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
<ol><li>
切割和清洗
	<ol>
<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。避免使用磨料擦洗器。</li>
		<li>在蒸馏水的流动中大量冲洗样品。随后, 将每个样品浸泡在30毫升的96% 乙醇中, 将其油脂实验为 300s, 并在30毫升的超纯水中重复300s。</li>
		<li>将样品从水中取出, 在室温下晾干1小时。</li>
	</ol>
</li>
	<li>
酸性蚀刻
	<ol>
<li>对于蚀刻反应, 在超纯水中制备 4 M 溶液 HCl13。将每个样品浸入这个溶液中的80毫升480s。当本机氧化物表面层被去除, 反应在大约360s 以后变得更加剧烈。 注意: 为了安全起见, 在遮光罩中进行这种反应。戴手套、实验室大衣和防护眼镜。</li>
		<li>在装有酸溶液的烧杯旁边, 用超纯水准备另一个烧杯, 突然停止反应。使用聚四氟乙烯镊子, 从酸溶液中取出样品并浸入水中。在丰富的超纯水中冲洗样品。</li>
		<li>通过过滤和压缩空气吹干样品。请注意, 蚀刻反应后的样品干火干燥可能是一项艰巨的任务。在水的宏观去除以后吹, 去除水的踪影在烤箱在120°c 为600s。 注意: 这个干燥过程中必不可少的, 特别是对样品以后硅烷化。</li>
	</ol>
</li>
	<li>
Hydrophobization
	<ol>
<li>
Hydrophobization FAS-17 硅烷化
		<ol>
<li>在蒸气相硅烷化之前, 用空气等离子体对样品进行 600s, 用 100 W 的等离子清洗剂处理。这个过程激活的表面功能组 (-OH 组) 作为链接器的硅烷分子。</li>
			<li>随后, 在玻璃培养皿中引入一些样品, 在吸管尖端的帮助下略微倾斜表面。在样品2旁边的培养皿上, 将两50µL 滴 1 h、1 h、2 h、13 h-癸-triethoxysilane (FAS-17) 存入。</li>
			<li>部分覆盖培养皿, 并将其放置在空气疏散干燥过夜。最后, 通风干燥。删除准备使用的示例。</li>
		</ol>
</li>
		<li>
Hydrophobization 氟聚合物(聚四氟乙烯) 沉积物
		<ol>
<li>用氟碳溶剂中的非晶态氟聚合物溶液, 在 1/20 (v/v)16的比例下, 将蚀刻样品16从约10厘米喷出。一个充满了溶液的香水扩散器可以用于这个目的。600s 在室温下晾干. 在清洁的无蚀刻表面上重复相同的过程, 使光滑的疏水性铝表面 (Ra = 0.25±0.03 µm)。</li>
			<li>应用第二层涂层, 并在110摄氏度烤箱中引入样品, 以确保600s 的溶剂完全去除, 并对含氟聚合物涂层进行交联。这一过程增加了耐久性, 正如制造商所指出的。</li>
		</ol>
</li>
		<li>
氧化铈-硬脂酸沉积 Hydrophobization
		<ol>
<li>清洁丙酮/乙醇/水中的蚀刻样品, 油脂实验它们在水中 300s, 并在压缩空气的流动中晾干。</li>
			<li>浸泡在50毫升的水溶液中含有2克三氯化铈水合物 (CeCl3· 7H2o) 的样品31 , 和3毫升的30% 过氧化氢 (H2O2)。在40摄氏度烤箱中浸泡在溶液中的样品1小时。</li>
			<li>把它从溶液中取出, 在蒸馏水中冲洗, 在100摄氏度的烤箱中600s。</li>
			<li>将样品浸入硬脂酸的30毫米乙醇溶液中 900s, 将其漂洗在乙醇中, 并在100摄氏度烤箱中将其烘干600s。 注: 一旦干燥冷却到室温, 样品就可以使用了。用氧化铈-硬脂酸涂层酸生产的 SH 表面以下简称铈-SA 涂层表面。</li>
		</ol>
</li>
	</ol>
</li>
</ol>2. 样品表征
<ol><li>
润湿分析
	<ol>
<li>
弹跳滴实验
		<ol>
<li>用弹跳滴实验法评价生产样品的憎水性程度13。通过从固定注射器中释放的针头, 其针位于表面上方 (10.1 厘米 0.2) 的位置, 量化所给出的反弹次数。下拉卷通常为4µL。</li>
			<li>用高速相机捕获序列。在高速视频采集软件中, 将采集速率固定在每秒4200张图像上, 曝光时间为235µs。</li>
			<li>录制完视频后, 从放置释放的那一刻起, 选择序列, 直到水滴已经与样品完全接触 (没有观察到更多的反弹)。保存视频文件。</li>
			<li>对于每个图像, 使用软件32检测放置配置文件。随后, 在播放视频序列时, 用肉眼来量化反弹的次数。在不容易识别的情况下, 计算静态降的质心位置的极大值 (大于 15-20%)。</li>
		</ol>
</li>
		<li>
倾斜板试验
		<ol>
<li>使用此测试仅对每个特定磨损测试所造成的损坏进行量化。采用实验室设计的摆式装置34, 分析了倾斜板试验 (TPE)33的水滴的剪切粘附性。</li>
			<li>使用侧面查看图像获取一个无柄下落放置在样本固定到一个倾平台。在图像采集过程中 (在 16 fps 的恒定捕获率) 下, 倾斜具有恒定角速度的平台 (5°)。因此, 每0.31°捕获一个 drop 图像。 注: 在特定倾角的上方, 在表面上的滴动 (滑动/滚出) 和这个状态可以用来同时确定前进和后退的接触角 (ACA 和 RCA)。产生接触线全局位移的最小倾角 (上坡和下坡接触线点同时移动) 称为滑动角 (SA)。SA 是从 TPE 这里报告的值。</li>
		</ol>
</li>
	</ol>
</li>
	<li>
粗糙度测量
	<ol>
<li>用白光共焦显微镜分析样品的显微粗糙度。设置扫描面积为 0.252 x 0.187 毫米每单一地形。</li>
		<li>每个样品至少取4个地形。使用放大50X 的目标, 以0.2 µm 的垂直步骤捕获200垂直平面. 确定 Ra 因子 (算术粗糙度振幅)。</li>
	</ol>
</li>
</ol>3. 耐久性试验
注: 分别评估每种磨损剂所引起的损伤。不要对每个样品进行多项磨损测试。
<ol><li>
横向磨损试验 注: 横向磨损试验 (见图 3a) 是通过商业线性磨料进行的。本试验旨在评估标准磨料尖端对表面的切向位移引起的磨损。该装置允许使用各种磨料, 设置广泛的应用压力, 横向速度和总数量的磨料循环35。<ol>
<li>使用制造商提供的标准橡胶磨料 CS-10。将速度固定在20周/分钟左右. 使用权重控制施加的压力。设置仪器所允许的最小压力, 对应于总重量为350克。 注: 考虑尖端宽度 (6.70±0.05 mm) 和使用的重量, 这些设置的相应的应用压力是97.3±1.4 帕。总磨损面积受尖端宽度和每个磨损周期总长度的限制。设置为38.1 毫米。</li>
		<li>对于每个样品, 评估1、2、3和5周期后的磨损。<ol>
<li>每次磨损处理后, 轻轻地刷表面 (使用制造商提供的刷子), 在水中冲洗, 并使用压缩空气吹。如2.1.2 节所述, 使用 TPE 评估润湿性能。</li>
		</ol>
</li>
	</ol>
</li>
	<li>
磨料颗粒冲击试验
	<ol>
<li>使用图 3b所示的设置进行粒子撞击测试, 这是由标准磨损测试 D968 的启发。从玻璃漏斗上释放30毫升 (约55克) 的磨料砂。在 (25±1) 厘米的表面定位其极端底部。</li>
		<li>使用漏斗丝锥直径 (12±1) 毫米和长度 (97±1) 毫米. 将漏斗垂直放置, 同时倾斜样品45°。撞击样品后, 将沙子收集在下面放置的容器中。</li>
		<li>一旦磨损循环, 用蒸馏水冲洗表面, 在压缩空气的流动中干燥, 并通过 TPE (2.1.2) 评估润湿性能。对每个示例重复此整个过程多达3次。</li>
	</ol>
</li>
	<li>
紫外线-臭氧表面降解试验
	<ol>
<li>使用臭氧清洗剂进行紫外线臭氧降解试验。在室温下对每个样品进行 600s, 重复一次循环。</li>
		<li>随后, 冲洗水中的表面, 用压缩空气晾干。</li>
		<li>评估2.1.2 节中描述的 TPE 的润湿性能, 以确定在紫外线照射后超疏水性的性能是否仍然存在。</li>
	</ol>
</li>
	<li>
水浸试验
	<ol>
<li>通过长时间浸泡在水中, 评估水接触引起的磨损。在100毫升的超纯水烧杯中介绍样品24小时。</li>
		<li>从水中取出样品, 用压缩空气干燥, 然后将它们放在一个120摄氏度的烤箱中 600s, 以确保从表面完全去除水。当表面完全干燥时, 使用2.1.2 节中描述的协议评估水暴露后的润湿性能。</li>
	</ol>
</li>
</ol>4. 防结冰效率评估
注: 防结冰效率评估是基于图 1所示的三方面。
<ol><li>
过冷水滴试验 注: 样品的过冷憎水性通过图 4a所示的设置进行测试。样品介绍在–20°c 的冷冻室内, 固定在倾斜 (30°) 平台的顶部。冰和蒸馏水的混合物在平衡 (在稳定的温度0°c) 被放置在结冰的房间外面。<ol>
<li>用蠕动泵将冷水泵入室内, 并在冰箱内循环, 然后每3秒降低1滴。单滴有大约50µL 的体积。</li>
		<li>一旦滴水过程开始, 每十年代捕获样本的横向图像, 以确定是否发生冰积。</li>
	</ol>
</li>
	<li>
冻结延时试验
	<ol>
<li>在前一节提到的同一冻结室内进行冻结延迟试验。</li>
		<li>确定在冷却过程中, 从室温降到大约-25 摄氏度的情况下, 在样品上沉积的无柄水滴的百分比。此测试的设置如图 4b所示。</li>
		<li>水平的样品 (零倾斜) 和存款无梗滴小心, 以避免翻滚。由于水滴在憎水性表面上的流动性很高, 所以在 SH 样品上放置了较低的数量。多次对 SH 表面重复实验。</li>
		<li>使用热探针监测温度和相对湿度。使用商用加湿器控制相对湿度 (RH)。当加湿器打开时, RH 大约是 95%, 当加湿器关闭时, 相对湿度会降低到大约40%。</li>
		<li>每个样品使用大约200滴30µL (下落结冰是一个随机现象, 并且分析要求使用大量滴)。 注: 因此, 这个测试使用较大的样本比那些用于其余的研究。在这种情况下, 大小是125毫米 x 62.5 毫米, 并调整协议, 以蚀刻样品或 hydrophobize 其表面到新的样本尺寸。</li>
		<li>把样品放在冰箱底部的一个隔离平台的顶部。轻轻地存入70滴每样的数组 (25 的超疏水性样品)。关闭冰箱并打开它。 注: 温度从室温降至约-25 摄氏度时线性下降。冷却速度取决于相对湿度。在低相对湿度 (未拔出加湿器), 整个过程大约需要2小时, 而它需要更少的时间 (约1小时), 如果加湿器连接。一旦温度低于0摄氏度, 水滴开始核核。</li>
		<li>计算每种温度下冻结的水滴数 (间隔为0.5 摄氏度), 直到所有水滴全部冻结为止。</li>
	</ol>
</li>
	<li>
冰粘附试验
	<ol>
<li>将必须应用的力量化为分离 (拉断) 一块冰, 并在每个样品上形成可控的接触区。使用图 4c所示的设置来执行这些测试。</li>
		<li>用剪刀把直径为10毫米的聚四氟乙烯管子切成28毫米高的圆筒。按下气缸对样品。用1.2 毫升蒸馏水填满它。在冷冻室中引入填充气缸, 等待1小时。 注: 一旦水完全冻结, 与气缸的样品是牢固固定在一个平台使用前锋板。</li>
		<li>用尼龙线将气缸与数字力计系在一起。这个气缸与螺纹连接的方式和圆柱体相对于螺纹的方向取决于所评估的类型 (剪切或拉伸) 附着力。把这个量规固定在一个机动的测试台上。关闭冷冻室, 等待600s。</li>
		<li>以恒定速度 (10 @ 0.5) 毫米/分钟取代试样。<ol>
<li>在机动测试台的控制面板中手动调整此速度。单击控制测功机读数的程序图标。按开始记录力。</li>
			<li>紧接着, 将测功机向上移动, 保持在电动支架控制面板内按下垂直位移底部。</li>
		</ol>
</li>
		<li>当测功机相对于试样的位移产生一个线的延伸和从样品中分离冰时, 单击停止并保存生成的数据文件。 注: 测量仪按时间对力进行监测。了解测功机偏移的速度 (10 毫米/分钟), 确定位移的力。这有助于确定断裂力 (最大挡力) 和每单位面积的附着力强度。</li>
		<li>在横向进行拉拔时, 对剪切附着力进行评价。这种情况下的力是平行应用于接触区 (见图 4b)。为此, 请垂直固定样品, 并使用金属环将气缸底座与螺纹连接。将这个环拉到测量器上, 直到试样从表面通过剪切位移分离出来。 注: 拉伸粘附试验评估峰值力和工作需要从表面分离一块冰时, 它是垂直拉。</li>
		<li>在这种情况下, 在气缸壁上钻两个小孔, 用来连接气缸和量规。然后, 垂直拉, 直到冰最终从表面分离出来。</li>
	</ol>
</li>
</ol>

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我们没有什么可透露的。

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 ...

fabrication-superhydrophobic-metal-surfaces-for-anti-icing

Research

JoVE Journal

Engineering

8.4K 次观看.  University of Granada. 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。

视频: Fabrication of Superhydrophobic Metal Surfaces for Anti-Icing Applications

Hyperpolarized Xenon for NMR and MRI Applications

Nuclear magnetic resonance (NMR) spectroscopy and imaging (MRI) suffer from intrinsic low sensitivity because even strong external magnetic fields of ~10 T generate only a small detectable net-magnetization of the sample at room temperature 1. Hence, most NMR and MRI applications rely on the detection of molecules at relative high concentration (e.g., water for imaging of biological tissue) or require excessive acquisition times. This limits our ability to exploit the very useful molecular specificity of NMR signals for many biochemical and medical applications. However, novel approaches have emerged in the past few years: Manipulation of the detected spin species prior to detection inside the NMR/MRI magnet can dramatically increase the magnetization and therefore allows detection of molecules at much lower concentration 2.
Here, we present a method for polarization of a xenon gas mixture (2-5% Xe, 10% N2, He balance) in a compact setup with a ca. 16000-fold signal enhancement. Modern line-narrowed diode lasers allow efficient polarization 7 and immediate use of gas mixture even if the noble gas is not separated from the other components. The SEOP apparatus is explained and determination of the achieved spin polarization is demonstrated for performance control of the method.
The hyperpolarized gas can be used for void space imaging, including gas flow imaging or diffusion studies at the interfaces with other materials 8,9. Moreover, the Xe NMR signal is extremely sensitive to its molecular environment 6. This enables the option to use it as an NMR/MRI contrast agent when dissolved in aqueous solution with functionalized molecular hosts that temporarily trap the gas 10,11. Direct detection and high-sensitivity indirect detection of such constructs is demonstrated in both spectroscopic and imaging mode.

The production of hyperpolarized xenon by means of spin exchange optical pumping (SEOP) is described. This method yields a ~10000-fold enhancement of the nuclear spin polarization of Xe-129 and has applications in nuclear magnetic resonance spectroscopy and imaging. Examples of gas phase and solution state experiments are given.

超极化氙NMR和MRI的应用

Nuclear magnetic resonance (NMR) spectroscopy and imaging (MRI) suffer from intrinsic low sensitivity because even strong external magnetic fields of ~10 ...

科研

工程学

Probing and Mapping Electrode Surfaces in Solid Oxide Fuel Cells

Solid oxide fuel cells (SOFCs) are potentially the most efficient and cost-effective solution to utilization of a wide variety of fuels beyond hydrogen 1-7. The performance of SOFCs and the rates of many chemical and energy transformation processes in energy storage and conversion devices in general are limited primarily by charge and mass transfer along electrode surfaces and across interfaces. Unfortunately, the mechanistic understanding of these processes is still lacking, due largely to the difficulty of characterizing these processes under in situ conditions. This knowledge gap is a chief obstacle to SOFC commercialization. The development of tools for probing and mapping surface chemistries relevant to electrode reactions is vital to unraveling the mechanisms of surface processes and to achieving rational design of new electrode materials for more efficient energy storage and conversion2. Among the relatively few in situ surface analysis methods, Raman spectroscopy can be performed even with high temperatures and harsh atmospheres, making it ideal for characterizing chemical processes relevant to SOFC anode performance and degradation8-12. It can also be used alongside electrochemical measurements, potentially allowing direct correlation of electrochemistry to surface chemistry in an operating cell. Proper in situ Raman mapping measurements would be useful for pin-pointing important anode reaction mechanisms because of its sensitivity to the relevant species, including anode performance degradation through carbon deposition8, 10, 13, 14 ("coking") and sulfur poisoning11, 15 and the manner in which surface modifications stave off this degradation16. The current work demonstrates significant progress towards this capability. In addition, the family of scanning probe microscopy (SPM) techniques provides a special approach to interrogate the electrode surface with nanoscale resolution. Besides the surface topography that is routinely collected by AFM and STM, other properties such as local electronic states, ion diffusion coefficient and surface potential can also be investigated17-22. In this work, electrochemical measurements, Raman spectroscopy, and SPM were used in conjunction with a novel test electrode platform that consists of a Ni mesh electrode embedded in an yttria-stabilized zirconia (YSZ) electrolyte. Cell performance testing and impedance spectroscopy under fuel containing H2S was characterized, and Raman mapping was used to further elucidate the nature of sulfur poisoning. In situ Raman monitoring was used to investigate coking behavior. Finally, atomic force microscopy (AFM) and electrostatic force microscopy (EFM) were used to further visualize carbon deposition on the nanoscale. From this research, we desire to produce a more complete picture of the SOFC anode.

We present a unique platform for characterizing electrode surfaces in solid oxide fuel cells (SOFCs) that allows simultaneous performance of multiple characterization techniques (e.g. in situ Raman spectroscopy and scanning probe microscopy alongside electrochemical measurements). Complementary information from these analyses may help to advance toward a more profound understanding of electrode reaction and degradation mechanisms, providing insights into rational design of better materials for SOFCs.

在固体氧化物燃料电池电极表面的探测和测绘

Solid oxide fuel cells (SOFCs) are potentially the most efficient and cost-effective solution to utilization of a wide variety of fuels beyond hydrogen ...

Fabrication of Nano-engineered Transparent Conducting Oxides by Pulsed Laser Deposition

Nanosecond Pulsed Laser Deposition (PLD) in the presence of a background gas allows the deposition of metal oxides with tunable morphology, structure, density and stoichiometry by a proper control of the plasma plume expansion dynamics. Such versatility can be exploited to produce nanostructured films from compact and dense to nanoporous characterized by a hierarchical assembly of nano-sized clusters. In particular we describe the detailed methodology to fabricate two types of Al-doped ZnO (AZO) films as transparent electrodes in photovoltaic devices: 1) at low O2 pressure, compact films with electrical conductivity and optical transparency close to the state of the art transparent conducting oxides (TCO) can be deposited at room temperature, to be compatible with thermally sensitive materials such as polymers used in organic photovoltaics (OPVs); 2) highly light scattering hierarchical structures resembling a forest of nano-trees are produced at higher pressures. Such structures show high Haze factor (&gt;80%) and may be exploited to enhance the light trapping capability. The method here described for AZO films can be applied to other metal oxides relevant for technological applications such as TiO2, Al2O3, WO3 and Ag4O4.

We describe the experimental method to deposit nanostructured oxide thin films by nanosecond Pulsed Laser Deposition (PLD) in the presence of a background gas. By using this method Al-doped ZnO (AZO) films, from compact to hierarchically structured as nano-tree forests, can be deposited.

制备纳米设计的脉冲激光沉积透明导电氧化物

Nanosecond Pulsed  Laser Deposition (PLD) in the presence of a background gas allows the deposition  of metal oxides with tunable morphology, structure, ...

Fabrication of VB2/Air Cells for Electrochemical Testing

A technique to investigate the properties and performance of new multi-electron metal/air battery systems is proposed and presented. A method for synthesizing nanoscopic VB2 is presented as well as step-by-step procedure for applying a zirconium oxide coating to the VB2 particles for stabilization upon discharge. The process for disassembling existing zinc/air cells is shown, in addition construction of the new working electrode to replace the conventional zinc/air cell anode with a the nanoscopic VB2 anode. Finally, discharge of the completed VB2/air battery is reported. We show that using the zinc/air cell as a test bed is useful to provide a consistent configuration to study the performance of the high-energy high capacity nanoscopic VB2 anode.

Fabrication of VB2/Air Cells for Electrochemical Testing

A protocol is presented to study multi-electron metal/air battery systems by using previous technology developed for the zinc/air cell. Electrochemical testing is then performed on fabricated batteries to evaluate performance.

VB制作<sub&gt; 2</sub&gt; /空气电池电化学测试

A technique to investigate the properties and performance of new multi-electron metal/air battery systems is proposed and presented. A method for ...

Monolayer Contact Doping of Silicon Surfaces and Nanowires Using Organophosphorus Compounds

Monolayer Contact Doping (MLCD) is a simple method for doping of surfaces and nanostructures1. MLCD results in the formation of highly controlled, ultra shallow and sharp doping profiles at the nanometer scale. In MLCD process the dopant source is a monolayer containing dopant atoms.
In this article a detailed procedure for surface doping of silicon substrate as well as silicon nanowires is demonstrated. Phosphorus dopant source was formed using tetraethyl methylenediphosphonate monolayer on a silicon substrate. This monolayer containing substrate was brought to contact with a pristine intrinsic silicon target substrate and annealed while in contact. Sheet resistance of the target substrate was measured using 4 point probe. Intrinsic silicon nanowires were synthesized by chemical vapor deposition (CVD) process using a vapor-liquid-solid (VLS) mechanism; gold nanoparticles were used as catalyst for nanowire growth. The nanowires were suspended in ethanol by mild sonication. This suspension was used to dropcast the nanowires on silicon substrate with a silicon nitride dielectric top layer. These nanowires were doped with phosphorus in similar manner as used for the intrinsic silicon wafer. Standard photolithography process was used to fabricate metal electrodes for the formation of nanowire based field effect transistor (NW-FET). The electrical properties of a representative nanowire device were measured by a semiconductor device analyzer and a probe station.

A detailed procedure for surface doping of Silicon interfaces is provided. The ultra-shallow surface doping is demonstrated by using phosphorus containing monolayers and rapid annealing process. The method can be used for doping of macroscopic area surfaces as well as nanostructures.

Monolayer Contact Doping (MLCD) is a simple method for doping of surfaces and nanostructures1. MLCD results in the formation of highly controlled, ultra ...

Fabrication Process of Silicone-based Dielectric Elastomer Actuators

This contribution demonstrates the fabrication process of dielectric elastomer transducers (DETs). DETs are stretchable capacitors consisting of an elastomeric dielectric membrane sandwiched between two compliant electrodes. The large actuation strains of these transducers when used as actuators (over 300% area strain) and their soft and compliant nature has been exploited for a wide range of applications, including electrically tunable optics, haptic feedback devices, wave-energy harvesting, deformable cell-culture devices, compliant grippers, and propulsion of a bio-inspired fish-like airship. In most cases, DETs are made with a commercial proprietary acrylic elastomer and with hand-applied electrodes of carbon powder or carbon grease. This combination leads to non-reproducible and slow actuators exhibiting viscoelastic creep and a short lifetime. We present here a complete process flow for the reproducible fabrication of DETs based on thin elastomeric silicone films, including casting of thin silicone membranes, membrane release and prestretching, patterning of robust compliant electrodes, assembly and testing. The membranes are cast on flexible polyethylene terephthalate (PET) substrates coated with a water-soluble sacrificial layer for ease of release. The electrodes consist of carbon black particles dispersed into a silicone matrix and patterned using a stamping technique, which leads to precisely-defined compliant electrodes that present a high adhesion to the dielectric membrane on which they are applied.

This manuscript shows the fabrication process for the manufacture of dielectric elastomer soft actuators based on silicone membranes. The three key stages of production are presented in detail: blade casting of thin silicone membranes; pad printing of compliant electrodes; and the assembly of all the components.

有机硅为基础的介电弹性体致动器的制作工艺

This contribution demonstrates the fabrication process of dielectric elastomer transducers (DETs). DETs are stretchable capacitors consisting of an ...

Fabrication of Polymer Microspheres for Optical Resonator and Laser Applications

This paper describes three methods of preparing fluorescent microspheres comprising &#960;-conjugated or non-conjugated polymers: vapor diffusion, interface precipitation, and mini-emulsion. In all methods, well-defined, micrometer-sized spheres are obtained from a self-assembling process in solution. The vapor diffusion method can result in spheres with the highest sphericity and surface smoothness, yet the types of the polymers able to form these spheres are limited. On the other hand, in the mini-emulsion method, microspheres can be made from various types of polymers, even from highly crystalline polymers with coplanar, &#960;-conjugated backbones. The photoluminescent (PL) properties from single isolated microspheres are unusual: the PL is confined inside the spheres, propagates at the circumference of the spheres via the total internal reflection at the polymer/air interface, and self-interferes to show sharp and periodic resonant PL lines. These resonating modes are so-called "whispering gallery modes" (WGMs). This work demonstrates how to measure WGM PL from single isolated spheres using the micro-photoluminescence (&#181;-PL) technique. In this technique, a focused laser beam irradiates a single microsphere, and the luminescence is detected by a spectrometer. A micromanipulation technique is then used to connect the microspheres one by one and to demonstrate the intersphere PL propagation and color conversion from coupled microspheres upon excitation at the perimeter of one sphere and detection of PL from the other microsphere. These techniques, &#181;-PL and micromanipulation, are useful for experiments on micro-optic application using polymer materials.

Protocols for the synthesis of microspheres from polymers, the manipulation of microspheres, and micro-photoluminescence measurements are presented.

用于光学谐振器和激光应用的聚合物微球的制造

This paper describes three methods of preparing fluorescent microspheres comprising &#960;-conjugated or non-conjugated polymers: vapor diffusion, ...

Scalable Solution-processed Fabrication Strategy for High-performance, Flexible, Transparent Electrodes with Embedded Metal Mesh

Here, the authors report the embedded metal-mesh transparent electrode (EMTE), a new transparent electrode (TE) with a metal mesh completely embedded in a polymer film. This paper also presents a low-cost, vacuum-free fabrication method for this novel TE; the approach combines lithography, electroplating, and imprint transfer (LEIT) processing. The embedded nature of the EMTEs offers many advantages, such as high surface smoothness, which is essential for organic electronic device production; superior mechanical stability during bending; favorable resistance to chemicals and moisture; and strong adhesion with plastic film. LEIT fabrication features an electroplating process for vacuum-free metal deposition and is favorable for industrial mass production. Furthermore, LEIT allows for the fabrication of metal mesh with a high aspect ratio (i.e., thickness to linewidth), significantly enhancing its electrical conductance without adversely losing optical transmittance. We demonstrate several prototypes of flexible EMTEs, with sheet resistances lower than 1 &#937;/sq and transmittances greater than 90%, resulting in very high figures of merit (FoM) &#8211; up to 1.5 x 104 &#8211; which are amongst the best values in the published literature.

This protocol describes a solution-based fabrication strategy for high-performance, flexible, transparent electrodes with fully-embedded, thick metal mesh. Flexible transparent electrodes fabricated by this process demonstrate among the highest reported performances, including ultra-low sheet resistance, high optical transmittance, mechanical stability under bending, strong substrate adhesion, surface smoothness, and environmental stability.

具有嵌入式金属网的高性能，灵活，透明电极的可扩展解决方案处理制造策略

Here, the authors report the embedded metal-mesh transparent electrode (EMTE), a new transparent electrode (TE) with a metal mesh completely embedded in a ...

Preparation of Large-area Vertical 2D Crystal Hetero-structures Through the Sulfurization of Transition Metal Films for Device Fabrication

We have demonstrated that through the sulfurization of transition metal films such as molybdenum (Mo) and tungsten (W), large-area and uniform transition metal dichalcogenides (TMDs) MoS2 and WS2 can be prepared on sapphire substrates. By controlling the metal film thicknesses, good layer number controllability, down to a single layer of TMDs, can be obtained using this growth technique. Based on the results obtained from the Mo film sulfurized under the sulfur deficient condition, there are two mechanisms of (a) planar MoS2 growth and (b) Mo oxide segregation observed during the sulfurization procedure. When the background sulfur is sufficient, planar TMD growth is the dominant growth mechanism, which will result in a uniform MoS2 film after the sulfurization procedure. If the background sulfur is deficient, Mo oxide segregation will be the dominant growth mechanism at the initial stage of the sulfurization procedure. In this case, the sample with Mo oxide clusters covered with few-layer MoS2 will be obtained. After sequential Mo deposition/sulfurization and W deposition/sulfurization procedures, vertical WS2/MoS2 hetero-structures are established using this growth technique. Raman peaks corresponding to WS2 and MoS2, respectively, and the identical layer number of the hetero-structure with the summation of individual 2D materials have confirmed the successful establishment of the vertical 2D crystal hetero-structure. After transferring the WS2/MoS2 film onto a SiO2/Si substrate with pre-patterned source/drain electrodes, a bottom-gate transistor is fabricated. Compared with the transistor with only MoS2 channels, the higher drain currents of the device with the WS2/MoS2 hetero-structure have exhibited that with the introduction of 2D crystal hetero-structures, superior device performance can be obtained. The results have revealed the potential of this growth technique for the practical application of 2D crystals.

Through the sulfurization of pre-deposited transition metals, large-area and vertical 2D crystal hetero-structures can be fabricated. The film transferring and device fabrication procedures are also demonstrated in this report.

硫化过渡金属膜制备大面积垂直2D 晶体杂化结构

We have demonstrated that through the sulfurization of transition metal films such as molybdenum (Mo) and tungsten (W), large-area and uniform transition ...

Fused Filament Fabrication (FFF) of Metal-Ceramic Components

Technical ceramics are widely used for industrial and research applications, as well as for consumer goods. Today, the demand for complex geometries with diverse customization options and favorable production methods is increasing continuously. With fused filament fabrication (FFF), it is possible to produce large and complex components quickly with high material efficiency. In FFF, a continuous thermoplastic filament is melted in a heated nozzle and deposited below. The computer-controlled print head is moved in order to build up the desired shape layer by layer. Investigations regarding printing of metals or ceramics are increasing more and more in research and industry. This study focuses on additive manufacturing (AM) with a multi-material approach to combine a metal (stainless steel) with a technical ceramic (zirconia: ZrO2). Combining these materials offers a broad variety of applications due to their different electrical and mechanical properties. The paper shows the main issues in preparation of the material and feedstock, device development, and printing of these composites.

Fused Filament Fabrication FFF of Metal-Ceramic Components

This study shows multi-material additive manufacturing (AM) using fused filament fabrication (FFF) of stainless steel and zirconia.

金属陶瓷元件的熔融长丝制造 (fff)

Technical ceramics are widely used for industrial and research applications, as well as for consumer goods. Today, the demand for complex geometries with ...