先溶解薄膜铂电极电化学粗加工的方法。该方法得到一种无裂纹的薄膜大电极表面,有源表面积增加40倍。在标准电化学表征实验室中,粗加工很容易进行,并引入电压脉冲的应用,随后在高氯酸溶液中扩展应用还原电压。该协议包括宏观尺度(1.2 mm直径)和微尺度(20微米直径)铂盘电极表面的化学和电化学制备,对电极表面进行粗加工,并描述表面粗加工对电极有源表面积。这种电化学表征包括循环伏抗和阻抗光谱,并针对宏电极和微电极进行了演示。粗加工可增加电极有源表面积,降低电极阻抗,增加相同几何形状的氮化钛电极的铂电荷注入极限,并改进基板,使其附着电化学沉积薄膜.

图2显示了对宏电极和微电极进行粗加工的电压应用的示意图。光学显微镜可用于可视化粗化宏电极(图3)或微电极(图4)外观的差异。此外,使用阻抗光谱和循环伏抗法对Pt表面的电化学表征可以很容易地显示粗化宏电极(图1)和微电极(图1)的活性表面积增加(图 5.<...

Watch this Scientific Journal Video about Electrochemical Roughening of Thin-Film Platinum Macro and Microelectrodes at JoVE.com

Electrochemical Roughening of Thin-Film Platinum Macro and Microelectrodes

该协议演示了一种在晶粒边界上不优先溶解的薄膜铂电极电化学粗加工方法。介绍了循环伏抗和阻抗光谱的电化学技术,以表征这些电极表面。

薄膜铂金宏观和微电极的电化学粗加工

This protocol demonstrates a method for electrochemical roughening of thin-film platinum electrodes without preferential dissolution at grain boundaries ...

我们的协议进一步开发了过去四十年使用的现有方法，将电化学粗加工的适用性扩展到薄膜，并开启了小型化的大门。通过增加铂电极的表面面积，无需额外的涂层，器件更坚固，可以比镀层设备更耐用，用于电刺激。我们处理过许多不同的电极几何形状，发现电极尺寸、形状和布局等参数会影响粗加工。我们鼓励研究人员改变其特定电极的脉动参数。首先，将器件的电极尖端淹没在500毫摩尔高氯酸溶液中，该溶液还含有铂线计数器电极和硫酸汞参考电极。将多电极器件的几个短电极作为工作电极连接在一起。然后，将工作电极、计数器电极和参考电极连接到电位。要通过重复电位循环以电化学的方式清洁电极表面，首先打开电位统计的 EC 实验室软件。要对电极应用循环电压图或 CV，请按加号以在实验选项卡下添加电化学技术。在弹出窗口中，将显示"插入技术"。点击电化学技术。扩展时，单击伏特测量技术。展开时，单击循环电压。在实验窗口中，填写相应的参数。在"安全高级设置"下，选择电极连接作为 CE 到接地。按"运行"按钮并选择文件名以开始实验。执行重复电位循环，直到电压图在视觉上从一个周期重叠到下一个周期，这通常发生在 50 到 200 个 CV 之后。为了执行电化学特性，将器件的电极尖端淹没在脱氧500毫摩尔高氯酸的烧杯中，该烧杯中还含有铂丝计数器电极和硫酸汞参考电极。在 EC 实验室软件中的"实验"选项卡下，按加号添加电化学技术。在弹出窗口中，将显示"插入技术"。点击电化学技术。扩展时，单击伏特测量技术。展开时，单击循环电压。在实验窗口中，填写相应的参数。在"安全高级设置"下，选择电极连接作为接地的 CE。如电极连接图所示，将工作电极、计数器电极和参考电极连接到仪器引线。按"运行"按钮并选择文件名以开始实验。执行重复的电位循环，直到电压图在视觉上显示从一个周期重叠到下一个周期。如果铂金 CV 的两个阴极峰解析不良，则从电极溶液接口的双层电容估计电极表面积。要测量开路条件下单个电极的阻抗光谱，首先将器件的电极尖端淹没在PBS中，该电极尖端还含有铂线计数器电极和硫酸汞参考电极。一次连接一个电极作为工作电极。在 EC Lab 软件中的"实验"选项卡下，按加号添加电化学技术。在弹出窗口中，将显示"插入技术"。点击电化学技术。展开时，单击阻抗光谱。扩展时，单击波滕特电化学阻抗光谱。在实验窗口中，填写相应的参数。在"高级安全设置"下，选择电极连接作为接地的 CE。如电极连接图所示，将工作电极、计数器电极和参考电极连接到仪器引线。按"运行"按钮并选择文件名以开始实验。将器件的电极尖端淹没在 500 毫摩尔高氯酸的烧杯中，该烧杯还含有铂线计数器电极和硫酸汞参考电极。然后将单个电极作为工作电极连接，并应用脉冲范式来粗加工电极。在 250 赫兹下，在负 0.15 伏特和 1.9 至 2.1 伏之间，以 1 到 1 的占空比 10 到 300 秒的负极性脉冲开始粗加工协议。打开帕尔瓦思工作室计划为 Par 电位统计。展开"实验"菜单并选择"新"。在"选择操作"弹出窗口中，选择"快速电位脉冲"，并在提示时输入所需的文件名。然后，"快速潜在脉冲线"将显示在"要执行的操作"选项卡下。在"快速电位脉冲属性"下，输入脉冲数为 2，电位 1 为负 0.59 伏，而参考为 0.002 秒，电位为 1.56 伏，参考为 0.002 秒。在"扫描属性"下，将每个点的时间输入为一秒，将周期数输入为 50，000，持续 200 秒。在"仪器属性"下，输入当前范围作为 Auto. 程序电位与长期应用恒定减小电位，通过首先按下加号按钮插入新步骤。单击计时测量。输入电位为负 0.59 伏，每点时间为一秒，持续时间为 180 秒。按"运行"按钮开始粗加工。粗加工过程完成后，程序将自动停止。粗加工完成后，确定宏选择的有效表面积的增加，如前所述。此处显示了显示用于粗加工宏选择和微电子的电压应用的示意图。光学显微镜可用于可视化粗糙的宏选择或微电子的外观差异。此外，使用阻抗光谱和循环电压法对铂表面进行电化学表征，可以清楚地显示粗糙的宏电极和微电极的活性表面积增加。此处显示了表面粗糙度与应用于微距电极的脉冲持续时间之间的关系。使用高纯度电解质进行粗加工。用去维水稀释高纯度高氯酸，只使用专用玻璃器皿。该程序将改进受益于高表面积的技术，例如增强表面吸收物种的光学光谱信号，提高电化学反应效率，以及通过传感器特性改进。这种方法将允许研究人员在不影响电极结构完整性或使用寿命的情况下，为许多不同的应用对薄膜电极表面进行粗加工。高氯酸是危险的。使用此试剂时，请使用所有适当的个人防护设备，并且仅在烟罩中操作手柄。

Research

JoVE Journal

Chemistry

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 ...

科研

化学

Electrochemical Impedance Spectroscopy as a Tool for Electrochemical Rate Constant Estimation

电化学阻抗谱作为电化学速率常数估计的一种工具

Electrochemical impedance spectroscopy (EIS) was used for advanced characterization of organic electroactive compounds along with cyclic voltammetry (CV). ...

Synthesis of Platinum-nickel Nanowires and Optimization for Oxygen Reduction Performance

铂镍纳米线的合成及减氧性能优化

Platinum-nickel (Pt-Ni) nanowires were developed as fuel cell electrocatalysts, and were optimized for the performance and durability in the oxygen ...

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 ...

Gold Nanoparticle Modified Carbon Fiber Microelectrodes for Enhanced Neurochemical Detection

用于增强神经化学检测的金纳米粒子改性碳纤维微电极

For over 30 years, carbon-fiber microelectrodes (CFMEs) have been the standard for neurotransmitter detection. Generally, carbon fibers are aspirated into ...

Asymmetric Thermoelectrochemical Cell for Harvesting Low-grade Heat under Isothermal Operation

用于在等温操作下收集低档热量的不对称热电化学电池

Low-grade heat is abundantly available in the environment as waste heat. The efficient conversion of low-grade heat into electricity is very difficult. We ...

The Effect of Anodization Parameters on the Aluminum Oxide Dielectric Layer of Thin-Film Transistors

阳极化参数对薄膜晶体管氧化铝介电层的影响

Aluminum-oxide (Al2O3) is a low cost, easily processable and high dielectric constant insulating material that is particularly appropriate for use as the ...

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

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 ...

Probing Surface Electrochemical Activity of Nanomaterials using a Hybrid Atomic Force Microscope-Scanning Electrochemical Microscope (AFM-SECM)

Probing Surface Electrochemical Activity of Nanomaterials using a Hybrid Atomic Force Microscope-Scanning Electrochemical Microscope AFM-SECM

使用混合原子力显微镜扫描电化学显微镜（AFM-SECM）探测纳米材料的表面电化学活性

Scanning electrochemical microscopy (SECM) is used to measure the local electrochemical behavior of liquid/solid, liquid/gas and liquid/liquid interfaces. ...

A Salt-Templated Synthesis Method for Porous Platinum-based Macrobeams and Macrotubes

多孔铂基微波和宏管的盐模板合成方法

The synthesis of high surface area porous noble metal nanomaterials generally relies on time consuming coalescence of pre-formed nanoparticles, followed ...