这项工作得到了中国国家自然科学基金 (51290292 号赠款) 的支持, 并得到了博士生北航学术优秀基金会的支持。

1. 不锈钢光刻
<ol><li>使用机械绘图软件设计光掩模, 并通过将其提交到光掩模打印机4来制造设计。</li>
	<li>清洗不锈钢 (316 SS; lengthx 宽度: 4 厘米 x 4 厘米, 厚度: 1 毫米), 在室温下用碱性溶液 (50 克/升氢氧化钠和40克/升 Na2CO3) 冲洗, 以除去油污。</li>
	<li>在超声波清洗机 (工作频率:40 赫, 超声波功率: 500 W) 上进行超声波清洗, 彻底清洁不锈钢。用去离子水、正己烷、丙酮和乙醇依次冲洗10分钟。</li>
	<li>将不锈钢放在150摄氏度的热板上晾干30分钟. 保护不锈钢, 用一张铝箔盖住它。</li>
	<li>将不锈钢放在旋转涂布机的中心。使用吸管将正光刻胶 (约1毫升) 存入不锈钢, 从中心到边缘, 直到光刻胶完全覆盖不锈钢。避免在光刻胶中形成气泡。<ol>
<li>执行自旋涂层, 首先以 700 rpm/分钟6秒的速度, 开始旋转周期, 然后以 1500 rpm/分钟的速度在十五年代, 均匀地传播光刻胶。</li>
	</ol>
</li>
	<li>松开真空阀, 用一双镊子回收不锈钢。将不锈钢放在热板上120摄氏度, 2 分钟烘烤光刻胶。</li>
	<li>将不锈钢放在光刻机的真空阀上。将光刻机的曝光时间设置为二十五年代。 注: 在这里, 光刻机是一个接触光刻与紫外线 (UV) 光波长的254毫微米和光强度为13兆瓦/厘米2。</li>
	<li>释放不锈钢, 并将其放在开发人员解决方案中1分钟, 以消除光刻胶, 而不暴露在 UV 光。从显影液中取出不锈钢, 用去离子水冲洗, 并在 N2气体下晾干。</li>
	<li>将不锈钢放在热板上烘烤120°c 2 分钟。</li>
	<li>用垂直显微镜放大 100x, 观察不锈钢表面, 检查所获得的光刻胶质地。</li>
</ol>2. 不锈钢的化学蚀刻
<ol><li>在100毫升烧杯中制备一个200毫升 (400 克/升 FeCl3, 20 克/升磷酸, 500 克/升盐酸) 的化学蚀刻溶液。</li>
	<li>将不锈钢与光刻胶质地放在化学溶液中10分钟。不要让不锈钢件相互接触。一次最多放置四个不锈钢件。</li>
	<li>用镊子取出化学蚀刻不锈钢, 用去离子水清洗1分钟, 用 N2气体将其烘干。</li>
	<li>通过将不锈钢在丙酮中浸入5分钟的超声波清洗, 去除光刻胶的质地。然后, 用 N2气体干燥化学蚀刻不锈钢。</li>
</ol>3. 化学蚀刻不锈钢的自组装
<ol><li>用稳定的去离子水清洗化学蚀刻不锈钢, 用 N2气体将其烘干, 并将其放在100摄氏度的热板上, 以使表面完全干燥。</li>
	<li>Hydroxylate 在射频等离子机中使用 O2等离子处理的化学蚀刻不锈钢, 其射频功率为100瓦特, 为10分钟, 系统压力为100毫巴, 流量为 20 sccm。</li>
	<li>在烧杯中制备无水甲苯1毫米溶液。在溶液准备前彻底干燥烧杯。</li>
	<li>在室温下用4小时的溶液冲洗化学蚀刻不锈钢。把烧杯放在密封的袋子里。不要让不锈钢件相互接触。</li>
	<li>取下不锈钢, 用无水甲苯清洗, 用10分钟进行超声波清洗, 用 N2气体将其烘干。</li>
</ol>4. 滑面制备
<ol><li>存约10毫升/厘米2硅油 (粘度: 350 cst; 表面张力: 21.1 锰/米) 上涂覆, 化学蚀刻不锈钢使用滴管。</li>
	<li>使用光学显微镜观察硅油在不锈钢表面的润湿过程 (放大率为 10x)。</li>
	<li>将不锈钢放置在垂直位置1小时, 除去多余的硅油。</li>
</ol>5. 滑面水滑动行为的研究
<ol><li>在滑面上沉积一个4µL 的水滴。将不锈钢置于光学显微镜下, 通过2°将基体倾斜。</li>
	<li>在低放大率 (50x) 下, 可视化水滴滑动在滑面上, 以检查滑面是否具有容易滑动的特性。</li>
</ol>6. 高温下湿滑表面的抗润湿性分析
<ol><li>用镊子将不锈钢与热板上的滑面放在一起。在不同的高温下设置热板 (即200 °c、250°c 和300°c), 以分析不同温度下的抗润湿行为。 注: 请勿用手直接接触高温不锈钢。</li>
	<li>用微型注射器在滑面上沉积10µL 的水滴。 注: 在水滴滴之前, 滑面的温度应达到平衡。</li>
	<li>使用高速相机记录水滴运动的帧速率为500赫兹。<ol>
<li>把相机固定在三脚架上, 将相机的镜头对准不锈钢。调整相机的焦距以获得清晰的水滴图像。通过推入相机的开始按钮, 记录不锈钢表面水滴的移动。当水滴滑离不锈钢以完成录音时, 按下相机的末端按钮。</li>
	</ol>
</li>
</ol>7. 滑面对软组织的抗粘连作用分析
<ol><li>使用机械手、测功机、热板和固定夹具设置粘附力测量平台4, 如图 3a所示。</li>
	<li>将测试面放在热板上。使用夹具固定在板上的不锈钢。将测试表面加热到一定的高温(例如, 300 °c)。 注: 试验表面应密切接触热板, 以确保有效的热运输到滑面。</li>
	<li>将测功器固定在机械手上。将气缸表 (直径: 2 厘米) 与一个力头连接, 作为一个软组织固定平台。</li>
	<li>修复软组织(例如,鸡胸肉; 长度: 5 厘米, 宽: 2 厘米, 厚度: 3 毫米), 用一根细线放在气缸上。确保软组织表面近似均匀。</li>
	<li>将软组织以1毫米/秒的速度加载到测试表面, 直到测功机通过旋转机械手的运动按钮达到一定的最大力 (例如, 4.5 N)。然后, 以同样的速度卸去软组织。</li>
	<li>使用数据传输线将计算机连接到测功机, 并记录软组织与测试表面之间的实时力。</li>
</ol>

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作者没有什么可透露的。

本手稿详细介绍了制造耐高温的光滑表面的协议。通过观察水滴的易滑动特性, 证明了所制备表面的光滑性能。通过在热面上沉积水滴, 研究了不同高温条件下制备的滑面的抗润湿性。结果表明, 即使在加热到300摄氏度以上的情况下, 所制备的滑面也保持了其光滑的性能。我们还确定了滑面对软组织的抗粘连作用。
与超疏水性表面不同, 滑面表面结构作为注入润滑剂的保温结构。根据前一项研究25, 由于硅油涂敷表面的优先亲和性, 水滴会漂浮在硅油注入的表面结构上, 如图 1B所示。此外, 这种液体/液体/固体界面给表面一个非常低的接触角滞后的液体液滴不溶于硅油。因此, 水滴可以很容易地滑动在准备好的滑面上。
由于不锈钢衬底的优良耐高温性、功能性层和注入硅油, 制备的滑面可在极高的温度下保持其光滑性能。然而, 在高温下, 水滴不会在表面滑动, 但它可以在表面上滚动。结果可归因于 Leidenfrost 效果26。在高温下, 硅油和水蒸发, 蒸汽可以形成一个蒸汽层之间的水滴和硅油层。事实上, 硅油和水滴的蒸发随着温度的升高而增加。因此, 在较高温度下的空气层有改善的能力, 以防止直接接触的水滴和硅油。类似的水滴在表面上滚动300°c (图 2C), 水滴几乎漂浮在空气层。接触是非常不稳定的, 因而它迅速地滑出表面。
润滑剂层也可作为软组织的抗粘连屏障。建立了粘附力测量平台, 研究了滑面对软组织的抗粘连作用。由于单纯的组织, 鸡乳房被选择为实验性软组织。软组织加载在光滑的不锈钢表面和滑面上。结果表明, 滑面上的粘附力显著降低 (即,从光滑表面上的0.80 到 0.18 n 到0.04 到 0.02 n 在滑面上)。这一概念为解决电切器械软组织粘连问题提供了新的见解。由于硅油和可生物相容的22,27, 我们的方法可以应用于电针仪器, 包括单手术刀和超声手术刀。
此外, 我们的方法是非常简单的, 可以进一步简化。柱结构使表面能够容纳更多的硅油, 而更多的硅油可以有效地充当软组织的屏障。但是, 如果不需要这么多的硅油, 例如当它用于防润湿的水滴, 不锈钢可以直接粗糙的化学蚀刻。简化方法简单, 可应用于不同的曲面类型, 包括曲面。应注意的是, 当表面加热到高温时, 硅油会蒸发, 并且在一定的时间后, 这种光滑的性能最终会失效。但是通过将硅油添加到表面, 它将重新获得光滑的性能。我们的协议的关键步骤是在表面结构上制备涂层, 这决定了滑面的最终光滑性能。因此, 应认真执行该程序集步骤。
滑面是一个新兴的功能表面, 以实现自我清洁, 抗粘连, 防结冰,等。它有许多优点, 包括易于制造, 不同液体的强健排斥, 良好的压力稳定性和自愈性。我们直接的方法提供了一种方法来构造一个具有高温电阻的光滑表面。我们认为, 所提出的方法将使滑面应用在医疗设备, 发动机, 热水管道等.

由于其在电刀仪器、发动机、管道等领域的广泛应用潜力, 在高温下用于液体和软组织的抗粘连表面受到了相当大的关注.1,2,3,4. Bioinspired 表面, 特别是超疏水性表面, 被认为是理想的选择, 因为它们具有优异的抗润湿能力和自清洁性能5。在超疏水性表面, 应将抗润湿能力归因于表面结构中的锁定空气。但是, 超疏水性状态不稳定, 因为它位于凯西-巴克斯特状态6, 7 中.同时, 在高温下, 由于从凯西-巴克斯特到 Wenzel 状态8的润湿状态转变, 液滴的抗润湿性可能会失败。这种润湿过渡是由于结构中的小液滴润湿引起的, 导致无法将空气锁定到位。
最近, 由于猪笼草的 peritome 的滑特性,猪笼草, 黄et 等. 报告了一个概念, 通过注入润滑剂到表面结构9,10, 构造光滑的表面 ,11。由于毛细力的缘故, 结构可以牢固地保持润滑剂到位, 就像在超疏水性表面的锁着的空气袋。因此, 润滑剂和表面结构可以形成稳定的固体/液体表面。当润滑剂对表面结构有优先的亲和力时, 复合表面的液滴会很容易滑动, 只有极低的接触角滞后 (例如, ~ 2°)12。这一润滑剂层还使表面具有显著的抗润湿能力13, 显示了医疗设备14,15的巨大潜力。然而, 以往对滑面的研究主要集中在室温或低温条件下的制备。对高温抗滑面的制备研究很少。例如, 张et表明, 润滑油的快速蒸发会迅速导致滑块的性能在稍高的温度下发生故障 (16)。
耐高温滑面可拓宽应用潜力;例如, 它们可以被用作液体屏障, 以减少对电刀器械的软组织粘连。手术过程中, 由于高频电刀提示的高温, 严重的软组织粘连发生。软组织可以烧焦, 导致它坚持的仪器提示, 然后撕裂软组织周围的提示17,18,19。术后粘附软组织对手术有负面影响, 也可能诱发止血失败19,20。这些影响严重损害了人们的健康和经济利益。因此, 解决电切器械软组织粘连问题迫在眉睫。事实上, 滑面提供了一个解决这个问题的机会。
在这里, 我们提出了一个协议, 以制造在高温下可用的滑面。不锈钢因其耐高温而被选为表面材料。采用光刻辅助化学蚀刻法对不锈钢进行了粗糙化。然后, 表面具有生物相容材料的功能, 生理盐水 octadecyltrichlorosilane ()21,22,23,24。通过添加硅油, 制备了一种光滑的表面。这些材料使光滑表面达到耐高温。研究了高温抗润湿性及对软组织的抗粘连作用。结果表明, 在高温下, 利用滑面来解决抗粘接问题的可能性很大。

<table width="614">
	<tbody>
		<tr height="48" style="height:36.0pt">
			<td class="xl17" height="48" style="width:128pt;height:36.0pt" width="171">Stainless steel</td>
			<td class="xl17" style="width:113pt" width="150">Hongtu Corporation</td>
			<td class="xl20" style="width:95pt" width="126">316</td>
			<td class="xl17" style="width:125pt" width="167">Use as received</td>
		</tr>
		<tr height="47" style="height:35.25pt">
			<td class="xl17" height="47" style="width:128pt;height:35.25pt" width="171">Octadecyltrichlorosilane</td>
			<td class="xl17" style="width:113pt" width="150">Huaxia Reagent</td>
			<td class="xl17" style="width:95pt" width="126">112-04-9</td>
			<td class="xl17" style="width:125pt" width="167">Use as received</td>
		</tr>
		<tr height="91" style="height:68.25pt">
			<td class="xl17" height="91" style="width:128pt;height:68.25pt" width="171">Photoresist</td>
			<td class="xl17" style="width:113pt" width="150">Kempur Microelectronic Corporation</td>
			<td class="xl16">317S</td>
			<td class="xl17" style="width:125pt" width="167">Use as received</td>
		</tr>
		<tr height="55" style="height:41.25pt">
			<td class="xl17" height="55" style="width:128pt;height:41.25pt" width="171">Silicone oil</td>
			<td class="xl17" style="width:113pt" width="150">Beijing Chemical Works</td>
			<td class="xl17" style="width:95pt" width="126">350 cst</td>
			<td class="xl17" style="width:125pt" width="167">Use as received</td>
		</tr>
		<tr height="52" style="height:39.0pt">
			<td class="xl16" height="52" style="height:39.0pt">Anhydrous toluene</td>
			<td class="xl17" style="width:113pt" width="150">Beijing Chemical Works</td>
			<td class="xl17" style="width:95pt" width="126">108-88-3</td>
			<td class="xl17" style="width:125pt" width="167">Use as received</td>
		</tr>
		<tr height="56" style="height:42.0pt">
			<td class="xl17" height="56" style="width:128pt;height:42.0pt" width="171">Phosphoric acid (H3PO4)</td>
			<td class="xl17" style="width:113pt" width="150">Tianjin Chemical Corporation</td>
			<td class="xl17" style="width:95pt" width="126">7664-38-2</td>
			<td class="xl17" style="width:125pt" width="167">Use as received</td>
		</tr>
		<tr height="63" style="height:47.25pt">
			<td class="xl17" height="63" style="width:128pt;height:47.25pt" width="171">Hydrochloric acid (HCl)</td>
			<td class="xl17" style="width:113pt" width="150">Tianjin Chemical Corporation</td>
			<td class="xl16">7647-01-0</td>
			<td class="xl17" style="width:125pt" width="167">Use as received</td>
		</tr>
		<tr height="56" style="height:42.0pt">
			<td class="xl16" height="56" style="height:42.0pt">Ferric chloride (FeCl3)</td>
			<td class="xl17" style="width:113pt" width="150">Tianjin Chemical Corporation</td>
			<td class="xl16">7705-08-0</td>
			<td class="xl17" style="width:125pt" width="167">Use as received</td>
		</tr>
		<tr height="54" style="height:40.5pt">
			<td class="xl17" height="54" style="width:128pt;height:40.5pt" width="171">Optical upright microscope</td>
			<td class="xl16">Olympus</td>
			<td class="xl16">BX51</td>
			<td class="xl16"></td>
		</tr>
		<tr height="46" style="height:34.5pt">
			<td class="xl17" height="46" style="width:128pt;height:34.5pt" width="171">Optical stereo microscope</td>
			<td class="xl16">Olympus</td>
			<td class="xl16">SZX16</td>
			<td class="xl16"></td>
		</tr>
		<tr height="50" style="height:37.5pt">
			<td class="xl16" height="50" style="height:37.5pt">High speed camera</td>
			<td class="xl16">Olympus</td>
			<td class="xl16">i-SPEED LT</td>
			<td class="xl16"></td>
		</tr>
		<tr height="52" style="height:39.0pt">
			<td class="xl17" height="52" style="width:128pt;height:39.0pt" width="171">Ultrasonic cleaner</td>
			<td class="xl19" style="width:113pt" width="150">KUNSHAN ULTRASONIC INSTRUMENTS CO. LTD</td>
			<td class="xl16">KQ-500E</td>
			<td></td>
		</tr>
		<tr height="49" style="height:36.75pt">
			<td class="xl17" height="49" style="width:128pt;height:36.75pt" width="171">Dynamometer</td>
			<td class="xl19" style="width:113pt" width="150">Yueqing Handapi Instruments Co. Ltd</td>
			<td class="xl16">HP-5</td>
			<td></td>
		</tr>
		<tr height="64" style="height:48.0pt">
			<td class="xl17" height="64" style="width:128pt;height:48.0pt" width="171">Manipulator</td>
			<td class="xl17" style="width:113pt" width="150">Yueqing Handapi Instruments Co. Ltd</td>
			<td class="xl16">HLD</td>
			<td></td>
		</tr>
		<tr height="62" style="height:46.5pt">
			<td class="xl17" height="62" style="width:128pt;height:46.5pt" width="171">Hot plate</td>
			<td class="xl17" style="width:113pt" width="150">Shenzhen Jingyihuang Corporation</td>
			<td class="xl16">DRB-1</td>
			<td></td>
		</tr>
	</tbody>
</table>

preparation and high-temperature anti-adhesion behavior of a slippery surface on stainless steel

耐高温抗粘连表面具有广泛的应用潜力, 在电刀仪器, 发动机和管道。典型的抗润湿超疏水性表面容易失效, 当暴露在高温液体。最近,猪笼草激发的滑面显示了解决粘附问题的新方法。在滑面上的润滑剂层可以充当被排斥材料与表面结构之间的屏障。然而, 以往研究中的滑面很少表现出耐高温。在这里, 我们描述了一个协议, 以制备耐高温光滑表面。采用光刻辅助法对不锈钢柱结构进行了制备。用盐水 functionalizing 表面, 通过添加硅油来制备光滑的表面。制备的滑面保持了水的抗润湿性, 即使表面加热到300摄氏度。同时, 滑面在高温下对软组织的抗粘连作用也很大。这种类型的不锈钢滑面在医疗设备, 机械设备,等方面的应用。

通过将硅油添加到涂覆的化学蚀刻不锈钢中, 制备了滑面。由于其相似的化学性质, 表面被硅油完全润湿。润湿过程显示在图 1a中。红色虚线标记润湿线。润湿后, 可见的油层可与干燥表面区分开来。用近似2°的角度, 在滑面上沉积水滴, 研究了制备的滑面的滑块性能。图 1b显示在滑面上的原位水滴移动。黄色虚线标记接触线, 结果显示水滴在滑面上漂浮和滑动。
研究了在高温下, 在水滴上制备的滑面的抗润湿行为。滑面被加热到不同的温度, 水滴沉积在表面。在200摄氏度 (图 2a) 中, 水滴首先牢固地接触到表面, 然后液滴和表面之间的接触区域减少。大约6200毫秒后, 水滴开始从表面滑落。在250摄氏度 (图 2b) 中, 水滴的初始接触区域与表面非常小。大约800毫秒后, 水滴开始从表面滑落。在300摄氏度 (图 2c) 中, 水滴在沉积后立即接触不稳定, 在250毫秒后迅速滑离滑面。
通过测定粘附力, 评价滑面对软组织的抗粘连作用。通过结合加热和操作系统 (图 3a), 我们建立了粘附力测量平台。该软组织被固定在测功机上, 连接到机械手, 测试表面固定在热板上。由于其纯组织, 鸡乳房被选为代表。在压力为 4.5 N 的测试表面加载软组织后, 卸载过程在软组织和试验表面之间产生了粘附力。结果显示在图 3b中。在光滑的不锈钢和滑面上, 粘附力分别为 0.80, 0.18 n 和 0.04, 0.02 n。与光滑的不锈钢表面相比, 粘附力在滑面上的大小阶数降低。
<img alt="Figure 1" class="xfigimg" src="/files/ftp_upload/55888/55888fig1.jpg"> 图1。滑面的形成过程及其滑块性质.(A) 硅油在涂覆的、化学蚀刻的不锈钢上的润湿过程。硅油由于分子层与硅油的相似化学性质, 可完全润湿表面。(B) 在硅油上漂浮的水滴, 并显示其容易滑动的性质。不锈钢的倾角约2°。<a href="https://cloudflare-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/55888/55888fig1large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>
<img alt="Figure 2" class="xfigimg" src="/files/ftp_upload/55888/55888fig2.jpg"> 图2。在高温下具有水滴的湿滑表面的抗润湿行为.水滴运动后, 被沉积在一个水平滑面在不同的高温: (a) 200 °c, (B) 250 °c, 和 (C) 300 °c。在一定时间后, 所有水滴从滑面上滑下, 水滴滑离的必要时间随着表面温度的升高而减小。<a href="https://cloudflare-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/55888/55888fig2large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>
<img alt="Figure 3" class="xfigimg" src="/files/ftp_upload/55888/55888fig3.jpg"> 图3。高温下软组织对滑面的抗粘附性评价.(A) 粘附力测量平台示意图。使用连接到测功机的机械手在测试表面加载软组织。粘附力被传送到计算机上。(B) 软组织与测试表面之间的粘附力。在300摄氏度的表面温度下, 软组织被加载到试验表面。与光滑的不锈钢表面相比, 滑面上的粘附力下降了约一级。显示的误差线是平均标准偏差 (SD)。<a href="https://cloudflare-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/55888/55888fig3large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>

Watch this Scientific Journal Video about Preparation and High-temperature Anti-adhesion Behavior of a Slippery Surface on Stainless Steel at JoVE.com

Preparation and High-temperature Anti-adhesion Behavior of a Slippery Surface on Stainless Steel

滑面为解决粘接问题提供了一种新的方法。本协议描述如何在高温下制造滑面。结果表明, 在高温下, 滑面表面对液体具有抗润湿性, 对软组织具有显著的抗粘附作用。

不锈钢滑面的制备及高温抗粘接性能研究

Anti-adhesion surfaces with high-temperature resistance have a wide application potential in electrosurgical instruments, engines, and pipelines. A ...

preparation-high-temperature-anti-adhesion-behavior-slippery-surface

Nanyang Technological University

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SCIENTISTS IN ACTION

7.5K 次观看.  Beihang University. 滑面为解决粘接问题提供了一种新的方法。本协议描述如何在高温下制造滑面。结果表明, 在高温下, 滑面表面对液体具有抗润湿性, 对软组织具有显著的抗粘附作用。

视频: Preparation and High-temperature Anti-adhesion Behavior of a Slippery Surface on Stainless Steel

Mechanical Expansion of Steel Tubing as a Solution to Leaky Wellbores

Wellbore cement, a procedural component of wellbore completion operations, primarily provides zonal isolation and mechanical support of the metal pipe (casing), and protects metal components from corrosive fluids. These are essential for uncompromised wellbore integrity. Cements can undergo multiple forms of failure, such as debonding at the cement/rock and cement/metal interfaces, fracturing, and defects within the cement matrix. Failures and defects within the cement will ultimately lead to fluid migration, resulting in inter-zonal fluid migration and premature well abandonment. Currently, there are over 1.8 million operating wells worldwide and over one third of these wells have leak related problems defined as Sustained Casing Pressure (SCP)1. 
The focus of this research was to develop an experimental setup at bench-scale to explore the effect of mechanical manipulation of wellbore casing-cement composite samples as a potential technology for the remediation of gas leaks. 
The experimental methodology utilized in this study enabled formation of an impermeable seal at the pipe/cement interface in a simulated wellbore system. Successful nitrogen gas flow-through measurements demonstrated that an existing microannulus was sealed at laboratory experimental conditions and fluid flow prevented by mechanical manipulation of the metal/cement composite sample. Furthermore, this methodology can be applied not only for the remediation of leaky wellbores, but also in plugging and abandonment procedures as well as wellbore completions technology, and potentially preventing negative impacts of wellbores on subsurface and surface environments.

This article reports on a laboratory scale investigation of an existing field procedure and its adaptation for sealing of leaky wellbores. It consists of mechanical expansion of metal pipe, which results in an improved metal/cement bond, ultimate sealing of hydraulic pathways and prevention of gas leaks caused by the presence of a microannular channel.

钢管机械性扩张为解决井眼漏

Wellbore cement, a procedural component of wellbore completion operations, primarily provides zonal isolation and mechanical support of the metal pipe ...

科研

工程学

Visualization of High Speed Liquid Jet Impaction on a Moving Surface

Two apparatuses for examining liquid jet impingement on a high-speed moving surface are described: an air cannon device (for examining surface speeds between 0 and 25 m/sec) and a spinning disk device (for examining surface speeds between 15 and 100 m/sec). The air cannon linear traverse is a pneumatic energy-powered system that is designed to accelerate a metal rail surface mounted on top of a wooden projectile. A pressurized cylinder fitted with a solenoid valve rapidly releases pressurized air into the barrel, forcing the projectile down the cannon barrel. The projectile travels beneath a spray nozzle, which impinges a liquid jet onto its metal upper surface, and the projectile then hits a stopping mechanism. A camera records the jet impingement, and a pressure transducer records the spray nozzle backpressure. The spinning disk set-up consists of a steel disk that reaches speeds of 500 to 3,000 rpm via a variable frequency drive (VFD) motor. A spray system similar to that of the air cannon generates a liquid jet that impinges onto the spinning disc, and cameras placed at several optical access points record the jet impingement. Video recordings of jet impingement processes are recorded and examined to determine whether the outcome of impingement is splash, splatter, or deposition. The apparatuses are the first that involve the high speed impingement of low-Reynolds-number liquid jets on high speed moving surfaces. In addition to its rail industry applications, the described technique may be used for technical and industrial purposes such as steelmaking and may be relevant to high-speed 3D printing.

Two experimental devices for examining liquid jet impingement on a high-speed moving surface are described: an air cannon device and a spinning disk device. The apparatuses are used to determine optimal approaches to the application of liquid friction modifier (LFM) onto rail tracks for top-of-rail friction control.

高速喷液嵌塞对移动表面的可视化

Two apparatuses for examining liquid jet impingement on a high-speed moving surface are described: an air cannon device (for examining surface speeds ...

Emission Spectroscopic Boundary Layer Investigation during Ablative Material Testing in Plasmatron

Ablative Thermal Protection Systems (TPS) allowed the first humans to safely return to Earth from the moon and are still considered as the only solution for future high-speed reentry missions. But despite the advancements made since Apollo, heat flux prediction remains an imperfect science and engineers resort to safety factors to determine the TPS thickness. This goes at the expense of embarked payload, hampering, for example, sample return missions. 
Ground testing in plasma wind-tunnels is currently the only affordable possibility for both material qualification and validation of material response codes. The subsonic 1.2MW Inductively Coupled Plasmatron facility at the von Karman Institute for Fluid Dynamics is able to reproduce a wide range of reentry environments. This protocol describes a procedure for the study of the gas/surface interaction on ablative materials in high enthalpy flows and presents sample results of a non-pyrolyzing, ablating carbon fiber precursor. With this publication, the authors envisage the definition of a standard procedure, facilitating comparison with other laboratories and contributing to ongoing efforts to improve heat shield reliability and reduce design uncertainties.
The described core techniques are non-intrusive methods to track the material recession with a high-speed camera along with the chemistry in the reactive boundary layer, probed by emission spectroscopy. Although optical emission spectroscopy is limited to line-of-sight measurements and is further constrained to electronically excited atoms and molecules, its simplicity and broad applicability still make it the technique of choice for analysis of the reactive boundary layer. Recession of the ablating sample further requires that the distance of the measurement location with respect to the surface is known at all times during the experiment. Calibration of the optical system of the applied three spectrometers allowed quantitative comparison. At the fiber scale, results from a post-test microscopy analysis are presented.

Development of new ablative materials and their numerical modeling requires extensive experimental investigation. This protocol describes procedures for material response characterization in plasma flows with the core techniques being non-intrusive methods to track the material recession along with the chemistry in the reactive boundary layer by emission spectroscopy.

烧蚀材料在试验过程中等离子体发生器发射光谱边界层研究

Ablative Thermal Protection Systems (TPS) allowed the first humans to safely return to Earth from the moon and are still considered as the only solution ...

The Evolution of Silica Nanoparticle-polyester Coatings on Surfaces Exposed to Sunlight

Corrosion of metallic surfaces is prevalent in the environment and is of great concern in many areas, including the military, transport, aviation, building and food industries, amongst others. Polyester and coatings containing both polyester and silica nanoparticles (SiO2NPs) have been widely used to protect steel substrata from corrosion. In this study, we utilized X-ray photoelectron spectroscopy, attenuated total reflection infrared micro-spectroscopy, water contact angle measurements, optical profiling and atomic force microscopy to provide an insight into how exposure to sunlight can cause changes in the micro- and nanoscale integrity of the coatings. No significant change in surface micro-topography was detected using optical profilometry, however, statistically significant nanoscale changes to the surface were detected using atomic force microscopy. Analysis of the X-ray photoelectron spectroscopy and attenuated total reflection infrared micro-spectroscopy data revealed that degradation of the ester groups had occurred through exposure to ultraviolet light to form COO&#903;, -H2C&#903;, -O&#903;, -CO&#903; radicals. During the degradation process, CO and CO2 were also produced.

Two types of surfaces, polyester-coated steel and polyester coated with a layer of silica nanoparticles, were studied. Both surfaces were exposed to sunlight, which was found to cause substantial changes in the chemistry and nanoscale topography of the surface.

表面上的纳米硅聚酯涂料暴露在阳光下的演变

Corrosion of metallic surfaces is prevalent in the environment and is of great concern in many areas, including the military, transport, aviation, ...

Applying X-ray Imaging Crystal Spectroscopy for Use as a High Temperature Plasma Diagnostic

X-ray spectra provide a wealth of information on high temperature plasmas; for example electron temperature and density can be inferred from line intensity ratios. By using a Johann spectrometer viewing the plasma, it is possible to construct profiles of plasma parameters such as density, temperature, and velocity with good spatial and time resolution. However, benchmarking atomic code modeling of X-ray spectra obtained from well-diagnosed laboratory plasmas is important to justify use of such spectra to determine plasma parameters when other independent diagnostics are not available. This manuscript presents the operation of the High Resolution X-ray Crystal Imaging Spectrometer with Spatial Resolution (HIREXSR), a high wavelength resolution spatially imaging X-ray spectrometer used to view hydrogen- and helium-like ions of medium atomic number elements in a tokamak plasma. In addition, this manuscript covers a laser blow-off system that can introduce such ions to the plasma with precise timing to allow for perturbative studies of transport in the plasma.

X-ray spectra provide a wealth of information on high temperature plasmas. This manuscript presents the operation of a high wavelength resolution spatially imaging X-ray spectrometer used to view hydrogen- and helium-like ions of medium atomic number elements in a tokamak plasma.

运用X射线成像光谱水晶的使用为高温等离子体诊断

X-ray spectra provide a wealth of information on high temperature plasmas; for example electron temperature and density can be inferred from line ...

Adsorption Device Based on a Langatate Crystal Microbalance for High Temperature High Pressure Gas Adsorption in Zeolite H-ZSM-5

We present a high-temperature and high-pressure gas adsorption measurement device based on a high-frequency oscillating microbalance (5 MHz langatate crystal microbalance, LCM) and its use for gas adsorption measurements in zeolite H-ZSM-5. Prior to the adsorption measurements, zeolite H-ZSM-5 crystals were synthesized on the gold electrode in the center of the LCM, without covering the connection points of the gold electrodes to the oscillator, by the steam-assisted crystallization (SAC) method, so that the zeolite crystals remain attached to the oscillating microbalance while keeping good electroconductivity of the LCM during the adsorption measurements. Compared to a conventional quartz crystal microbalance (QCM) which is limited to temperatures below 80 &#176;C, the LCM can realize the adsorption measurements in principle at temperatures as high as 200-300 &#176;C (i.e., at or close to the reaction temperature of the target application of one-stage DME synthesis from the synthesis gas), owing to the absence of crystalline-phase transitions up to its melting point (1,470 &#176;C). The system was applied to investigate the adsorption of CO2, H2O, methanol and dimethyl ether (DME), each in the gas phase, on zeolite H-ZSM-5 in the temperature and pressure range of 50-150 &#176;C and 0-18 bar, respectively. The results showed that the adsorption isotherms of these gases in H-ZSM-5 can be well fitted by Langmuir-type adsorption isotherms. Furthermore, the determined adsorption parameters, i.e., adsorption capacities, adsorption enthalpies, and adsorption entropies, compare well to literature data. In this work, the results for CO2 are shown as an example.

A protocol for high-temperature and high-pressure gas adsorption measurements on zeolite H-ZSM-5 using an adsorption measurement device based on a langatate crystal microbalance is presented. Prior to the adsorption measurements, the synthesis of zeolite H-ZSM-5 on the langatate crystal microbalance sensor by the steam-assisted crystallization (SAC) method is demonstrated.

基于一个Langatate体微天平的高温高压气体吸附在分子筛吸附器H-ZSM-5

We present a high-temperature and high-pressure gas adsorption measurement device based on a high-frequency oscillating microbalance (5 MHz langatate ...

High Temperature Fabrication of Nanostructured Yttria-Stabilized-Zirconia (YSZ) Scaffolds by In Situ Carbon Templating Xerogels

We demonstrate a method for the high temperature fabrication of porous, nanostructured yttria-stabilized-zirconia (YSZ, 8 mol% yttria - 92 mol% zirconia) scaffolds with tunable specific surface areas up to 80 m2&#183;g-1. An aqueous solution of a zirconium salt, yttrium salt, and glucose is mixed with propylene oxide (PO) to form a gel. The gel is dried under ambient conditions to form a xerogel. The xerogel is pressed into pellets and then sintered in an argon atmosphere. During sintering, a YSZ ceramic phase forms and the organic components decompose, leaving behind amorphous carbon. The carbon formed in situ serves as a hard template, preserving a high surface area YSZ nanomorphology at sintering temperature. The carbon is subsequently removed by oxidation in air at low temperature, resulting in a porous, nanostructured YSZ scaffold. The concentration of the carbon template and the final scaffold surface area can be systematically tuned by varying the glucose concentration in the gel synthesis. The carbon template concentration was quantified using thermogravimetric analysis (TGA), the surface area and pore size distribution was determined by physical adsorption measurements, and the morphology was characterized using scanning electron microscopy (SEM). Phase purity and crystallite size was determined using X-ray diffraction (XRD). This fabrication approach provides a novel, flexible platform for realizing unprecedented scaffold surface areas and nanomorphologies for ceramic-based electrochemical energy conversion applications, e.g. solid oxide fuel cell (SOFC) electrodes.

High Temperature Fabrication of Nanostructured Yttria-Stabilized-Zirconia YSZ Scaffolds by In Situ Carbon Templating Xerogels

A protocol for fabricating porous, nanostructured yttria-stabilized-zirconia (YSZ) scaffolds at temperatures between 1,000 &#176;C and 1,400 &#176;C is presented.

通过纳米氧化钇稳定的二氧化锆（YSZ）的支架的高温加工<em&gt;原位</em&gt;碳模板干凝胶

We demonstrate a method for the high temperature fabrication of porous, nanostructured yttria-stabilized-zirconia (YSZ, 8 mol% yttria - 92 mol% zirconia) ...

Preparation of Aligned Steel Fiber Reinforced Cementitious Composite and Its Flexural Behavior

The aim of this work is to present an approach, inspired by the way in which a compass needle maintains a consistent orientation under the action of the Earth&#39;s magnetic field, for manufacturing a cementitious composite reinforced with aligned steel fibers. Aligned steel fiber reinforced cementitious composites (ASFRC) were prepared by applying a uniform electromagnetic field to fresh mortar containing short steel fibers, whereby the short steel fibers were driven to rotate in alignment with the magnetic field. The degree of alignment of steel fibers in hardened ASFRC was assessed both by counting steel fibers in fractured cross-sections and by X-ray computed tomography analysis. The results from the two methods show that the steel fibers in ASFRC were highly aligned while the steel fibers in non-magnetically treated composites were randomly distributed. The aligned steel fibers had a much higher reinforcing efficiency, and the composites, therefore, exhibited significantly enhanced flexural strength and toughness. The ASFRC is thus superior to SFRC in that it can withstand greater tensile stress and more effectively resist cracking.

This protocol describes an approach for manufacturing aligned steel fiber reinforced cementitious composite by applying a uniform electromagnetic field. Aligned steel fiber reinforced cementitious composite exhibits superior mechanical properties to ordinary fiber reinforced concrete.

定向钢纤维增强水泥基复合材料的制备及其弯曲性能研究

The aim of this work is to present an approach, inspired by the way in which a compass needle maintains a consistent orientation under the action of the ...

Radio Frequency Magnetron Sputtering of GdBa2Cu3O7&#8722;&#948;/ La0.67Sr0.33MnO3 Quasi-bilayer Films on SrTiO3 (STO) Single-crystal Substrates

Here, we demonstrate a method of coating ferromagnetic La0.67Sr0.33MnO3 (LSMO) nanoparticles on (001) SrTiO3 (STO) single-crystal substrates by radio frequency (RF) magnetron sputtering. LSMO nanoparticles were deposited with diameters from 10 to 20 nm and heights between 20 and 50 nm. At the same time, (Gd) Ba2Cu3O7&#8722;&#948; ((Gd) BCO) films were fabricated on both undecorated and LSMO nanoparticle decorated STO substrates using RF magnetron sputtering. This report also describes the properties of GdBa2Cu3O7&#8722;&#948;/ La0.67Sr0.33MnO3 quasi-bilayer films structures (e.g., crystalline phase, morphology, chemical composition); magnetization, magneto-transport, and superconducting transport properties were also evaluated.

Radio Frequency Magnetron Sputtering of GdBa2Cu3O7ÃƒÆ’Ã‚Â¢Ãƒâ€¹Ã¢â‚¬Â 'ÃƒÆ’Ã…Â½ Â´/ La0.67Sr0.33MnO3 Quasi-bilayer Films on SrTiO3 STO Single-crystal Substrates

Here, we present a protocol to grow LSMO nanoparticles and (Gd) BCO films on (001) SrTiO3 (STO) single-crystal substrates by radio frequency (RF)-sputtering.

Gdba2cu 3 o7 的射频磁控管散射-/la0.67sr 0.67 mno 3 准双层薄膜上的 srtio 3 (sto) 单晶基板上

Here, we demonstrate a method of coating ferromagnetic La0.67Sr0.33MnO3 (LSMO) nanoparticles on (001) SrTiO3 (STO) single-crystal substrates by radio ...

Generating Lap Joints Via Friction Stir Spot Welding on DP780 Steel

Friction stir spot welding (FSSW), a derivative of friction stir welding (FSW), is a solid-state welding technique that was developed in 1991. An industry application was found in the automotive industry in 2003 for the aluminum alloy that was used in the rear doors of automobiles. Friction stir spot welding is mostly used in Al alloys to create lap joints. The benefits of friction stir spot welding include a nearly 80% melting temperature that lowers the thermal deformation welds without splashing compared to resistance spot welding. Friction stir spot welding includes 3 steps: plunging, stirring, and retraction. In the present study, other materials including high strength steel are also used in the friction stir welding method to create joints. DP780, whose traditional welding process involves the use of resistance spot welding, is one of several high strength steel materials used in the automotive industry. In this paper, DP780 was used for friction stir spot welding, and its microstructure and microhardness were measured. The microstructure data showed that there was a fusion zone with fine grain and a heat effect zone with island martensite. The microhardness results indicated that the center zone exhibited a greater degree of hardness compared with the base metal. All data indicated that the friction stir spot welding used in dual phase steel 780 can create a good lap joint. In the future, friction stir spot welding can be used in high-strength steel welding applied in industrial manufacturing processes.

Here, we present a friction stir spot welding (FSSW) protocol on dual phase 780 steel. A tool pin with high-speed rotation generates heat from friction to soften the material, and then, the pin plunges into 2 sheet joints to create the lap joint.

通过 DP780 钢上的摩擦搅拌点焊生成圈接头

Friction stir spot welding (FSSW), a derivative of friction stir welding (FSW), is a solid-state welding technique that was developed in 1991. An industry ...