Name: localized bathless metal-composite plating via electrostamping
Uploaded: 2020-09-22T12:30:00
Description: Watch this Scientific Journal Video about Localized Bathless Metal-Composite Plating via Electrostamping at JoVE.com

这项工作得到了飞机设备可靠性和可维护性改进计划和帕图森特伙伴关系的支持。汤森得到了 ONR 学院研究金的支持。作者还感谢 SMCM 化学和生物化学系教职员工和学生的一般支持，包括 SMCM 足球队的支持。

1. 制备涂层盐
注意：镍盐和玻酸是有毒的，应使用适当的个人防护设备，包括硝酸盐手套、护目镜和实验室外套进行处理。在烟罩中应处理强酸和碱，所有废物应作为危险废物处理。
<ol><li>使用平衡，权衡以下粉末在这些比率：10.000 g 的 NiSO4+6H2O，2.120 g 的 NiCl2+6H2O，1.600 g 的 H3BO3并组合在一个小瓶中。有关浓度，请参?...

<ol>
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R., Buelens, C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+Mathematical+Model+for+the+Electrolytic+Codeposition+of+Particles+with+a+Metallic+Matrix.">A Mathematical Model for the Electrolytic Codeposition of Particles with a Metallic Matrix.</a> Journal of The Electrochemical Society. 134 (6), 1402-1408 (1987).</li><li>He, Y., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+monitoring+of+coating+health+by+in+situ+luminescent+layers.">The monitoring of coating health by in situ luminescent layers.</a> RSC Advances. 5 (53), 42965-42970 (2015).</li><li>Ganapathi, M., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrodeposition+of+luminescent+composite+metal+coatings+containing+rare-earth+phosphor+particles.">Electrodeposition of luminescent composite metal coatings containing rare-earth phosphor particles.</a> Journal of Materials Chemistry. 22 (12), 5514-5522 (2012).</li><li>Monnens, W., Deferm, C., Sniekers, J., Fransaer, J., Binnemans, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrodeposition+of+indium+from+non-aqueous+electrolytes.">Electrodeposition of indium from non-aqueous electrolytes.</a> Chemical Communications. 55 (33), 4789-4792 (2019).</li><li>Low, C. T. J., Wills, R. G. A., Walsh, F. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrodeposition+of+composite+coatings+containing+nanoparticles+in+a+metal+deposit.">Electrodeposition of composite coatings containing nanoparticles in a metal deposit.</a> Surface and Coatings Technology. 201 (1), 371-383 (2006).</li><li>Gerwitz, C. N., David, H. M., Yan, Y., Shaw, J. P., Townsend, T. K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Bathless+Inorganic+Composite+Nickel+Plating:+Dry-Cell+Stamping+of+Large+Hygroscopic+Phosphor+Crystals.">Bathless Inorganic Composite Nickel Plating: Dry-Cell Stamping of Large Hygroscopic Phosphor Crystals.</a> Advanced Materials Interfaces. 7 (4), (2020).</li><li>Bite, I., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Novel+method+of+phosphorescent+strontium+aluminate+coating+preparation+on+aluminum.">Novel method of phosphorescent strontium aluminate coating preparation on aluminum.</a> Materials and Design. 160 (15), 794-802 (2018).</li><li>Feldstein, M. D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Coatings+with+identification+and+authentication+properties.">Coatings with identification and authentication properties.</a> US Patent. , (2012).</li><li>Rose, I., Whittingham, C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Nickel Plating Handbook. , (2014).</li><li>Anderson, D. M., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Electroplating Engineering Handbook. , (1996).</li><li>Helle, K., Walsh, F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrodeposition+of+Composite+Layers+Consisting+of+Inert+Inclusions+in+a+Metal+Matrix.">Electrodeposition of Composite Layers Consisting of Inert Inclusions in a Metal Matrix.</a> Transactions of the Institute of Metal Finishing. 75 (2), 53-58 (1997).</li><li>Kerr, C., Barker, D., Walsh, F., Archer, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+Electrodeposition+of+Composite+Coatings+based+on+Metal+Matrix-Included+Particle+Deposits.">The Electrodeposition of Composite Coatings based on Metal Matrix-Included Particle Deposits.</a> Transactions of the Institute of Metal Finishing. 78 (5), 171-178 (2000).</li><li>Walsh, F. 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电击的关键步骤。 无浴电击与传统沐浴电镀共享许多相同的关键步骤。其中包括正确清洁电极，将金属离子混合到电解质中，并施用外部或化学（无电电镀）电镀，使金属在阴极上减少。此外，在酸活化后，应避免阳极和阴极的氧化，通过快速用水冲洗，并添加这些电极到设置中。
与传统的沐浴电镀相比，电镀。据报道，一些金属复合荧光金属薄膜...

传统的电镀广泛用于将各种金属、合金和金属复合材料的薄膜沉积到导电表面，以使它们的功能化，适用于预期的1、2、3、4、5、6、7、8、9、10、11、12。该方法为航空航天、汽车、军事、医疗和电子设备制造的部件添加了金属表面处理。要镀的物体阴极浸入含有金属盐前体的水浴中，通过应用化学或电位，这些前体在物体表面被减为金属。非带电复合颗粒可通过在涂层期间将其添加到浴池中，以提高涂层的薄膜性能，以提高金属氧化物和碳化物的硬度，聚合物的平滑度或液体油润滑12，13。然而，由于这些粒子对阴极缺乏内在的吸引力，在电镀13、14、15的金属中，合成的比例仍然很低。对于没有吸附到阴极足够长的时间被生长的金属薄膜嵌入的大颗粒来说，这尤其成问题。此外，吸湿颗粒在水溶液中溶解，其水化壳充当阻碍与阴极16接触的物理屏障。
一些有希望的方法已被证明，通过使用干燥的非极性溶剂完全去除水化屏障17，或通过装饰复合颗粒与带电表面活性剂分子16，扰乱水化壳，使粒子和阴极之间的接触，以减轻这种影响。但是，由于这些方法涉及有机材料，薄膜中可能发生碳污染，这些有机材料的分解可能发生在电极上。例如，使用的有机溶剂（DMSO2和乙酰胺）在惰性气氛中加热至 130°C，用于无气涂层;然而，我们发现他们在空气中的涂层是不稳定的。由于电极的电阻加热，与有机材料的氧化还原反应可能导致杂质或金属纳米粒子异构成核和生长的点。因此，需要一种无有机水电镀方法，解决粒子阴极吸附的长期挑战。到目前为止，金属复合浴涂层已被证明嵌入直径达19微米的颗粒，高达15%的负载16，17。
对此，我们描述了一种无机无浴电击方法，该方法迫使复合颗粒在高表面覆盖下嵌入薄膜，尽管其体积大，具有吸湿性20。通过去除浴池，该工艺不涉及危险涂层液体容器，且要镀膜的物体无需被淹没。因此，大型、繁琐或其他腐蚀或对水敏感的物体，可以在复合材料的特定区域进行镀压或"盖章"。此外，清除多余的水需要减少液体危险废物的清理。
在这里，我们演示了这种方法，通过共同沉积无毒和空气稳定的欧氏和掺杂的钚，氧化铝（87±30μm）与镍在高负荷（高达80%）共同沉积。，生产明亮的荧光金属薄膜。这与以前在浴缸里镀上的例子形成鲜明对比，因此仅限于小（纳米到几微米）荧光粉12。此外，以前报道的电极沉积膜只有在短波紫外光下才产生荧光，但最近的一份报告称，在具有等离子电解质氧化的氧化铝膜中，含有1~5公明氧化铝氧化晶体。荧光金属薄膜在许多行业可有影响深远的应用，包括路标照明21、飞机维修设备定位和识别20、汽车和玩具装饰、隐形信息、产品认证22、安全照明、机械应力识别10和摩擦磨损目视检查12、16。尽管这些潜在的用途发光的金属表面，此方法也可以扩大，包括额外的大和/或吸湿复合颗粒，以产生新的品种金属复合功能涂层，以前不可能通过电镀。

<table>
	<tbody>
		<tr>
			<td>37% M Hydrochloric Acid (aq)</td>
			<td>SigmaAldrich</td>
			<td>320331-500ML</td>
			<td>corrosive - handle in fume hood</td>
		</tr>
		<tr>
			<td>70% Nitric Acid (aq)</td>
			<td>SigmaAldrich</td>
			<td>438073-500ML</td>
			<td>corrosive - handle in fume hood</td>
		</tr>
		<tr>
			<td>Barium magnesium aluminate, europium doped (s)</td>
			<td>SigmaAldrich</td>
			<td>756512-25G</td>
			<td>fine powder</td>
		</tr>
		<tr>
			<td>Boric Acid (s)</td>
			<td>SigmaAldrich</td>
			<td>B6768-500G</td>
			<td>toxic</td>
		</tr>
		<tr>
			<td>Cotton Swab</td>
			<td>Q-tips</td>
			<td>Q-tips Cotton Swabs</td>
			<td></td>
		</tr>
		<tr>
			<td>ImageJ</td>
			<td>National Institutes of Health</td>
			<td>IJ 1.46r</td>
			<td>free software</td>
		</tr>
		<tr>
			<td>Nickel (II) chloride hexahydrate (s)</td>
			<td>SigmaAldrich</td>
			<td>223387-500G</td>
			<td>toxic</td>
		</tr>
		<tr>
			<td>Nickel (II) sulfate hexahydrate (s)</td>
			<td>SigmaAldrich</td>
			<td>227676-500G</td>
			<td>toxic</td>
		</tr>
		<tr>
			<td>Nickel foil (s)</td>
			<td>AliExpress</td>
			<td>Ni99.999</td>
			<td></td>
		</tr>
		<tr>
			<td>Nitrile gloves</td>
			<td>Fisher Scientific</td>
			<td>19-149-863B</td>
			<td></td>
		</tr>
		<tr>
			<td>nylon membrane (s)</td>
			<td>Tisch Scientific</td>
			<td>RS10133</td>
			<td></td>
		</tr>
		<tr>
			<td>Optical Microscope equipped with FTIC filter (470 &#177; 20 nm)</td>
			<td>Nikon</td>
			<td>Eclipse 80i</td>
			<td></td>
		</tr>
		<tr>
			<td>Plastic Wrap</td>
			<td>Fisher Scientific</td>
			<td>22-305654</td>
			<td></td>
		</tr>
		<tr>
			<td>Porcelain Mortar</td>
			<td>Fisher Scientific</td>
			<td>FB961A</td>
			<td></td>
		</tr>
		<tr>
			<td>Porcelain Pestle</td>
			<td>Fisher Scientific</td>
			<td>FB961K</td>
			<td></td>
		</tr>
		<tr>
			<td>Potassium Hydroxide (s)</td>
			<td>SigmaAldrich</td>
			<td>221473-25G</td>
			<td>corrosive</td>
		</tr>
		<tr>
			<td>Potentiostat with platinum wire</td>
			<td>Gamry Instruments</td>
			<td>1000E</td>
			<td></td>
		</tr>
		<tr>
			<td>Scoopula</td>
			<td>Fisher Scientific</td>
			<td>14-357Q</td>
			<td></td>
		</tr>
		<tr>
			<td>Spectrofluorometer</td>
			<td>Photon Technology International</td>
			<td>QM-40</td>
			<td></td>
		</tr>
		<tr>
			<td>Strontium aluminate, europium and dysprosium doped (s)</td>
			<td>GloNation</td>
			<td>756539-25G</td>
			<td>powder</td>
		</tr>
		<tr>
			<td>Variable linear DC power supply</td>
			<td>Tekpower</td>
			<td>TP3005T</td>
			<td></td>
		</tr>
		<tr>
			<td>Yttrium oxide, europium doped (s)</td>
			<td>SigmaAldrich</td>
			<td>756490-25G</td>
			<td>fine powder</td>
		</tr>
	</tbody>
</table>

localized bathless metal-composite plating via electrostamping

将嵌入金属基质中的颗粒进行复合电镀可增强金属涂层的特性，使其或多或少导电、坚硬、耐用、润滑或荧光。然而，它比金属电镀更具挑战性，因为复合颗粒要么1）没有充电，所以它们对阴极没有很强的静电吸引力，2） 是吸湿的，被水化壳阻塞，或者3） 太大，在搅拌时不能保持阴极的停滞。在这里，我们描述了无浴镀电方法的细节，该方法涉及阳极和阴极镍板夹层水浓缩电解质糊，含有大型吸湿磷银颗粒和亲水膜。施加电位后，镍金属沉积在停滞的磷颗粒周围，将它们困在薄膜中。复合涂层的特点是光学显微镜，用于薄膜粗糙度、厚度和复合表面载荷。此外，荧光光谱可用于量化这些薄膜的照明亮度，以评估各种电流密度、涂层持续时间和磷负载的影响。

遵循此协议后，金属薄涂层应镀到阴极表面，并包含添加到涂层膏中的复合颗粒。荧光或彩色颗粒的结合可以通过目视检查来观察，因为与未涂装表面相比，外观发生变化（图1A1-A3）。为了研究复合颗粒的表面覆盖率百分比，并观察涂层的表面形态，可以使用光学显微镜（图1）。样品可以自上而下观察（图1B1-B...

Watch this Scientific Journal Video about Localized Bathless Metal-Composite Plating via Electrostamping at JoVE.com

Localized Bathless Metal-Composite Plating via Electrostamping

此处介绍的是无洗澡电镀协议，其中含有复合颗粒的停滞金属盐膏在高负载下被减少为金属复合材料。此方法解决了将复合材料颗粒嵌入金属基质的其他常见电镀形式（喷射、刷子、浴）所面临的挑战。

通过电子压图进行本地化无浴金属复合电镀

Composite plating with particles embedded into the metal matrix can enhance the properties of the metal coating to make it more or less conductive, hard, ...

电冲压的工作原理是将复合颗粒困住在电解质中，迫使它们用金属进行板式。有了这项新技术，即使在对水敏感的物体上，也可能发生高复合颗粒负载。与典型的电镀不同，这种技术不需要将物体淹没在液体浴中。任何导电物体，无论其大小或形状如何。可涂覆功能性材料。荧光金属复合涂层在昏暗的光线环境中具有深远的应用，包括飞机维修设备位置、路标照明和机械机械部件中的旅行逻辑标记。开始称量硫酸镍、氯化镍六氢和玻酸，如文本手稿所述，将它们组合在一个小瓶中。将这种盐混合物彻底研磨成细粉。确保使用适当的防护设备、烟罩和危险废物处理系统。接下来，重量1.8克的欧氏磷酸氧化铝、掺杂的氧化钛或掺杂的欧氏氧化铝、镁氧化镁，使用瓷砂浆和害虫研磨成细粉约10分钟。将地面复合粉末与盐混合物混合在容器中进行储存。每平方厘米的涂层面积重0.188克这种混合物，并将其添加到一个开放的顶部容器中，将每平方厘米的涂层区域添加40微升水，搅拌溶解盐，形成厚厚的糊状物。使用剪刀，将阳极切割成与要镀的物体相匹配的大小和形状，以便从阳极箔表面去除有机物质，阴极使用 10 穆勒氢氧化钾或氢氧化钠使用棉签或布将其清洁。按照激活特定金属表面和合金的建议，用水冲洗表面以去除多余的底座，然后激活金属表面，使用棉签或布用选择性浓缩酸擦拭涂层。在烟气罩中执行此操作，以避免暴露于氯化氢蒸汽中，快速将准备好的涂层膏沉积到阴极物体上，覆盖整个区域，并确保避免间隙。使用棉签或布用浓缩酸擦拭阳极表面，从而激活阳极表面。如果需要计算电流效率，则使用分析平衡记录阳极和阴极的质量。将电源预设为所需的电流或电压模式。切割一块亲水膜（如尼龙片）并将其放在阳极涂层膏的顶部，以避免与阴极直接接触。在薄片上加入少量糊状或干盐混合物。接下来，加入两滴水，部分溶解盐。这个过程使尼龙板导电，允许离子通过电解质的大规模运输，这是平衡涂层反应中的电荷所必需的。这也可以通过将尼龙膜浸入水性镍盐混合物中来完成。将激活的阳极放在顶部，同时将负引线和正引线连接到阴极对象。用塑料盖住整个系统，以帮助保持水和施加中等压力。打开电源并继续涂装所需的持续时间。关闭电源并打开系统。断开引线，用水冲洗阴极物体，将系统的其他部件浸泡在水中，然后将这种水溶液丢弃在正确标记的危险废物容器中。去除任何未涂覆的复合颗粒，用手戴手套轻轻摩擦阴极物体。使用分析平衡记录阳极和阴极的质量，并计算与原始质量的差异。使用紫外灯观察荧光涂层，以验证金属复合材料的亮度和一致性。使用计时电流测量来监测恒定电流下的电压变化和计时波测量仪，以监测恒定电压下电流的变化。打开电位螺柱并指定持续时间和应用的电流或电压。如前所述，准备涂层。使用校准的三电极系统将电压标准化为参考标准。将铂丝作为阳极和尼龙板之间的伪参考电极放置。并覆盖它与一个单独的尼龙板，以避免接触。在阳极上沉积几滴水和少量涂层膏。最后将引线连接到电极，然后按压并开始涂装，如文本手稿中所述。监控电压或电流的变化。荧光或彩色颗粒的合并可以观察到由于外观的变化相比，未涂层的表面。光学显微镜用于研究表面覆盖和观察涂层的表面形态。从上到下观察或切割样品，以揭示横截面的复合粒子表面覆盖率百分比，作为计时测量时间函数，以及在涂层期间时位测量增加的电流密度的函数。表面覆盖也与厚度相关。在常压下，可以使用计时测量和在常电流下使用计时位测量来监测涂层参数。金属复合涂层的亮度用荧光光谱进行量化，并使用峰值区域的比率进行发光量子产量的计算。尝试此协议时，在涂装前正确清洁和激活电极非常重要。此外，彻底研磨前体电解质混合物将有助于导致光滑均匀涂层。前体复合电解质膏也可以通过喷涂涂层或粉末涂层沉积，以节省时间和材料。这样，对象可以更大规模地涂覆。这项新技术可以刺激科学探索，将以前与沐浴、喷射或刷电镀不相容的其他大型或吸湿复合颗粒纳入其中。

Research

JoVE Journal

Chemistry

Preparing Silica Aerogel Monoliths via a Rapid Supercritical Extraction Method

通过快速超临界萃取法制备二氧化硅气凝胶巨石

A procedure for the fabrication of monolithic silica aerogels in eight hours or less via a rapid supercritical extraction process is described. The ...

科研

化学

Fluorescence-based Monitoring of PAD4 Activity via a Pro-fluorescence Substrate Analog

PAD4活动通过亲荧光底物类似物基于荧光监测

Post-translational modifications may lead to altered protein functional states by increasing the covalent variations on the side chains of many protein ...

Synthesis of Protein Bioconjugates via Cysteine-maleimide Chemistry

Synthesis of Protein Bioconjugates via Cysteine-maleimide Chemistry

蛋白质生物缀合物的合成<em&gt;通过</em&gt;半胱氨酸马来酰亚胺化学

The chemical linking or bioconjugation of proteins to fluorescent dyes, drugs, polymers and other proteins has a broad range of applications, such as the ...

Epitaxial Growth of Perovskite Strontium Titanate on Germanium via Atomic Layer Deposition

锗通过原子层沉积钙钛矿型钛酸锶的外延生长

Atomic layer deposition (ALD) is a commercially utilized deposition method for electronic materials. ALD growth of thin films offers thickness control and ...

The Preparation and Properties of Thermo-reversibly Cross-linked Rubber Via Diels-Alder Chemistry

热可逆交联橡胶通过的Diels-Alder反应的化学制备与性能

A method for using Diels Alder thermo-reversible chemistry as cross-linking tool for rubber products is demonstrated. In this work, a commercial ...

Synthesizing Sodium Tungstate and Sodium Molybdate Microcapsules via Bacterial Mineral Excretion

通过细菌矿物排泄合成钨酸钠和钼酸钠微胶囊

We present a method, the bacterial mineral excretion (BME), for synthesizing two kinds of microcapsules, sodium tungstate and sodium molybdate, and the ...

Fabrication and Testing of Catalytic Aerogels Prepared Via Rapid Supercritical Extraction

快速超临界萃取制备催化气凝胶的制备与试验研究

Protocols for preparing and testing catalytic aerogels by incorporating metal species into silica and alumina aerogel platforms are presented. Three ...

Membrane Remodeling of Giant Vesicles in Response to Localized Calcium Ion Gradients

局部钙离子梯度对大泡囊膜重塑的响应

In a wide variety of fundamental cell processes, such as membrane trafficking and apoptosis, cell membrane shape transitions occur concurrently with local ...

Synthesis of Substrate-Bound Au Nanowires Via an Active Surface Growth Mechanism

通过活性表面生长机制合成基片束缚金纳米线

Advancing synthetic capabilities is important for the development of nanoscience and nanotechnology. The synthesis of nanowires has always been a ...

A Two-Step Protocol for Umpolung Functionalization of Ketones Via Enolonium Species

Enolonium 种极性转换酮功能化的两步协议

&#945;-Functionalization of ketones via umpolung of enolates by hypervalent iodine reagents is an important concept in synthetic organic chemistry. ...