这项工作是由阿克苏诺贝尔通过与曼彻斯特大学合作协议的支持。 PMG是感谢丰多扇形国家科学技术委员会 - SENER Hidrocarburos和研究所的墨西哥德Peteróleo财政支持。 TB感谢Mellitah石油与天然气Companyfor资助她的助学金。 KK确认来自通过材料的EPSRC（EP / L01680X / 1）财政支持要求苛刻的环境中心博士培训。"PAL感谢国家科学技术委员会的财政支持她在曼彻斯特的时光。最后，所有的作者承认本·斯宾塞对他的技术支持和建议。

1.基板/溶液的制备<ol><li> 碳制基板的制备 <ol><li>从一圆柱形碳钢杆（10±2毫米直径）3毫米厚的盘，使用精密切割机 - 剪切一个约2。采用在切割过程中的冷却流体，以尽量减少机械损伤。 </li><li>研磨既圆形面，并且与一系列的SiC砂纸盘形样品的边缘， 即 600目，800号粒度，1200号粒度的2400砂砾，和4000号粒度。 </li><li>得到波兰两个圆形面，并且所述盘形样品与任一金刚石糊剂或氧化铝粉末（3微米和/或1微米），直到一镜面光洁度的边缘。 </li><li>超声处理在室温下大约10分钟的样品中的每一个下面的:去离子水，丙酮，乙醇，最后再次去离子水。 </li><li>干燥的空气流下的样品的所有表面。 </li><li>在商店的样品或者干燥器或真空干燥器直到需要。理想情况下，最终制成碳钢基体之前，为了溶液浸泡。 </li></ol></li><li> 抑制的1M HCl溶液中制备 <ol><li>添加10.2 M盐酸到去离子水中以产生的1M HCl溶液中。注意:盐酸是有害的，有腐蚀性。承接在通风橱这一步，穿着合适的个人防护装备。 </li><li>在1M HCl溶液溶解选定的有机-Cl（ 如 X =0.300克2-巯基苯并咪唑）的XG以产生含有x毫有机-Cl（ 例如 X = 2毫摩尔2-巯基苯并咪唑）中的1M HCl溶液。 </li></ol></li></ol> 2.底物浸入抑制的酸溶液<ol><li>倒入一个小体积-中的1M HCl + X毫（ 例如 X = 2毫摩尔2-巯基苯并咪唑）有机-Cl溶液到一个小玻璃烧杯中（一般为25 50毫升）中。 </li><li>拾起盘形碳钢样品与陶瓷或复astic镊子是至1M的HCl抗性。只摸与镊子将样品的边缘。 </li><li>引入样品进入含有的1M HCl + X毫有机-Cl溶液的玻璃烧杯中。定向样品以便圆柱面是在垂直平面上。沉积样品直接到烧杯的底部，或顶上的短玻璃管的开口端。确保样品完全浸没。 </li></ol> 3.样品转移<ol><li> 手套箱准备 <ol><li>定位在手套箱的底部的圆形样品转移开口到该XPS加载互锁法兰安装。保证手套箱和装载锁定凸缘之间的密封是正确形成。 </li><li>手套箱连接到惰性气体筒（不管是N 2或Ar）。 </li><li>坚持双面碳（导电）带的一个小广场上XPS样吧。 </li><li>插入所需样品转移到XPS仪器硬件通过手套箱开放端口，附有碳纤维带，塑料/陶瓷镊子，丁腈手套，实验室组织，塑料石蜡膜，空/干洗瓶带嘴和玻璃烧杯即样品条含〜200克Na 2 CO 3粉末。 </li><li>含碳钢样品中的1M HCl + X毫（ 例如 X = 2毫摩尔2-巯基苯并咪唑）手套箱内有机-Cl溶液代替玻璃烧杯中。确保样品始终在这一步完全浸没。 </li><li>密封在手套箱的所有端口/入口点，并开始与N 2（或Ar）清除。 </li><li>不断清除手套箱直到样品传输完成。 </li></ol></li><li> 从溶液中的XPS分析室 <ol><li>允许样品中的1 M盐酸+所需浸渍期间离开Xmm有机-Cl溶液保持淹没， 如 4小时，作为用于该XPS数据如下。 </li><li>检查RELA手套箱内略去湿度被最小化，其通常实现后60 - 发起吹扫90分钟。 8％的相对湿度的值与样品传输继续之前必需的;清除前值通常是35 - 40％。 注意:通常情况下，有手套箱内没有专用的 O 2传感器，而试验测量结果与这样的设备指示该清洗过程由〜1000倍导致的 O 2浓度的降低。 </li><li>引进双手放进手套箱手套，再涂戴手套的手与位于手套箱内丁腈手套。这一步骤减少了污染的样品处理过程中的可能性，以及增加了便于样品操纵。 </li><li>取下的1M HCl + X毫（ 例如 X = 2毫摩尔2-巯基苯并咪唑）有机-Cl溶液的碳钢试样，使用陶瓷材料/塑料镊子。只摸与镊子将样品的边缘。 </li><li> Immediat伊利再现后，通过引导惰性气体流，反复挤空/干洗瓶位于手套箱内，到样品表面产生吹样品干燥。 注:在此阶段用溶剂漂洗未进行，以尽量减少损坏抑制界面， 例如除去抑制剂或接口氧化的电位。 </li><li>含有1M的HCl + X毫有机-Cl塑料石蜡膜溶液覆盖烧杯中。 </li><li>加盖样品连接到XPS样品条双面碳（导电）胶带的小广场。请勿触摸到的XPS被探测的表面。 </li><li>泄该XPS加载互锁真空室到N 2 /氩。确保相关的涡轮/机械泵组合执行此操作前关闭。 </li><li>打开负载锁定凸缘。 </li><li>转移样品条放入装载室并将其推到试样固定插脚。 </li><li>关闭负载锁凸缘。 </li><li>开关关于涡轮/旋转泵组合抽空装载室。 </li><li>一旦在装载锁定腔室的压力达到至少约5×10 -7毫巴，手动样品使用传送臂传送到中间室。 </li><li>等到在中间室的压力达到约1×10 -8毫巴，然后使用第二传送臂在分析室样品手动转移到样品操纵器。 </li></ol></li></ol> 4. XPS数据采集<ol><li>样品的取向角，使用小键盘来驱动样品操纵器马达，以期望的光电子发射角， 例如 0°（沿表面法线发射），作为用于以下提出的XPS数据。 </li><li>通过点击位于桌面上的图标打开的XPS数据采集软件。打开仪器手动控制窗口。 </li><li>输入端10 mA和分别为15千伏，作为阳极排放和阳极HT参数的值。然后，单击"X射线枪"部分的单色化的AlKαX射线源功率达"中"按钮。在此之后，点击"中和剂"部分中的"ON"按钮打开充电中和剂。 </li><li>选择电子分析仪"的频谱/混合"测量距离"模式"模式和"镜头"下拉菜单中的"分析"部分。 </li><li>输入所需的动能/结合能范围内，通过能源（IES），步长（s）和停留时间（s）到"采集/扫描控制"部分。例如输入参数值:1200 - 0 eV的结合能范围，80 eV的通能，0.5 EV步长大小，和0.1秒停留时间获取概述谱。 </li><li>通过调整样本机械手的位置，使用键盘驱动样品操纵电机优化样品位置，最大限度地从选定的核心层面， 例如 C 1或铁2P信号。 </li><li>在XPS数据采集启动数据采集获得X射线光电子能谱软件。 </li></ol>

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The authors declare that they have no competing financial interests.

XPS光谱显示在图1和2清楚地表明，样品转移过程中所用的惰性气氛是至关重要的，以避免这些碳钢/有机-Cl接口的交浸入氧化。在此基础上，从其他类似的XPS研究的结果（ 如 18，19），其中所涉及的抑制基底到环境实验室气氛的曝光，应该严格重新评估，作为界面化学可能是通过氧化改性。应当指出的是，没有理由假定所有有机顺吸附到在酸性溶液中的氧化物/氢氧化物自由表面。在某些情况下，这种相可确实促进有机-Cl表面结合。区分后浸入氧化这种情况并非如此简单。一个可能的解决方案是获得来自参考抑制接口XPS数据（ <eM&gt;如1 M盐酸+ 2mM的MBI）在与感兴趣的样品以检查后浸入氧化串联是不是一个问题。 以确保成功的结果，以样品传输的程序，它是必不可少的手套箱完全用惰性气体（N 2 /氩）置换，即在手套箱中的 O 2浓度被最小化。应注意，以验证在手套箱端口/入口点的所有密封件被正确地形成，包括手套箱和XPS装载锁定凸缘之间的密封。理想情况下， 在原位传感器应该被用来直接监测O 2的浓度，虽然不是必要的，由我们自己的工作所证明。如步骤3.3.2所示，我们通常使用一个相对湿度传感器作为时承接了样品转移的指南。 与手套箱环境中的一个进一步的潜在问题是挥发性的溶液成分的存在，其可污染以下从溶液中并在插入之前移除到负载锁定样品表面。例如，在手套箱中的1M HCl溶液中的存在导致的HCl蒸气，它可与碳的钢试样导致不定C1信号在XPS数据起反应的演化。为了尽量减少这样的污染是显著的可能性，盐酸溶液小体积应采用与样品传输应尽可能快地完成。在此基础上，作为协议中所指出的，通常只有一个烧杯/样品被插入到为在任一时刻样品转移手套箱。此外，应尽量减少HCl溶液的表面积，以及覆盖下面的示例再现的烧杯中。 的 Na 2 CO 3粉末（步骤3.1.4）被插入到手套式操作箱中试图控制的HCl蒸气量。此外，它可以用来清理任何酸性溶液溢漏。 除了手套的B小心控制牛的环境中，样品处理也是获得XPS光谱的完整性至关重要。人们不应从已接触到任何固体物体， 如镊子或手套接触的任何表面获取XPS数据。此外，在除去从溶液的样品，应当立即吹入干燥的惰性气体（步骤3.2.5）。此过程进行的，以防止蒸发和溶液组分的后续物理沉积到样品表面上，这可能导致数据的误解。作为附加的预防措施，还可以考虑用新鲜对取代的腈手套（步骤3.2.3）对样品棒转移到加载互锁真空室， 即前到步骤3.1.10。 最后，鉴于此处所述的方法的有效性，我们期望它在腐蚀可以应用于其他主题（ 即除了缓蚀），其中XPS数据的从空气敏感接口采集将添加到understanding。此外，这样的做法应该在XPS测量从形成于液体环境空气敏感的接口进行的其他领域加以考虑。显然，该过程并不限于XPS，但也可以从先前已经浸入在液体中的表面， 例如 ，扫描探针显微术应用到任何其他基于UHV-测量。

腐蚀抑制剂（CI）的是物质，当引入侵蚀性环境，通过在固/液界面1，2，3，4，5诱导的变化降低的金属材料的腐蚀速率。这种方法来腐蚀控制被广泛用于工业，具有高性能的CI具有用于各种应用已研制成功。但是仍然存在，相当缺乏的表现CI基本认识，阻碍了以知识为基础的优化。例如，通过有机顺腐蚀性酸性溶液形成接口的确切性质目前还不清楚。 鉴于假设有机顺通形成中吸附的2-D层2的抑制酸性腐蚀，表面敏感的技术是必需的牛逼Ø描述这些接口。因此，X射线光电子能谱（XPS）6已成为选择的技术来探测这些界面的元素/化学组成易地 7，8，9; XPS测量典型地执行在，或接近，超高真空（UHV）。各种见解已声称，包括一个表面的氧化物或氢氧化物的存在，以促进有机-Cl结合到金属基片10，11，12。该接口描述的有效性，但是，是值得怀疑的XPS数据是从已被从抑制溶液和引入到UHV-XPS光谱仪暴露于实验室气氛中去除之间的样本获得的。这样的程序可能会导致接口氧化，破坏了有关结论界面的化学组成。另一种方法是必需的，这对于后浸入氧化的可能性降至最低。 在本文中，我们详细设计了一个方法，让一个从没有经过氧化以下从酸性溶液中再现有机-CI /金属界面获取XPS数据。的手套箱中，用惰性气体吹扫，这是直接附连到UHV-XPS仪器的真空加载互锁采用。我们的方法的效用是通过XPS数据的呈现从以下除了足够的CI以显著降低在水性1M盐酸（HCl）的溶液在基板的腐蚀速率的形成的两个有机-CI /碳钢接口验证。

<table border="1" fo:keep-together.within-page="1" fo:keep-with-next.within-page="always">
	<tbody>
		<tr>
			<td>Mild steel rod, 1m x 10 mm diameter</td>
			<td>RS Components&#160;</td>
			<td>770-412</td>
			<td></td>
		</tr>
		<tr>
			<td>Silicon Carbide Grinding papers</td>
			<td>Spectrographic Limited</td>
			<td>T13316, T13317, T13318, T13156, T13153</td>
			<td></td>
		</tr>
		<tr>
			<td>Polishing Cloth</td>
			<td>Spectrographic Limited</td>
			<td>62113</td>
			<td></td>
		</tr>
		<tr>
			<td>Monocrystalline Diamond compound</td>
			<td>Spectrographic Limited</td>
			<td>G22003</td>
			<td></td>
		</tr>
		<tr>
			<td>OmegaPol TWIN 250mm Metallurgical Polisher</td>
			<td>Spectrographic Limited</td>
			<td>n/a</td>
			<td></td>
		</tr>
		<tr>
			<td>BRILLANT 220 - Wet Abrasive Cut-Off Machine</td>
			<td>ATM GmbH Advanced Materialography</td>
			<td>n/a</td>
			<td></td>
		</tr>
		<tr>
			<td>Ultrasonic Bath</td>
			<td>NICKEL-ELECTRO LTD.</td>
			<td>SW3H</td>
			<td></td>
		</tr>
		<tr>
			<td>Vacuum Desiccator</td>
			<td>DURAN</td>
			<td>24 782 57</td>
			<td></td>
		</tr>
		<tr>
			<td>Low form beaker 25mL</td>
			<td>Fisher Scientific</td>
			<td>FB33170</td>
			<td></td>
		</tr>
		<tr>
			<td></td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>N2 gas cylinders, 230 bar, size W, UN1066</td>
			<td>BOC</td>
			<td>n/a</td>
			<td></td>
		</tr>
		<tr>
			<td>Regulator for N2 gas cylinders</td>
			<td>Freshford Ltd.</td>
			<td>MS-10B-N2</td>
			<td></td>
		</tr>
		<tr>
			<td>Nitrogen Purge Glove Box</td>
			<td>Terra Universal, Inc</td>
			<td>n/a</td>
			<td></td>
		</tr>
		<tr>
			<td>Dual Purge System</td>
			<td>Terra Universal, Inc</td>
			<td>1606-61</td>
			<td></td>
		</tr>
		<tr>
			<td>NitroWatch System with sensor</td>
			<td>Terra Universal, Inc</td>
			<td>9500-00A, 9500-02A</td>
			<td></td>
		</tr>
		<tr>
			<td>Big Digit Hygro-Thermometer</td>
			<td>FLIR Commercial Systems, Inc. Extech Instruments Division</td>
			<td>445703</td>
			<td></td>
		</tr>
		<tr>
			<td>Kratos Axis Ultra (XPS spectrometer)</td>
			<td>Kratos Analytical Ltd</td>
			<td>n/a</td>
			<td></td>
		</tr>
	</tbody>
</table>

determining the chemical composition of corrosion inhibitor/metal interfaces with xps: minimizing post immersion oxidation

用于获取从腐蚀抑制剂/金属界面更可靠的X射线光电子能谱法数据的方法进行说明。更具体而言，重点是在浸渍在含有有机腐蚀抑制剂的酸性溶液金属基材，因为这些系统可以如下从溶液中除去是对氧化特别敏感。为了尽量减少这样的降解的可能性，将样品从用惰性气体吹扫的手套箱内溶液中除去，或者N 2或Ar。手套箱被直接附着到超高真空X射线光电子能谱仪器的加载互锁，避免任何暴露于实验室环境的气氛，从而降低交浸入底物氧化的可能性。在此基础上，人们可以更确信所观察到的X射线光电子能谱特征很可能是代表的原位淹没的情况下， 例如第m的氧化态等人没有被修改。

图1显示了概述，澳1S和Fe 2P XPS数据碳钢样本收购已浸泡4小时，在两个不同的1M HCl + X毫米有机-CI的解决方案之一，并转移了XPS测量上面详细。从抛光样品类似数据也被显示。碳钢具有C（0.08-0.13），锰（0.30-0.50），P（0.04），S（0.05）的标称重量％的组合物，和Fe（平衡量）。研究了两种有机顺有:2-巯基苯（MBI）和（Z）-2-2（2-（十八碳-9-烯-1-基）-4,5-二氢-1H-咪唑-1-基）乙胺（OMID）。在所使用的浓度（MBI:2毫米; OMID:1毫米）的腐蚀速率的测量13,14表明所有物种的显著抑制碳钢， 即抑制效率（η％）2&gt; 90％的腐蚀。最适合向O 1和铁2P光谱图也显示。光电子峰用高斯洛伦兹（GL）线的形状的功能（30％洛伦兹）建模，用金属铁，其中使用洛伦兹不对称线形状与尾阻尼（LF）中的Fe 2P级除外。阳离子铁X +的状态，用由3和4 GL功能的Fe 2+和Fe 3+，15多峰信封建模。一个雪莉型功能16被用来描述非弹性散射电子的背景。 重点概述XPS数据（ 图1（a）），从抛光样品获得的光谱显示三个主峰， 即铁2P，澳1S，和C 1秒。这些特征可以如下分配:铁2P源于碳钢，O- 1秒从同时具有表面氧化膜和吸附物派生，以及C 1秒信号以不定碳水化合物是由于上。淹没在任何给相应的频谱概述变化显著的1 M盐酸+ X毫米有机-CI方案的结果。分配给N 1s电子出现的水平，这是与抑制剂的表面吸附一致的特征; MBI和OMID都包含N.此外，O1s的核心层信号显著减少。 如从抛光的衬底方面Ô1秒的数据（ 图1（b）），该简档可以配备四个组件。在较低的结合能的两种组分（BE），〜530.0 eV和〜531.3 eV的，可以分配到铁氧化物（O 2-）和氢氧化（OH - ）相，分别两个较高结合能的组件，标记为O 1（BE〜532.2 EV）和O 2（BE〜533.3电子伏特），很可能与吸附OH（O 1）和不定碳物种（O 1和O 2）17相关联。沉浸在任的t他的1M HCl + X毫米有机-CI方案导致O 2-和OH完全淬火-组件。在此基础上，可以得出结论认为，腐蚀抑制剂被吸附在氧化物/氢氧化物自由表面。在图1（c）该铁的2p光谱是一致的这个结果，因为只有一个金属的Fe（铁0）峰是在抑制衬底显而易见。 的 Fe 2+和Fe 3+特征存在于抛光样品，由于表面氧化物/氢氧化物。 Ò1和铁的2p芯能级的XPS谱图从浸入的1M HCl + 2毫MBI两个碳-钢样在图2中进行了比较。一个样品用一个充分的 N 2 -purged手套箱传送，而另一个是从溶液中去除到部分N 2 -purged手套箱， 即 O 2的浓度比目标值显著高。对于后者样品，我t是显而易见已经发生交浸入氧化， 即 的 Fe 2 + / 3 +和O 2- / OH -功能都存在。 <img alt="图1" src="/files/ftp_upload/55163/55163fig1.jpg" /> 从抛光和抑制碳钢样品 图1. XPS谱。 （ 一 ）概述（ 二 ）O 1S，和（c）铁2P XPS光谱。在每个面板中表示的数据是从已被浸渍4小时在一个的两个不同的1M HCl + X毫有机-Cl溶液， 即 2毫MBI，和1mM OMID碳钢样品获得的。光谱所有以0°（沿表面法线发射）的光电子发射角（θE）获得的。为（b）和（c）该最佳拟合（浅蓝色的标记）的实验数据（实心黑色线）也被显示，与GL的组合来实现（碎红色线），LF（破ř<html>编线），和Shirley型（破灰线）的功能。山顶标签在正文中说明。 <a href="http://ecsource.jove.com/files/ftp_upload/55163/55163fig1large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图2" src="/files/ftp_upload/55163/55163fig2.jpg" /> 图 2. XPS光谱后浸泡氧化的影响。 （ 一 ）O 1S和（b）铁2P XPS光谱。数据是从已被浸渍于1 M盐酸+ 2mM的MBI溶液（η（％）= 99％）4小时碳钢样品获得的。谱在θE = 0°收购。在每个面板，下部（上部）的频谱是从通过一个完全（部分） 的 N 2 -purged手套箱转移样品。山顶标签在正文中说明。 （参考文献中的修改版图5。9）OAD / 55163 / 55163fig2large.jpg"目标="_空白"&gt;点击此处查看该图的放大版本。

Watch this Scientific Journal Video about Determining the Chemical Composition of Corrosion Inhibitor/Metal Interfaces with XPS: Minimizing Post Immersion Oxidation at JoVE.com

Determining the Chemical Composition of Corrosion Inhibitor/Metal Interfaces with XPS: Minimizing Post Immersion Oxidation

A protocol to avoid the oxidation of metallic substrates during sample transfer from an inhibited acidic solution to an X-ray photoelectron spectrometer is presented.

确定缓蚀剂/金属界面的化学成分与XPS:最小化后浸入氧化

An approach for acquiring more reliable X-ray photoelectron spectroscopy data from corrosion inhibitor/metal interfaces is described. More specifically, ...

determining-chemical-composition-corrosion-inhibitormetal-interfaces

Research

JoVE Journal

Chemistry

15.7K 次观看.  The University of Manchester. A protocol to avoid the oxidation of metallic substrates during sample transfer from an inhibited acidic solution to an X-ray photoelectron spectrometer is presented. 

视频: Determining the Chemical Composition of Corrosion Inhibitor/Metal Interfaces with XPS: Minimizing Post Immersion Oxidation

Isolation and Chemical Characterization of Lipid A from Gram-negative Bacteria

Lipopolysaccharide (LPS) is the major cell surface molecule of gram-negative bacteria, deposited on the outer leaflet of the outer membrane bilayer. LPS can be subdivided into three domains: the distal O-polysaccharide, a core oligosaccharide, and the lipid A domain consisting of a lipid A molecular species and 3-deoxy-D-manno-oct-2-ulosonic acid residues (Kdo). The lipid A domain is the only component essential for bacterial cell survival. Following its synthesis, lipid A is chemically modified in response to environmental stresses such as pH or temperature, to promote resistance to antibiotic compounds, and to evade recognition by mediators of the host innate immune response. The following protocol details the small- and large-scale isolation of lipid A from gram-negative bacteria. Isolated material is then chemically characterized by thin layer chromatography (TLC) or mass-spectrometry (MS). In addition to matrix-assisted laser desorption/ionization-time of flight (MALDI-TOF) MS, we also describe tandem MS protocols for analyzing lipid A molecular species using electrospray ionization (ESI) coupled to collision induced dissociation (CID) and newly employed ultraviolet photodissociation (UVPD) methods. Our MS protocols allow for unequivocal determination of chemical structure, paramount to characterization of lipid A molecules that contain unique or novel chemical modifications. We also describe the radioisotopic labeling, and subsequent isolation, of lipid A from bacterial cells for analysis by TLC. Relative to MS-based protocols, TLC provides a more economical and rapid characterization method, but cannot be used to unambiguously assign lipid A chemical structures without the use of standards of known chemical structure. Over the last two decades isolation and characterization of lipid A has led to numerous exciting discoveries that have improved our understanding of the physiology of gram-negative bacteria, mechanisms of antibiotic resistance, the human innate immune response, and have provided many new targets in the development of antibacterial compounds.

Isolation and characterization of the lipid A domain of lipopolysaccharide (LPS) from gram-negative bacteria provides insight into cell surface based mechanisms of antibiotic resistance, bacterial survival and fitness, and how chemically diverse lipid A molecular species differentially modulate host innate immune responses.

隔离和脂质A的化学表征革兰氏阴性菌

Lipopolysaccharide (LPS) is the major cell surface molecule of gram-negative bacteria, deposited on the outer leaflet of the outer membrane bilayer. LPS ...

科研

化学

Chemical Vapor Deposition of an Organic Magnet, Vanadium Tetracyanoethylene

Recent progress in the field of organic materials has yielded devices such as organic light emitting diodes (OLEDs) which have advantages not found in traditional materials, including low cost and mechanical flexibility. In a similar vein, it would be advantageous to expand the use of organics into high frequency electronics and spin-based electronics. This work presents a synthetic process for the growth of thin films of the room temperature organic ferrimagnet, vanadium tetracyanoethylene (V[TCNE]x, x~2) by low temperature chemical vapor deposition (CVD). The thin film is grown at &#60;60 &#176;C, and can accommodate a wide variety of substrates including, but not limited to, silicon, glass, Teflon and flexible substrates. The conformal deposition is conducive to pre-patterned and three-dimensional structures as well. Additionally this technique can yield films with thicknesses ranging from 30 nm to several microns. Recent progress in optimization of film growth creates a film whose qualities, such as higher Curie temperature (600 K), improved magnetic homogeneity, and narrow ferromagnetic resonance line-width (1.5 G) show promise for a variety of applications in spintronics and microwave electronics.

We present the synthesis of the organic-based ferrimagnet vanadium tetracyanoethylene (V[TCNE]x, x~2) via low temperature chemical vapor deposition (CVD). This optimized recipe yields an increase in Curie temperature from 400 K to over 600 K and a dramatic improvement in magnetic resonance properties.

化学气相沉积的有机磁体，钒四氰

Recent progress in the field of organic materials has yielded devices such as organic light emitting diodes (OLEDs) which have advantages not found in ...

Layer-by-layer Synthesis and Transfer of Freestanding Conjugated Microporous Polymer Nanomembranes

CMP as large surface area materials have attracted growing interest recently, due to their high variability in the incorporation of functional groups in combination with their outstanding thermal and chemical stability, and low densities. However, their insoluble nature causes problems in their processing since usually applied techniques such as spin coating are not available. Especially for membrane applications, where the processing of CMP as thin films is desirable, the processing problems have hindered their commercial application.
Here we describe the interfacial synthesis of CMP thin films on functionalized substrates via molecular layer-by-layer (l-b-l) synthesis. This process allows the preparation of films with desired thickness and composition and even desired composition gradients.
The use of sacrificial supports allows the preparation of freestanding membranes by dissolution of the support after the synthesis. To handle such ultra-thin freestanding membranes the protection with sacrificial coatings showed great promise, to avoid rupture of the nanomembranes. To transfer the nanomembranes to the desired substrate, the coated membranes are upfloated at the air-liquid interface and then transferred via dip coating.

In this paper we describe the interfacial synthesis of conjugated microporous polymers (CMP) on sacrificial substrates, and the dissolution of the substrate for the preparation of freestanding CMP nanomembranes. In addition, we will describe how the fragile nanomembranes can be transferred to other substrates.

层 - 层的合成和独立式共轭微孔聚合物纳米薄膜的转移

CMP as large surface area materials have attracted growing interest recently, due to their high variability in the incorporation of functional groups in ...

Assessment of Boron Doped Diamond Electrode Quality and Application to In Situ Modification of Local pH by Water Electrolysis

Boron doped diamond (BDD) electrodes have shown considerable promise as an electrode material where many of their reported properties such as extended solvent window, low background currents, corrosion resistance, etc., arise from the catalytically inert nature of the surface. However, if during the growth process, non-diamond-carbon (NDC) becomes incorporated into the electrode matrix, the electrochemical properties will change as the surface becomes more catalytically active. As such it is important that the electrochemist is aware of the quality and resulting key electrochemical properties of the BDD electrode prior to use. This paper describes a series of characterization steps, including Raman microscopy, capacitance, solvent window and redox electrochemistry, to ascertain whether the BDD electrode contains negligible NDC i.e. negligible sp2 carbon. One application is highlighted which takes advantage of the catalytically inert and corrosion resistant nature of an NDC-free surface i.e. stable and quantifiable local proton and hydroxide production due to water electrolysis at a BDD electrode. An approach to measuring the local pH change induced by water electrolysis using iridium oxide coated BDD electrodes is also described in detail.

Assessment of Boron Doped Diamond Electrode Quality and Application to In Situ Modification of Local pH by Water Electrolysis

A protocol is described for the characterization of the key electrochemical parameters of a boron doped diamond (BDD) electrode and subsequent application for in situ pH generation experiments.

掺硼金刚石电极质量和应用，以评估<em&gt;原位</em&gt;本地pH值通过水电改造

Boron doped diamond (BDD) electrodes have shown considerable promise as an electrode material where many of their reported properties such as extended ...

A Method to Manipulate Surface Tension of a Liquid Metal via Surface Oxidation and Reduction

Controlling interfacial tension is an effective method for manipulating the shape, position, and flow of fluids at sub-millimeter length scales, where interfacial tension is a dominant force. A variety of methods exist for controlling the interfacial tension of aqueous and organic liquids on this scale; however, these techniques have limited utility for liquid metals due to their large interfacial tension.
Liquid metals can form soft, stretchable, and shape-reconfigurable components in electronic and electromagnetic devices. Although it is possible to manipulate these fluids via mechanical methods (e.g., pumping), electrical methods are easier to miniaturize, control, and implement. However, most electrical techniques have their own constraints: electrowetting-on-dielectric requires large (kV) potentials for modest actuation, electrocapillarity can affect relatively small changes in the interfacial tension, and continuous electrowetting is limited to plugs of the liquid metal in capillaries.
Here, we present a method for actuating gallium and gallium-based liquid metal alloys via an electrochemical surface reaction. Controlling the electrochemical potential on the surface of the liquid metal in electrolyte rapidly and reversibly changes the interfacial tension by over two orders of magnitude ( &#820;500 mN/m to near zero). Furthermore, this method requires only a very modest potential (&#60; 1 V) applied relative to a counter electrode. The resulting change in tension is due primarily to the electrochemical deposition of a surface oxide layer, which acts as a surfactant; removal of the oxide increases the interfacial tension, and vice versa. This technique can be applied in a wide variety of electrolytes and is independent of the substrate on which it rests.

We present a method to control the interfacial energy of a liquid metal in an electrolyte via electrochemical deposition (or removal) of a surface oxide layer. This simple method can control the capillary behavior of gallium-based liquid metals by tuning the interfacial energy rapidly, significantly, and reversibly using modest voltages.

方法通过表面氧化还原操纵液态金属的表面张力

Controlling interfacial tension is an effective method for manipulating the shape, position, and flow of fluids at sub-millimeter length scales, where ...

Sulfate Separation by Selective Crystallization with a Bis-iminoguanidinium Ligand

A simple and effective method for selective sulfate separation from aqueous solutions by crystallization with a bis-guanidinium ligand, 1,4-benzene-bis(iminoguanidinium) (BBIG), is demonstrated. The ligand is synthesized as the chloride salt (BBIG-Cl) by in situ imine condensation of terephthalaldehyde with aminoguanidinium chloride in water, followed by crystallization as the sulfate salt (BBIG-SO4). Alternatively, BBIG-Cl is synthesized ex situ in larger scale from ethanol. The sulfate separation ability of the BBIG ligand is demonstrated by selective and quantitative crystallization of sulfate from seawater. The ligand can be recycled by neutralization of BBIG-SO4 with aqueous NaOH and crystallization of the neutral bis-iminoguanidine, which can be converted back into BBIG-Cl with aqueous HCl and reused in another separation cycle. Finally, 35S-labeled sulfate and &#946; liquid scintillation counting are employed for monitoring the sulfate concentration in solution. Overall, this protocol will instruct the user in the necessary skills to synthesize a ligand, employ it in the selective crystallization of sulfate from aqueous solutions, and quantify the separation efficiency.

A protocol for in situ aqueous synthesis of a bis(iminoguanidinium) ligand and its utilization in selective separation of sulfate is presented.

分离硫酸选择性结晶用双 -  iminoguanidinium配体

A simple and effective method for selective sulfate separation from aqueous solutions by crystallization with a bis-guanidinium ligand, ...

Facile Preparation of (2Z,4E)-Dienamides by the Olefination of Electron-deficient Alkenes with Allyl Acetate

Direct cross-coupling between two alkenes via vinylic C-H bond activation represents an efficient strategy for the synthesis of butadienes with high atomic and step economy. However, this functionality-directed cross-coupling reaction has not been developed, as there are still limited directing groups in practical use. In particular, a stoichiometric amount of oxidant is usually required, producing a large amount of waste. Due to our interest in novel 1,3-butadiene synthesis, we describe the ruthenium-catalyzed olefination of electron-deficient alkenes using allyl acetate and without external oxidant. The reaction of 2-phenyl acrylamide and allyl acetate was chosen as a model reaction, and the desired diene product was obtained in 80% isolated yield with good stereoselectivity (Z,E/Z,Z = 88:12) under optimal conditions: [Ru(p-cymene) Cl2]2 (3 mol %) and AgSbF6 (20 mol %) in DCE at 110 &#186;C for 16 h. With the optimized catalytic conditions in hand, representative &#945;- and/or &#946;-substituted acrylamides were investigated, and all reacted smoothly, regardless of aliphatic or aromatic groups. Also, differently N-substituted acrylamides have proven to be good substrates. Moreover, we examined the reactivity of different allyl derivatives, suggesting that the chelation of acetate oxygen to the metal is crucial for the catalytic process. Deuterium-labeled experiments were also conducted to investigate the reaction mechanism. Only Z-selective H/D exchanges on acrylamide were observed, indicating a reversible cyclometalation event. In addition, a kinetic isotope effect (KIE) of 3.2 was observed in the intermolecular isotopic study, suggesting that the olefinic C-H metalation step is probably involved in the rate-determining step.

Facile Preparation of 2Z,4E-Dienamides by the Olefination of Electron-deficient Alkenes with Allyl Acetate

The ruthenium-catalyzed olefination of electron-deficient alkenes with allyl acetate is described here. By using aminocarbonyl as a directing group, this external oxidant-free protocol has high efficiency and good stereo- and regioselectivity, opening a novel synthetic route to (Z,E)-butadiene skeletons.

（2<em&gt;ž</em&gt;，4<em&gt;电子</em&gt;） - 通过电子缺陷烯烃与烯丙基乙酸酯的烯化反应制备二烯酰胺

Direct cross-coupling between two alkenes via vinylic C-H bond activation represents an efficient strategy for the synthesis of butadienes with high ...

Phase Behavior of Charged Vesicles Under Symmetric and Asymmetric Solution Conditions Monitored with Fluorescence Microscopy

Phase-separated giant unilamellar vesicles (GUVs) exhibiting coexisting liquid-ordered and liquid-disordered domains are a common biophysical tool to investigate the lipid raft hypothesis. Numerous studies, however, neglect the impact of physiological solution conditions. On that account, the current work presents the effect of high-salinity buffer and trans-membrane solution asymmetry on liquid-liquid phase separation in charged GUVs grown from dioleylphosphatidylglycerol, egg sphingomyelin, and cholesterol. The effects were studied under isothermal and varying temperature conditions.
We describe equipment and experimental strategies applicable for monitoring the stability of coexisting liquid domains in charged vesicles under symmetric and asymmetric high-salinity solution conditions. This includes an approach to prepare charged multicomponent GUVs in high-salinity buffer at high temperatures. The protocol entails the option to perform a partial exchange of the external solution by a simple dilution step while minimizing the vesicle dilution. An alternative approach is presented utilizing a microfluidic device that allows for a complete external solution exchange. The solution effects on phase separation were also studied under varying temperatures. To this end, we present the basic design and utility of an in-house built temperature control chamber. Furthermore, we reflect on the assessment of the GUV phase state, pitfalls associated with it and how to circumvent them.

Experiments on phase separated giant unilamellar vesicles (GUVs) frequently neglect physiological solution conditions. This work presents approaches to study the effect of high-salinity buffer on liquid-liquid phase separation in charged multicomponent GUVs as a function of trans-membrane solution asymmetry and temperature.

用荧光显微镜监测对称和非对称溶液条件下带电泡的相行为

Phase-separated giant unilamellar vesicles (GUVs) exhibiting coexisting liquid-ordered and liquid-disordered domains are a common biophysical tool to ...

Imaging Corrosion at the Metal-Paint Interface Using Time-of-Flight Secondary Ion Mass Spectrometry

Corrosion developed at the paint and aluminum (Al) metal-paint interface of an aluminum alloy is analyzed using time-of-flight secondary ion mass spectrometry (ToF-SIMS), illustrating that SIMS is a suitable technique to study the chemical distribution at a metal-paint interface. The painted Al alloy coupons are immersed in a salt solution or exposed to air only. SIMS provides chemical mapping and 2D molecular imaging of the interface, allowing direct visualization of the morphology of the corrosion products formed at the metal-paint interface and mapping of the chemical after corrosion occurs. The experimental procedure of this method is presented to provide technical details to facilitate similar research and highlight pitfalls that may be encountered during such experiments.

Time-of-flight secondary ion mass spectrometry is applied to demonstrate the chemical mapping and corrosion morphology at the metal-paint interface of an aluminum alloy after being exposed to a salt solution compared with a specimen exposed to air.

利用飞行时二次离子质谱法成像金属颜料界面的腐蚀

Corrosion developed at the paint and aluminum (Al) metal-paint interface of an aluminum alloy is analyzed using time-of-flight secondary ion mass ...

Studying Surfactant Effects on Hydrate Crystallization at Oil-Water Interfaces Using a Low-Cost Integrated Modular Peltier Device

We introduce an approach to study the formation and growth of hydrates under the influence of nonionic surfactants. The experimental system includes a temperature regulator, visualization techniques, and inner pressure measurements. The temperature control system contains a low-cost, programmable temperature regulator made with solid-state Peltier components. Along with the temperature control system, we incorporated visualization techniques and internal pressure measurements to study hydrate formation and inhibition in the presence of nonionic surfactants. We studied the hydrate-inhibiting ability of nonionic surfactants (sorbitane monolaurate, sorbitane monooleate, PEG-PPG-PEG, and polyoxyethylenesorbitan tristearate) at low (i.e., 0.1 CMC), medium (i.e., CMC), and high (i.e., 10 CMC) concentrations. Two types of crystals were formed: planar and conical. Planar crystals were formed in plain water and low surfactant concentrations. Conical crystals were formed in high surfactant concentrations. The results of the study show that conical crystals are the most effective in terms of hydrate inhibition. Because conical crystals cannot grow past a certain size, the hydrate growth rate as a conical crystal is slower than the hydrate growth rate as planar crystal. Hence, surfactants that force hydrates to form conical crystals are the most efficient. The goal of the protocol is to provide a detailed description of an experimental system that is capable of investigating the cyclopentane hydrate crystallization process on the surface of a water droplet in the presence of surfactant molecules.

We present a protocol to study the formation of hydrates in the presence of nonionic surfactants on the interface of a water droplet submerged in cyclopentane. The protocol consists of building a low-cost, programmable, temperature regulator. The temperature control system is combined with visualization techniques and internal pressure measurements.

使用低成本集成模块化 Peltier 器件研究油水界面水合物结晶的超活性剂效应

We introduce an approach to study the formation and growth of hydrates under the influence of nonionic surfactants. The experimental system includes a ...

确定缓蚀剂/金属界面的化学成分与XPS:最小化后浸入氧化

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