Name: applying dynamic strain on thin oxide films immobilized on a pseudoelastic nickel-titanium alloy
Uploaded: 2020-07-28T14:30:00
Description: Watch this Scientific Journal Video about Applying Dynamic Strain on Thin Oxide Films Immobilized on a Pseudoelastic Nickel-Titanium Alloy at JoVE.com

这项工作由所有合著者、可持续能源联盟有限责任公司的员工、美国能源部国家可再生能源实验室的经理和运营商根据第1号合同进行。DE-AC36-08GO28308。由美国能源部、科学办公室、基础能源科学办公室、化学科学司、地球科学和生物科学、太阳能光化学项目提供的资金。

1. 制备镍钛/TiO2 电极
<ol><li>NiTi 基材的化学和机械抛光<ol>
<li>将超弹性 NiTi 箔（0.05 毫米厚度）切成 1 厘米 x 5 厘米条。</li>
		<li>使用 320、600 和 1200 砂纸进行抛光样品，然后用超纯水（18.2 MΩ）冲洗。</li>
		<li>波兰样品，带 1 μm 金刚石、0.25 μm 金刚石和 0.05 μm 氧化铝抛光。</li>
		<li>抛光后，在超纯水（18.2 MΩ）、异丙醇、乙醇、超纯水（18.2 MΩ）的连续浴中进行5分钟的声波化，然后在氮?...

<ol>
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镍醇是一种合适的弹性基板，用于在薄膜上施加机械应力。它是市售的，高导电性，可以很容易地功能化。制备红十二金TiO 2薄膜，通过热处理硝基醇，导致高n型掺杂TiO2。2必须强调，NiTi/TiO2是一个独特的系统，其中 TiO2薄膜通过 NiTi 的热处理而不是沉积方法进行准备。我们以前的出版物已经表明，适用于NiTi/TiO2的应变主要影响氧气空缺的分布、扩散和能?...

通过引入应变来改变催化材料表面反应的能力已得到广泛认可，1、2、3。1,2,3晶体材料中应变的影响可以通过调整材料结构（静态应变）或施加可变static strain外力（动态应变）来引入。在晶体材料中，静态应变可以通过掺杂4、去合金5、6、,6退火7、外延生长在不匹配的晶体晶格2或大小约束22、3中引入3。在多晶材料中，由于晶体结对8，应变可能发生在晶粒边界内。使用材料结构确定静态应变的最佳程度需要为每个离散应变级别设计一个新样本，这既耗时又昂贵。此外，引入静态应变往往引入化学或配体效应9,9，10，使得分离菌株的贡献变得困难。应用由外力精确控制的动态应变允许系统地调整材料的结构/功能关系，以便在不引入其他效果的情况下探索应变空间的动态范围。
为了研究动态应变对电催化的影响，金属或金属氧化物沉积在弹性形状或体积可调基材,上，如有机聚合物11、12、13、14、1511,12或13,14,15合金16、17。,17机械、热负荷或电气负载的应用会导致弹性基板的弯曲、压缩、伸长或膨胀，进一步导致沉积催化材料的应力应变响应。迄今为止，利用动态应变的催化剂工程对各种金属和半导体材料的电催化活性进行调调。例如：i）2上的氢演化反应 （HER）， Au， Pt， Ni， Cu， WC11，,12，,13，,14，ii） 氮气演进反应 （OER） 在 Niox16上， 镍铁合金18和 iii） 在 Pt 上减氧反应 （ORR）， Pd12，15， 19，,19,20。,在大多数这些报告中，有机聚合物，如聚甲基甲基丙烯酸酯（PMMA），被用作弹性基板。我们之前演示了弹性金属基板的应用，如不锈钢16和超弹性/形状记忆NiTi合金（Nitinol17，21）用于17,21应变研究。Nitinol还被用作用于用于 ORR19的铂薄膜沉积和电池阴极材料沉积的弹性基板，用于储能22、23,23。由于其形状记忆和伪弹性特性，NiTi合金可以通过分别应用中热19或机械应变17来变形。与有机弹性基板相比，金属基材通常不需要粘附促进剂沉积，导电性高，易于功能化。尼蒂诺被用作不锈钢 （SS） 更具弹性的替代品。虽然SS可以可可逆应变至0.2%，但硝酸盐可可可逆应变至7%。Nitinol其独特的特性归功于马腾西固态晶体的变换，它允许大弹性变形24，25。24,这两种材料都以不同的几何形状（例如，箔、电线和弹簧）在商业上提供。当形成弹性弹簧时，金属基板可用于研究动态应变对电催化的影响，而无需昂贵的仪器16;然而，与其他几何形状一样，定义应力应变响应更具挑战性。
在以往利用过渡金属催化剂进行的实验研究中，受压力催化表面活性的变化归因于d轨道的电能变化，俗称d波段理论26。相比之下，应变对金属氧化物的影响要复杂得多，因为它会影响带状gap、载体移动性、扩散和缺陷分布，甚至直接/间接过渡21、27、28、29、30、31。,27,28,29,30,31在这里，我们提供详细的协议，用于制备和表征n型掺杂TiO2薄膜，以及研究这些薄膜在可调、拉伸应变下的电催化活动的协议。等效系统可应用于研究不同材料的电催化活动，作为动态应变的函数。

<table>
	<tbody>
		<tr>
			<td>2-Propanol</td>
			<td>Sigma Aldrich</td>
			<td>109634</td>
			<td></td>
		</tr>
		<tr>
			<td>Ag/AgCl (3M NaCl) Reference Electrode</td>
			<td>BASi</td>
			<td>MF-2052</td>
			<td></td>
		</tr>
		<tr>
			<td>Alkaline Reference Electrode</td>
			<td>Basi</td>
			<td>EF-1369</td>
			<td></td>
		</tr>
		<tr>
			<td>Ethyl alcohol, Pure, 200 proof, anhydrous, =99.5%</td>
			<td>Sigma Aldrich</td>
			<td>459836</td>
			<td></td>
		</tr>
		<tr>
			<td>MT I I / F u l l am SEMTester Series</td>
			<td>MTI Instruments</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Nitinol foil, 0.05mm (0.002in) thick, superelastic, flat annealed, pickled surface</td>
			<td>Alfa Aesar</td>
			<td>45492</td>
			<td></td>
		</tr>
		<tr>
			<td>PK-4 Electrode Polishing Kit</td>
			<td>BASi</td>
			<td>MF-2060</td>
			<td></td>
		</tr>
		<tr>
			<td>Potentiostat 600D</td>
			<td>CHI instruments</td>
			<td>600D</td>
			<td></td>
		</tr>
		<tr>
			<td>Pt wire</td>
			<td>Sigma Aldrich</td>
			<td>267228-1G</td>
			<td></td>
		</tr>
		<tr>
			<td>Sodium hydroxide</td>
			<td>Sigma Aldrich</td>
			<td>221465</td>
			<td></td>
		</tr>
		<tr>
			<td>Sulfuric acid</td>
			<td>Sigma Aldrich</td>
			<td>30743</td>
			<td></td>
		</tr>
	</tbody>
</table>

applying dynamic strain on thin oxide films immobilized on a pseudoelastic nickel-titanium alloy

通过应变直接改变材料结构/功能是一个不断增长的研究领域，使材料的新特性的出现。通过控制强加于材料的外部力和诱导应力应变反应（即施加动态应变），可以调整材料 结构。电活性薄膜通常沉积在形状或体积可调弹性基材上，其中机械载荷（即压缩或张力）可以通过施加的应变影响薄膜结构和功能。在这里，我们总结了通过伪弹性镍钛合金（Nitinol）的热处理准备的n型掺杂二氧化钛（TiO2）薄膜的应变方法。所述方法的主要目的是研究应变如何影响金属氧化物的电催化活性，特别是氢演化和氧进化反应。同一系统可以适应更广泛地研究应变的影响。应变工程可用于材料功能的优化，以及外部应力控制下的可调多功能（光）电催化材料的设计。

在有氧条件下，预处理的 NiTi 箔在 500°C 下氧化（图 1）。由于钛的氧化性质，在高温下烧结会导致金石钛2的表面层。n型掺杂的层和程度受退火时间和温度的影响，这反映在从灰色（未经处理的样品）到均匀的蓝色/紫色20分钟加热后的颜色变化（图2）。更长的加热时间会导致较厚的 TiO2 薄膜（100 nm 薄膜为 60 分钟），并伴有蓝色/紫色?...

Watch this Scientific Journal Video about Applying Dynamic Strain on Thin Oxide Films Immobilized on a Pseudoelastic Nickel-Titanium Alloy at JoVE.com

Applying Dynamic Strain on Thin Oxide Films Immobilized on a Pseudoelastic Nickel-Titanium Alloy

动态拉伸应变应用于TiO2 薄膜上，研究应变对电催化的影响，特别是质子还原和水氧化。TiO2 薄膜通过伪弹性镍钛（Nitinol）的热处理来制作。

将动态应变应用于固定在伪弹性镍钛合金上的薄氧化物薄膜

Direct alteration of material structure/function through strain is a growing area of research that has allowed for novel properties of materials to ...

将可行的外部力应用于材料的能力使我们能够能够同时改变其表面特性，并找到最佳催化活性并展示新的特性。这种技术使我们能够应用菌株并研究它们对电催化活动的影响，而无需为每种隐蔽的应变程度准备多种材料。这些方法还可用于研究一系列翅片及其电化学特性，如电化学活性和腐蚀。对于镍钛基材的化学和机械抛光，首先，将一块0.05毫米厚的超弹性镍钛切成一比五厘米的条带，然后用320、600和1200砂砂纸依次抛光所得样品。每次抛光时用超纯水冲洗样品。最后一次冲洗后，用1微米金刚石、0.3微米金刚石和0.05微米氧化铝抛光剂对样品进行抛光。抛光后，在超纯水、异丙醇、乙醇和超纯水中连续洗五分钟浴，对样品进行声波处理，然后将样品在氮气下干燥。要准备50纳米厚的金光钛二氧化钛薄膜，干燥后，在有氧条件下将抛光镍钛箔放入500摄氏度的烤箱中30分钟。加热会导致表面颜色从灰色变成蓝紫色。要对加热膜样品施加拉伸应力，请轻轻将一个铝箔夹在机械测试仪中，让两端暴露一厘米的铝箔。然后，以每分钟两毫米的速度对镍钛、二氧化钛样品进行应变，使应变保持在零至3% 之间。在开始电化学测量之前，将铝箔预应变到五牛顿。要进行应用应变下的电化学实验，在镍钛、二氧化钛箔周围松散地组装一个定制的电化学电池。小心地将电池定位在中间，以确保铝箔的中心暴露在外。轻轻地将电池拧紧到样品上，以创建用于电化学测量的溶液紧固电池，并用电解质填充电池。用氮气轻轻清除溶液后，将应变从零增加至0.5%，并进行循环光度测量或线性扫描光度测量。以0.5摩尔硫酸为电解质，以银、氯化银为参考电极，以10厘米长、0.5毫米直径盘绕铂线作为反电极进行氢演化反应实验。将开路电压之间的电位扫描到 0.8 倍，而 RHE 是可逆氢电极，从最高电位值开始，扫描速率为 5 到 50 毫伏/秒。要利用一个氢氧化钠作为电解质、汞、汞氧作为参考电极，用盘绕的铂线作为计数器电极进行氧演化反应实验，请从最低电位值和5至50毫伏/秒的扫描速率开始扫描开路电压到两伏之间的电位。完成测量后，松开镍钛、二氧化钛箔周围的电化学电池，使样品能够自由移动，轻轻地将电池拧回样品上，以重新调整铝箔周围的组件。然后，重新填充和清除电解质，然后将应变从 0.5% 增加至 1%，并重复电化学实验。要确定氢演化反应活动的增加是否由于电活性表面的增加，请以不同的扫描速率运行循环光度测量，其潜在范围是法拉达电流可以忽略不计的，因此电流仅表示电双层层的电荷放电，并绘制扫描速率与电流。对于开裂薄膜的特性，在通过扫描电化学显微镜分析表面开裂之前，将五十纳米氧化钛箔的应变度保持百分之七，持续三十分钟或更长时间。然后，使用适当的样品架进行所需的测量，用于扫描电子显微镜或电化学电池，用于电化学测量，以不同增量、增加和减少应变值，使用原始且故意破裂的二氧化钛薄膜进行。对于样品的表面表征，在电化学测量后，用水清洗样品，以去除任何残留的解液，并在拉伸担架中组装冲洗过的箔。将定制样品架固定在紧绷样品周围。然后，可以通过根据标准协议扫描电子显微镜来评估样品表面。在500摄氏度下氧化镍钛箔会导致钙化和表面层二氧化金。加热30分钟后，从灰色到均匀的蓝紫色颜色变化，影响退火时间和温度的影响，该层的厚度和N型掺杂程度受到影响。加热时间较长，导致二氧化钛薄膜较厚，并伴有蓝紫色逐渐丧失。在热应力和机械应力下，镍醇的行为反映了两种不同马腾石晶体相之间的可逆固态相变，使其成为伪弹性材料，而不是弹性材料。循环光度测量和线性扫描光度测量实验对于了解电化学系统（如法拉达与非法拉达范围）非常重要。进一步的电化学特性，可以包括电化学阻抗，研究电极表面应变重新活性的变化。确定氢演化反应和氧进化反应活动的增加是否仅仅是由于电活性表面的增加。电容测量可以在不同的应变值下进行。为了进一步确定应变电活动的变化是由于施加的拉伸应力下弹性或无弹性变形引起的，可以使用原始且有目的的二氧化钛薄膜进行实验。样品必须正确安装才能获得并产生更多结果。这种模具担架可以纳入许多不同的特征和技术，包括光谱学，转吸收，共声拉曼或探针显微镜。

Research

JoVE Journal

Chemistry

Manufacturing of Three-dimensionally Microstructured Nanocomposites through Microfluidic Infiltration

通过微流体渗透制备三维微结构纳米复合材料的制造

Microstructured composite beams reinforced with complex three-dimensionally (3D) patterned nanocomposite microfilaments are fabricated via nanocomposite ...

科研

化学

Reductive Electropolymerization of a Vinyl-containing Poly-pyridyl Complex on Glassy Carbon and Fluorine-doped Tin Oxide Electrodes

在玻碳和氟掺杂的氧化锡电极的含乙烯基聚吡啶基复合还原电聚合

Controllable electrode surface modification is important in a number of fields, especially those with solar fuels applications. Electropolymerization is ...

Atomically Defined Templates for Epitaxial Growth of Complex Oxide Thin Films

原子定义模板复合氧化物薄膜的外延生长

Atomically defined substrate surfaces are prerequisite for the epitaxial growth of complex oxide thin films. In this protocol, two approaches to obtain ...

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 ...

Cooling Rate Dependent Ellipsometry Measurements to Determine the Dynamics of Thin Glassy Films

冷却率相关的椭偏仪测量确定薄膜玻膜的动力学

This report aims to fully describe the experimental technique of using ellipsometry for cooling rate dependent Tg (CR-Tg) experiments. These measurements ...

Preparation of Macroporous Epitaxial Quartz Films on Silicon by Chemical Solution Deposition

化学溶液沉积在硅外延大孔石英薄膜的制备

This work describes the detailed protocol for preparing piezoelectric macroporous epitaxial quartz films on silicon(100) substrates. This is a three-step ...

Photochemical Oxidative Growth of Iridium Oxide Nanoparticles on CdSe@CdS Nanorods

铱氧化物纳米颗粒对硒化镉硫化镉@纳米棒光化学氧化增长

We demonstrate a procedure for the photochemical oxidative growth of iridium oxide catalysts on the surface of seeded cadmium selenide-cadmium sulfide ...

Capillary Electrophoresis to Monitor Peptide Grafting onto Chitosan Films in Real Time

毛细管电泳监视肽接枝壳聚糖膜实时

Free-solution capillary electrophoresis (CE) separates analytes, generally charged compounds in solution through the application of an electric field. ...