Name: fabrication of superhydrophobic metal surfaces for anti-icing applications
Uploaded: 2018-08-15T13:30:00
Description: Watch this Scientific Journal Video about Fabrication of Superhydrophobic Metal Surfaces for Anti-Icing Applications at JoVE.com

这项研究得到了项目的支持: MAT2014-60615-R 和 MAT2017-82182-R 由国家研究局和欧洲区域发展基金 (ERDF) 资助。

注意: 该协议遵循图 2所示的方案。
1. 样品准备
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切割和清洗
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<li>使用金属剪切, 切割250毫米 x 250 毫米 x 0.5 毫米铝板成25毫米 x 45 毫米 x 0.5 毫米件。 注: 使用金属剪切时必须特别小心, 必要时需特别训练。</li>
		<li>卸下覆盖样品一侧的保护膜, 用大约50毫升的清洗液清洗这一边。用戴手套的手轻轻地冲洗样品。避免使用磨料擦洗?...

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	<li>Fang, G., Amirfazli, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Understanding+the+anti-icing+behavior+of+superhydrophobic+surfaces.">Understanding the anti-icing behavior of superhydrophobic surfaces.</a> Surface Innovations. 2 (2), 94-102 (2014).</li><li>Wang, N., 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=Robust+superhydrophobic+coating+and+the+anti-icing+properties+of+its+lubricants-infused-composite+surface+under+condensing+condition.">Robust superhydrophobic coating and the anti-icing properties of its lubricants-infused-composite surface under condensing condition.</a> New Journal of Chemistry. 41 (4), 1846-1853 (2017).</li><li>Jung, S., 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=Are+superhydrophobic+surfaces+best+for+icephobicity?.">Are superhydrophobic surfaces best for icephobicity?.</a> Langmuir. 27 (6), 3059-3066 (2011).</li><li>Milionis, A., Loth, E., Bayer, I. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Recent+advances+in+the+mechanical+durability+of+superhydrophobic+materials.">Recent advances in the mechanical durability of superhydrophobic materials.</a> Advances in Colloid and Interface Science. 229, 57-79 (2016).</li><li>Li, X. -. M., Reinhoudt, D., Crego-Calama, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=What+do+we+need+for+a+superhydrophobic+surface?+A+review+on+the+recent+progress+in+the+preparation+of+superhydrophobic+surfaces.">What do we need for a superhydrophobic surface? A review on the recent progress in the preparation of superhydrophobic surfaces.</a> Chemical Society Reviews. 36 (8), 1350-1368 (2007).</li><li>Sun, 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=Artificial+Lotus+Leaf+by+Nanocasting.">Artificial Lotus Leaf by Nanocasting.</a> Langmuir. 21 (19), 8978-8981 (2005).</li><li>Darmanin, T., Guittard, F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Superhydrophobic+and+superoleophobic+properties+in+nature.">Superhydrophobic and superoleophobic properties in nature.</a> Materials Today. 18 (5), 273-285 (2015).</li><li>Marmur, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Soft+contact:+Measurement+and+interpretation+of+contact+angles.">Soft contact: Measurement and interpretation of contact angles.</a> Soft Matter. 2 (1), 12-17 (2006).</li><li>Li, W., Amirfazli, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Hierarchical+structures+for+natural+superhydrophobic+surfaces.">Hierarchical structures for natural superhydrophobic surfaces.</a> Soft Matter. 4 (3), 462-466 (2008).</li><li>Ruiz-Cabello, F. 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在本文中, 我们展示了在铝基板上产生憎水性表面的策略。此外, 我们还展示了其润湿性、粗糙度、耐久性和抗结冰性能的表征方法。
为了准备 SH 表面, 我们使用了两种策略。第一种策略采用适当的粗糙度, 通过酸蚀来实现 SH 表面的固有层次结构。这个过程是特别关键的, 这可能需要进一步的工作, 其他金属或铝基板具有不同的组成。寻找合适的蚀刻条件可能是一个问题, 通常?...

超疏水性 (SH) 表面对水的排斥能力是传统上提出的防止结冰1、2的一种解决方案的原因。然而, 对 sh 表面的抗结冰剂的适用性有担心: 1) 生产的高成本, 2) 那 superhydrophobicity 不总导致冰-phobicity3和 3) sh 表面的值得怀疑的耐久性4.超疏水性表面具有与其地形和化学成分有关的两个性质5: 它们是粗糙的, 具有特殊的地形特征;它们的表面能量很低 (本质上是疏水性的)。
疏水性表面的粗糙度有助于降低实际固液面积与表面接触面积的比值。水没有完全接触固体由于莲花效应6,7, 当下降休息或移动到表面粗糙。在这种情况下, 固液界面行为异种地两个化学领域: 固体表面本身和被困在固体和水之间的微小气泡8。由于空气斑块光滑, 其固有接触角为 180°, 因此, 防水程度与被困空气量有关。一些研究报告将分层的表面纹理与微粗糙和纳米结构结合在一起, 作为最佳的策略, 以提供更好的防水性能 (在固体-液体界面更大的空气存在)9。对于一些金属, 一个低成本的战略, 以创造两个层次的粗糙度特征是酸性蚀刻10,11。这个程序在工业中经常使用。随着某些酸浓度和蚀刻时间的推移, 金属表面显示出适当的分层粗糙度。通常情况下, 表面粗糙是通过改变酸浓度, 蚀刻时间, 或两个12的优化。金属的表面能量很高, 因此, 制造防水金属表面需要以后 hydrophobization。
Hydrophobization 一般通过疏水性膜沉积采用不同的方法: 硅烷化10、13、浸镀14、自旋涂层15、喷涂16或等离子沉积17.硅烷化已被建议18作为提高 SH 表面耐久性的最有希望的工具之一。与其他沉积技术不同, 硅烷化过程是基于硅 OH 基团与金属衬底的表面羟基10之间的共价键键。硅烷化过程的一个缺点是, 需要以前的金属基底活化, 以创造足够的羟基, 以高度的覆盖面和均匀度。最近提出的另一项生产抗超疏水性表面的策略是使用稀土涂层19,20。氧化铈涂层有两个属性, 这是合理的使用: 它们可以是本质上疏水性21, 他们是机械和化学的健壮。特别是, 他们被选择作为保护涂层的最重要的原因之一是他们的防腐能力20。
为了生产持久的 SH 金属表面, 考虑了两个问题: 表面纹理不能损坏, 疏水性薄膜/涂层必须牢固地锚定在基体上。表面通常暴露于磨损起源于横向磨损或颗粒撞击4。如果粗糙损坏, 可以大大减少憎水性。在极端环境下, 疏水性涂层可以部分地从表面上去除, 或者通过紫外线照射、湿度或腐蚀而化学降解。耐用的 SH 表面涂层的设计是涂层和表面工程的一个重要挑战。
对于金属, 最苛刻的要求之一是, 抗结冰能力是基于三相互关联的方面22 , 如图 1所示: 过冷憎水性, 冻结延迟, 低冰粘附。室外结冰发生时, 过冷的水, 典型的降雨下降, 接触固体表面, 并迅速冻结的异质核23。形成的冰 (霜) 牢固地附有在表面。因此, 避免结冰的第一步是减少固水接触时间。如果表面超疏水性, 在结冰前可能会从表面排出雨滴。此外, 已经证明, 在潮湿的条件下, 高接触角度的表面延迟冻结比那些低接触角24。由于这两个原因, SH 表面是最合适的表面, 以减轻结冰。然而, 超疏水性表面的寿命可能是一个关键点, 因为结冰条件通常是积极的25。一些研究得出结论, SH 表面不是减少冰粘附26的最佳选择。一旦冰形成在表面上, 它保持牢固地附有由于表面粗糙。粗糙度增加了冰面接触面积, 粗糙作为联锁剂26。建议使用耐用的 SH 表面, 以避免结冰, 如果没有冰的痕迹已经存在的表面上。
在这项工作中, 我们提出了几个协议, 以生产耐用的 SH 表面的金属基板。我们使用铝 (Al) 作为基体, 因为它是广泛应用于工业, 并纳入防结冰的性质特别适用于某些应用 (滑雪胜地设施, 航空等)。我们准备了三种类型的表面: 一种表面涂有氟聚合物涂层的质感铝面, 一种带有 fluorosilane 的质感铝表面硅烷化, 以及铝基板上的氧化铈-硬脂酸双层。类似的技术17,27,28,29提供 100-300 nm 薄膜厚度, 甚至单层薄膜。对于每个表面, 我们测量了它们的润湿性和进行磨损试验。最后, 我们分析了它们的抗结冰性能, 通过使用三测试来独立探测图 1所示的三属性。
我们的协议基于图 2所示的方案。制备了 SH 铝表面后, 对其润湿性能和形貌进行了分析, 以确定其憎水性和粗糙度特征。通过弹滴实验分析了其润湿性能, 这是一种与水的拉伸粘接相结合的技术。由于对降反射的观察是必需的, 这种技术仅适用于超疏水性表面13。对于每种表面处理, 我们准备了至少四个样品进行防结冰试验, 另外四个样品进行耐久性试验。通过测量润湿性能和粗糙度特征的损失, 分析了每次耐久性试验后所造成的损伤。类似的耐久性试验的建议, 在这项工作最近用于其他金属表面27,30。
关于防结冰试验, 本研究的目的是确定所生产的 SH 铝表面的使用是否方便作为防结冰剂。因此, 我们分析了两种控制样品的性能: a) 未经处理的 Al 样品 (光滑亲水性样品) 和 b) hydrophobized, 但不具有纹理的样品 (平滑疏水性样品)。出于同样的目的, 使用有质感但不 hydrophobized 的表面可能是有兴趣的。不幸的是, 这个表面是非常润湿的, 抗结冰测试不能为他们进行。

<table>
	<tbody>
		<tr>
			<td>Hydrochloric acid, 37%</td>
			<td>SICAL, S.A.</td>
			<td>AC07411000</td>
			<td>used for acid etching</td>
		</tr>
		<tr>
			<td>1H,1H,2H,2H-Perfluorodecyltriethoxysilane, 97%</td>
			<td>Sigma-Aldrich</td>
			<td>658758</td>
			<td>used for silanization with FAS-17</td>
		</tr>
		<tr>
			<td>Dupont AF1600</td>
			<td>Dupont</td>
			<td>D10389631</td>
			<td>used for fluropolymer deposition</td>
		</tr>
		<tr>
			<td>FC-72</td>
			<td>3M, Fluorinet</td>
			<td>1100-2-93</td>
			<td>used for fluropolymer deposition (flurocarbon solvent)</td>
		</tr>
		<tr>
			<td>Cerium(III) chloride heptahydrate, 99.9%</td>
			<td>Sigma-Aldrich</td>
			<td>228931</td>
			<td>used for Ceria coating deposition</td>
		</tr>
		<tr>
			<td>Hydrogen peroxide solution, 30%</td>
			<td>Sigma-Aldrich</td>
			<td>H1009</td>
			<td>used for Ceria coating deposition</td>
		</tr>
		<tr>
			<td>Stearic acid, &#8805;98.5%</td>
			<td>Sigma-Aldrich</td>
			<td>S4751</td>
			<td>used for Ceria coating deposition</td>
		</tr>
		<tr>
			<td>Ethanol</td>
			<td>SICAL, S.A.</td>
			<td>16271</td>
			<td>used throughout</td>
		</tr>
		<tr>
			<td>Acetone</td>
			<td>SICAL, S.A.</td>
			<td>1090</td>
			<td>used throughout</td>
		</tr>
		<tr>
			<td>Aluminum sheets 0.5mm</td>
			<td>MODULOR (Germany)</td>
			<td>125993</td>
			<td>substrates used throught</td>
		</tr>
		<tr>
			<td>Micro-90 concentrated cleaning solution</td>
			<td>Sigma-Aldrich</td>
			<td>Z281506</td>
			<td></td>
		</tr>
		<tr>
			<td>Ultra pure Milli-Q water</td>
			<td>Millipore</td>
			<td>discontinued</td>
			<td>used throughout</td>
		</tr>
		<tr>
			<td>Plasma Etcher/Asher/Cleaner EMITECH K1050X</td>
			<td>Aname</td>
			<td>K1500XDEV-001</td>
			<td>used throughout</td>
		</tr>
		<tr>
			<td>PCC software</td>
			<td>AMETEK</td>
			<td>discontinued</td>
			<td>sofware controlling the high speed camera Phantom MIRO 4</td>
		</tr>
		<tr>
			<td>High Speed Camera Phantom Miro 4</td>
			<td>AMETEK</td>
			<td>discontinued</td>
			<td>used for bouncing drop experiments</td>
		</tr>
		<tr>
			<td>Open Loop PL&#181; 2.32</td>
			<td>UPC-CD6 &#38; Sensofar Tech S.L.</td>
			<td>version 2.32</td>
			<td>Sofware controlling PL&#181; Confocal Imaging Profiler</td>
		</tr>
		<tr>
			<td>Pl&#181;-Confocal Imaging Profiler 2300</td>
			<td>Sensofar Tech S.L.</td>
			<td>discontinued</td>
			<td>used for roughness measurements</td>
		</tr>
		<tr>
			<td>TABER 5750 LINEAL ABRASER</td>
			<td>TABER</td>
			<td>5750</td>
			<td>used for lateral abrasion tests</td>
		</tr>
		<tr>
			<td>Abbrasive sand: ASTM 20-30 SAND C778</td>
			<td>U.S. SILICA COMPANY (USA)</td>
			<td>1-800-635-7263</td>
			<td>used for abrasive partcile impact tests</td>
		</tr>
		<tr>
			<td>Ozone cleaner: PSDP-UV4T, Digital UV Ozone System</td>
			<td>Novascam</td>
			<td>discontinued</td>
			<td>UV-ozone degradation test</td>
		</tr>
		<tr>
			<td>Peristalitic Pump GILSON 312, France</td>
			<td>GILSON (France)</td>
			<td>discontinued</td>
			<td>used for water dripping test</td>
		</tr>
		<tr>
			<td>Nylon thread</td>
			<td>Dracon fishing line, Izorline internacional, inc. (USA)</td>
			<td>discontinued</td>
			<td>used for ice adhesion tests</td>
		</tr>
		<tr>
			<td>Digital force gauge (ZTA-200N, ZTA Series</td>
			<td>IMADA (USA)</td>
			<td>370199</td>
			<td>used for ice adhesion tests</td>
		</tr>
		<tr>
			<td>Motorized test stand I, MH2-500N-FA</td>
			<td>IMADA (USA)</td>
			<td>366942</td>
			<td>used for ice adhesion tests</td>
		</tr>
		<tr>
			<td>Force Recorder Professional</td>
			<td>IMADA (USA)</td>
			<td>version 1.0.2</td>
			<td>software provided by IMADA to register the force</td>
		</tr>
		<tr>
			<td>HYGROCLIP XD - STANDARD PROBE</td>
			<td>Rotronic</td>
			<td>discontinued</td>
			<td>Temperature and humidity probe</td>
		</tr>
		<tr>
			<td>HW3 Lite software</td>
			<td>Rotronic</td>
			<td>version 2.1.2</td>
			<td>Sofware controlling the HYGROCLIP Probe</td>
		</tr>
	</tbody>
</table>

fabrication of superhydrophobic metal surfaces for anti-icing applications

本文介绍了几种生产超疏水性金属表面的方法。铝因其在工业中的广泛应用而被选为金属基体。通过弹滴实验分析了产生表面的润湿性, 并用共焦显微技术对其形貌进行了分析。此外, 我们还展示了测量其耐久性和抗结冰性能的各种方法。超疏水性表面保持一种特殊的质地, 必须保存, 以保持其防水。为了制造耐用的表面, 我们遵循了两种策略来整合一种耐药性的纹理。第一种策略是通过酸性蚀刻直接将粗糙度与金属基体结合在一起。表面挤压后, 硅烷化或含氟聚合物沉积物降低了表面能量。第二种策略是氧化铈层 (表面挤压后) 的生长, 以提高表面硬度和耐腐蚀性。用硬脂酸膜降低了表面能量。
超疏水性表面的耐久性通过粒子撞击试验、横向磨损的机械磨损和紫外线-臭氧电阻来检验。通过研究消除过冷水、冻结延迟和冰粘附能力, 探讨了抗结冰性能。

本文研究的 SH 表面的润湿性和粗糙度特性如图 5所示。每个样本的平均反弹次数显示在图 5a中, 平均粗糙度如图 5b所示。粗糙度和润湿性之间没有相关性。聚四氟乙烯涂层试样的反弹次数与 Ce 样品一致。然而, Ce SA 的样本显然是粗糙的 (~ 40% 更大的 Ra 值)。相比之下, FAS-17 样品的 Ra 值与聚四氟乙烯非常相似...

Watch this Scientific Journal Video about Fabrication of Superhydrophobic Metal Surfaces for Anti-Icing Applications at JoVE.com

Fabrication of Superhydrophobic Metal Surfaces for Anti-Icing Applications

我们阐述了几种生产超疏水性金属表面的方法, 并探讨了它们的耐久性和抗结冰性能。

防结冰用超疏水性金属表面的制备

Several ways to produce superhydrophobic metal surfaces are presented in this work. Aluminum was chosen as the metal substrate due to its wide use in ...

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