The Research at Oak Ridge National Laboratory's Spallation Neutron Source and Center for Nanophase Materials Sciences was sponsored by the Scientific User Facilities Division, Office of Basic Energy Sciences, U.S. Department of Energy. The author, Zhe Zhang, gratefully acknowledges the financial support from J&#252;lich Center for Neutron Science, Research center J&#252;lich.

注:此协议需要特别注意的纳米材料的处理。如购买的单壁碳纳米管（SWNT）的细粉末的形式存在，因此，它们应在水溶液中分散之前被认为是纳米有害物质。请使用材料安全数据表（MSDS）中相应的安全设备。 1.泊洛沙姆407 / SWNT水悬浮液的制备注:在比使用的嵌段共聚物的临界胶束温度（CMT）更低的温度下所有的样品制备程序继续。在20℃，制备了泊洛沙姆407 / SWNT样品，泊洛沙姆407（30℃）的CMT的下方。21 <ol><li> 泊洛沙姆407水溶液的制备（0.25％w / w的） <ol><li>完全溶解0.175克泊洛沙姆407粉末与70克D 2 O的 注:D 2 O用于SANS测量。 70克D 2 O中为约63.2毫升室温。对于其他目的，H 2 O，建议使用。 </li></ol></li><li> 原油泊洛沙姆407 /单壁碳纳米管悬浮液的制备 <ol><li>添加0.01克SWNT粉两个50毫升锥形离心管（管1和管2）分开。 </li><li>加31.6毫升泊洛沙姆407溶液（1.1.1），进管1和31.6剩余溶液到管2的混合物中。 </li><li>通过涡旋混合5-10分钟混合悬浮液在管1和2。 </li><li>放置管1的水浴中。牢固地固定在管位置。 （ 图1）浸入该管，直到空气悬浮接口达到的水在浴表面上。 </li><li>浸超声发生器的尖端插入悬架管1的从0％渐渐增加超声功率，至少直到沉积在试管底部的单壁碳纳米管开始碎裂和扩频由于超声波传播˚F<html> ROM中的超声波发生器一角。治疗用超声波的悬浮液60分钟，在20℃，同时保持悬浮液温度低于25℃。 注意:不要把尖端更深超过1厘米进入暂停。保持低于25℃的悬浮液的温度，无论是通过控制水储存器的温度，或通过适当地重新填充浴。 </li><li>重复步骤管2 1.2.4和1.2.5。 </li></ol></li><li> 泊洛沙姆407 / SWNT悬浮液在5甲基水杨酸的不存在和存在准备 <ol><li>离心机在管1的粗混悬液和2在9800×g下2小时在20℃。 </li><li>移动15毫升从每个管的上清液到新的管中，单独地。 </li><li>溶解0.015克5-甲基水杨酸（5MS）插入从管2取上清液，并标记该混合物作为样品＃2。从管1与样品＃1标记的另一上清液。 </li></ol></li></ol>E"&gt; 2。扩展Q-范围内小角度中子散射（EQ-SANS）测量注意:要在散裂中子源（SNS）的光束线的工作，需要一个公认的beamtime建议。辐射安全培训等仪器具体培训也需要提前。由SNS用户办事处提供接入和培训内容，并可以在neutrons.ornl.gov找到。 <ol><li> 样品装载 <ol><li>的样品＃1负载0.3毫升成无定形石英班卓琴细胞和样品＃2到另一个班卓琴细胞（ 图2A-1）。戴上两个单元眼睑和周围的盖子安全包装胶带密封。 </li><li>放置间隔件之间的密封细胞（ 图2A-ii）用于铝池支架（ 图2A-ⅲ）中的一个，并组装铝班卓琴单元保持体（ 图2B）。组装其他细胞与以相同的方式不同的一组班卓琴单元保持的。 </li><li>加载组装细胞进入EQ-SANS样品桨（ 图3A）的不同样本位置。使该桨叶的样本位置的列表。 </li></ol></li><li> 测量 <ol><li>设置配置为在与仪器的科学家的帮助下一个脚本SANS的测量，指的是给定的示例脚本。 注:在简短的评论的补充材料中提供的实际SANS测量中使用的脚本的例子。本实施例是专为使用9.1埃&lt;λ&lt;在固定1.3米样品到检测器的距离为10毫米的样本孔径13.2埃的波长频带中的两个样品（样品＃1和＃2）的SANS测量而设计30毫米梁停止。示例脚本可以在不为＃1试样和＃2的任何修改地使用。 <ol><li>以覆盖0.01的q范围- 0.4埃- 1，选择9.1埃&lt;的波长带λ&lt;13.2埃，由如图所示的示例脚本输入1300到检测器的位置和9成波长的样品到检测器的距离为1.3微米。 </li><li>要使用10毫米口径的样品和30毫米波束停止，设定在脚本中梁停止，孔XY位置。 </li><li>设置发射和样品散射测量的样品位置和对应的名称。 </li><li>对应束流时间的文件夹中保存脚本。 </li></ol></li><li>执行通过点击"运行脚本&#39;上PyDAS控制窗口（ 图3B）的右侧和加载保存的脚本执行测量该脚本。 </li><li>在实验结束后通知测量的完成的文书团队。 </li></ol></li></ol> 3. SANS数据简化与分析<ol><li> SANS数据还原过程 <ol><li>对所测量的数据的还原使用在analysis.sns.gov提供MantidPlot 23-24软件，与仪器团队的帮助。 注:可以在网页analysis.sns.gov中找到运行MantidPlot软件的详细说明。 </li><li>在MantidPlot，从打开的界面菜单EQSANS还原界面。 （接口&gt; SANS&gt; ORNL SANS）。输入数据还原过程的所有必要信息。 注意:大多数的数据还原过程中的重要信息是由仪表组提供。有关信息，在补充材料，还提供相关的截图。 </li><li> 输入在"还原选项"标签的所有必要信息。 <ol><li>输入从标准样品测量的绝对比例因子。从充分表征的标准样品的测定，其散射强度是已知的获得绝对强度（I（0）= 450nm厘米3 - 1），适合与德拜-丁酰胆碱酯酶，散射型。 </LI&gt; <li>输入的暗电流的文件名，它是由仪器团队提供。 </li><li>检查"立体角校正&#39;，&#39;Q分辨率"，"使用配置文件&#39;，&#39;正确TOF&#39;，和&#39;从配置文件作为适用的用户掩模&#39;选项。 </li><li>设置样品孔直径10毫米。设置数量为Q箱200与线性Q分级方案。输入掩模文件名，其也由仪器团队提供。 </li></ol></li><li> 输入所有必要的信息来完成"检测"选项卡。 <ol><li>选中"使用寻束器&#39;（相契合直射光束选项​​）和"执行灵敏度校正"。查找使用空波束测量的运行数量的梁中心"数据文件"。 </li><li>输入的灵敏度数据的文件名，它是由仪器科学家提供。允许的灵敏度范围分别设定为0.5和2.5的最小和最大。检查＆＃39;使用样品光束中心"。 </li></ol></li><li> 输入"数据"选项卡上的所有必要信息。 <ol><li>在"散射数据文件&#39;输入样品散射运行次数。指定厘米样品厚度。选择"计算传输"。 </li><li>在"样品直接束数据文件&#39;输入样品传输运行次数。在&#39;空直射数据文件"中输入空束运行次数。 </li><li>检查"背景数据文件"，然后输入背景散射运行次数。选择"计算传输"。在"样品直接束数据文件"中输入后台传输运行次数。 注意:在这种情况下，空的班卓琴细胞散射数据文件的背景散射。 </li><li>在&#39;空直射数据文件"中输入空束运行次数。通常情况下，这个数字是一样的空束运行次数（3.1.5.2）。 </li></ol></li><li>点击"减少"执行数据还原。 注意:输出被写入所指定的文件夹中##### _ Iq.txt哪里#####是样品散射文件的运行次数。 ASCII格式用于数据文件。 </li></ol></li><li> 模型拟合分析 注:SasView是一个小角散射分析软件包，它最初是作为NSF DANSE项目的一部分，目前正在由设施的国际合作（http://www.sasview.org/）管理。软件包可以在http://sourceforge.net/projects/sasview/files/下载。 <ol><li>运行SasView，并通过点击"加载数据"从"数据资源管理器"窗口中加载数据文件。 </li><li>点击"发送到"用&#39;配件&#39;选项，并检查弹出窗口上的数据图。 </li><li>在"飞度面板"，选择下的模型类别"形状"，并从模型下拉框选择"CoreShellCylinderModel"。 </li> &lt;LI&gt;调整参数值，所以模型曲线是接近尽可能数据曲线。 注:使用SLD（散射长度密度）计算器从工具菜单来计算散射长度密度。 </li><li>选择拟合面板"使用唐吉诃德数据"和"使用的dI数据"。调整为拟合数据的Q系列，。点击&#39;飞度&#39;来执行数据拟合。 </li></ol></li></ol> 4.实时太空观测用原子力显微镜（AFM） <ol><li> 使用旋涂硅晶片样品制备 <ol><li>对于AFM测定，取从样品＃1（1.3.3）0.1毫升样品溶液中，它为1.9毫升去离子水混合。 </li><li>放置在旋涂机清洁Si晶片（12毫米×12毫米）。固定用真空卡盘的晶片的位置。 </li><li>分别设定的旋转速度，并以每分钟（rpm）1500转和60秒的运行时间。湿的晶片的露出的表面稀释样品。开始旋涂。 </li><li>关掉真空泵，并从旋涂器取出涂覆的晶片。 </li></ol></li><li> AFM测量 <ol><li>使用双面粘合碳胶带的铁盘上附上旋涂晶片（4.1.4）。 </li><li>使样品盘（4.2.1）更靠近扫描仪的曝光区域的边缘的第一，和盘朝向中心滑动，直到盘的底表面完全覆盖扫描器的顶部。 注意:避免突然接触，因为在扫描仪的顶磁铁强烈吸引铁盘。轻轻使磁盘和扫描仪的两个边缘之间的接触。 </li><li>安装在扫描仪的扫描探针显微镜（SPM）的头，插上数据线。 注:特别关注的同时，移动SPM头或对接（删除）到（离）扫描器支付。当磁头从扫描器阶段分离，保持头部朝向u​​pwa的底面RDS所有的时间。 </li><li>运行该工具提供的控制软件，并选择"系统配置"窗口中的窃听方式。 </li><li>通过调整光学显微镜的粗，细旋钮和通过移动的x和y光级放置在显示屏窗口的中心的悬臂刀片。 </li><li>通过调整对SPM头的激光准直旋钮调整激光。定位红色激光点的悬臂大致，并通过跟踪在显示屏所示的点移动至点到悬臂刀片的中间。 注意:当激光正确对齐，粉红色的反射光斑出现的激光对准窗口。 </li><li>通过在激光对准窗口的中心定位粉红反射图像对齐检测器。调整于SPM头的光检测器旋钮直到象限光电二极管（QPD）信号之和大于2 V至少（2.1 - 2.4 V）。 </li><li>调入调悬臂使用无线自动调谐悬臂ndow。 1000千赫 - 在0的频率范围内运行的自动调谐。 </li><li>通过调整焦点旋钮使晶片表面进入显微镜的焦点。 </li><li>慢慢地推动悬臂尖端倾向于使用在"电机平台"窗口中的向上和向下箭头晶片表面。停止运动的前端接触到样品表面之前。 注意:作为前端接近晶片，尖端的模糊黑图像显示在监视器和当尖端和晶片表面进行接触的图像变得清晰。不要让尖端物理接触标本。它破坏样品和仪器。停止尖端示出的暗的模糊图像时。 </li><li>点击工具栏上的按钮搞。 </li><li>选择扫描尺寸（5-10微米），采样数（512-1,024），并在弹出的窗口的扫描速度（0.5〜0.6赫兹），以首先获取大规模的形象。 </li><li>开始扫描。逐渐调整P（比例增益），I（积分增益），和D（垂直德屈曲）值如果颗粒和基板背景之间的对比度太低而不能认清颗粒形状和边界从扫描的图像。 注意:当进入一个新的PID值设定，扫描过程中会自动重新启动。 </li><li>如果存在的大规模图像中的感兴趣的任何区域，重新运行与一组适当的扫描尺寸的扫描，X偏移量，Y轴偏移量，和样本号。 </li><li>测量完成后脱开探头。 注:提高探针头以防止在悬臂针尖与样品的任何损害。首先拆下探头，然后取下样品盘。 </li></ol></li></ol>

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S., Kim, T. H., Kline, S. R., Choi, S. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Thermally+switchable+one-and+two-dimensional+arrays+of+single-walled+carbon+nanotubes+in+a+polymeric+system.">Thermally switchable one-and two-dimensional arrays of single-walled carbon nanotubes in a polymeric system.</a> J Am Chem Soc. 131 (45), 16568-16572 (2009).</li><li>Doe, C., Jang, H. S., Kline, S. R., Choi, S. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=SANS+Investigation+of+Selectively+Distributed+Single-Walled+Carbon+Nanotubes+in+a+Polymeric+Lamellar+Phase.">SANS Investigation of Selectively Distributed Single-Walled Carbon Nanotubes in a Polymeric Lamellar Phase.</a> Macromolecules. 43 (12), 5411-5416 (2010).</li><li>Han, Y., Ahn, S. K., Zhang, Z., Smith, G. S., Do, C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Tunable+Encapsulation+Structure+of+Block+Copolymer+Coated+Single-Walled+Carbon+Nanotubes+in+Aqueous+Solution.">Tunable Encapsulation Structure of Block Copolymer Coated Single-Walled Carbon Nanotubes in Aqueous Solution.</a> Macromolecules. 48 (11), 3475-3480 (2015).</li><li>Kim, T. H., Han, Y. S., Jang, J. D., Seong, B. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=SANS+study+on+self-assembled+structures+of+Pluronic+F127+triblock+copolymer+induced+by+additives+and+temperature.">SANS study on self-assembled structures of Pluronic F127 triblock copolymer induced by additives and temperature.</a> J Appl Cryst. 47 (1), 53-59 (2013).</li><li>Arnold, O., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Mantid-Data+analysis+and+visualization+package+for+neutron+scattering+and+&#181;+SR+experiments.">Mantid-Data analysis and visualization package for neutron scattering and &#181; SR experiments.</a> Nucl Instrum Meth A. 764 (1), 156-166 (2014).</li><li>Alvarez, R., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Mantid+3.4:+Manipulation+and+Analysis+Toolkit+for+Instrument+Data.">Mantid 3.4: Manipulation and Analysis Toolkit for Instrument Data.</a> Mantid Project. , (2015).</li><li>Nagarajan, R., Bradley, R. A., Nair, B. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Thermodynamically+stable,+size+selective+solubilization+of+carbon+nanotubes+in+aqueous+solutions+of+amphiphilic+block+copolymers.">Thermodynamically stable, size selective solubilization of carbon nanotubes in aqueous solutions of amphiphilic block copolymers.</a> J Chem Phys. 131 (10), 104906 (2009).</li><li>Nikolaev, P., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Gas-phase+catalytic+growth+of+single-walled+carbon+nanotubes+from+carbon+monoxide.">Gas-phase catalytic growth of single-walled carbon nanotubes from carbon monoxide.</a> Chem. Phys Lett. 313 (1), 91-97 (1999).</li></ol>

The authors have nothing to disclose.

SANS和AFM测量表明，单壁碳纳米管已成功解捆绑并单独使用泊洛沙姆407三嵌段共聚物分散在水溶液中。在此样品的制备方法，超声波处理并离心过程是确定最终悬浮液的特征的关键步骤。的单壁碳纳米管间的强相互作用，这迫使未涂覆的SWNT在溶液中捆绑在一起，必须克服与嵌段共聚物稳定的各个单壁碳纳米管。提供足够的能量，适当长的时间使聚合物克服能垒，并成功地稳定了单壁碳纳米管。然?...

碳纳米管（CNT）是通过轧制微米级石墨片成纳米管形成的中空圆筒状的纳米颗粒。因为他们的非凡的机械，热和电性能的，碳纳米管已经被广泛1-3调查作为一个新的候选用于治疗和生物传感应用，以及在自组装的纳米复合材料的纳米填料官能纳米粒子。然而，它们的溶解性差并有志于做出常用的有机和水性溶剂束强烈的偏好阻碍生物应用方便，环保的处理以及进步。因此，各种官能化的方法，例如超声处理，表面化学改性，并通过使用表面活性剂和嵌段共聚物的非共价官能化，4-9已经开发来修改在CNT表面和提高其分散性在广泛的溶剂。非共价泛函基于物理的表面处理补肾中药方法，特别是，被认为是一个有希望的和健壮的策略，因为在固有的CNT特性的任何表面改性诱导抑制可以最小化。10迄今为止，已经有不少努力提高分散效率的通过采用各种类型的分散剂，包括基本的表面活性剂（ 如，SDS CTAB，NaDDBS），7,11两亲嵌段共聚物，8生物材料（ 如 DNA），12,13和合成的官能聚合物的非共价官能化的方法（ 例如 ，共轭聚合物，芳族聚合物）。14,15 PEO-PPO-PEO聚合物，一种由两个亲水聚（环氧乙烷）的三嵌段共聚物（PEO）在两条链末端共价结合到一个疏水聚（环氧丙烷）在中心处（PPO）链，可以延长电势非共价键的官能化碳纳米管的应用我2N水溶液。这些聚合物提供接口，这不仅是为了在CNT表面，但也向水介质和其它聚合物基质并且表现出巨大的生物相容性友好由于PEO链的毒性最小。这在一个宽的范围内分散的环境中，以及在生物医学应用的聚合物涂覆的CNT的利用率便于更容易处理。12,16-17此外，这些聚合物的基于其对外部刺激敏感反应的富热力学相行为使在其中内和粒子间结构可以可逆地和精确地控制智能嵌段共聚物的CNT混合纳米结构的制造。18-21在这里，我们提出了一个协议，用于基于CNT的混合纳米粒子具有的可调谐封装层的制造PEO105-PPO70-PEO105（泊洛沙姆407）。所得到的结构的特征在于通过小角中子散射（SANS）。这项工作预计将introducË智能功能构建块的概念，并帮助非专业人士轻松地准备嵌段共聚物功能化的碳纳米管悬浮液和使​​用SANS在橡树岭国家实验室的详细特征。

<table border="0" cellpadding="0" cellspacing="0" width="634">
	<tbody>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">HiPco Single-walled carbon nanotubes</td>
			<td style="width:71px;">Unidym</td>
			<td style="width:119px;">P2771</td>
			<td style="width:228px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Pluronic F127</td>
			<td style="width:71px;">BASF</td>
			<td>9003-11-6</td>
			<td>Mw = 12.6 kg/mol</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">5-methylsalicylic acid</td>
			<td style="width:71px;">TCI America</td>
			<td>C0410</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Ultrasonic processor</td>
			<td style="width:71px;">Cole-Parmer</td>
			<td>ML-04714-52</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Sorvall 6 plus centrifuge</td>
			<td style="width:71px;">Thermo Scientific</td>
			<td align="right" style="width:119px;">46910</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Innova AFM&#160;</td>
			<td style="width:71px;">Bruker</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="89">
			<td height="89" style="height:89px;width:216px;">Si-wafer</td>
			<td style="width:71px;">Silicon Quest International</td>
			<td style="width:119px;"></td>
			<td style="width:228px;">150 mm in diameter&#160; ; N type &#60;1-1-1&#62; cut ; 1-10 Ohm/cm ; Single-side polyshed (675 +- 25 um) ; Diced (12 mm x 12 mm)</td>
		</tr>
	</tbody>
</table>

functionalization of single-walled carbon nanotubes with thermo-reversible block copolymers and characterization by small-angle neutron scattering

We demonstrate a protocol for single-walled carbon nanotube functionalization using thermo-sensitive PEO-PPO-PEO triblock copolymers in an aqueous solution. In a carbon nanotube/PEO105-PPO70-PEO105 (poloxamer 407) aqueous solution, the amphiphilic poloxamer 407 adsorbs onto the carbon nanotube surfaces and self-assembles into continuous layers, driven by intermolecular interactions between constituent molecules. The addition of 5-methylsalicylic acid changes the self-assembled structure from spherical-micellar to a cylindrical morphology. The fabricated poloxamer 407/carbon nanotube hybrid particles exhibit thermo-responsive structural features so that the density and thickness of poloxamer 407 layers are also reversibly controllable by varying temperature. The detailed structural properties of the poloxamer 407/carbon nanotube particles in suspension can be characterized by small-angle neutron scattering experiments and model fit analyses. The distinct curve shapes of the scattering intensities depending on temperature control or addition of aromatic additives are well described by a modified core-shell cylinder model consisting of a carbon nanotube core cylinder, a hydrophobic shell, and a hydrated polymer layer. This method can provide a simple but efficient way for the fabrication and in-situ characterization of carbon nanotube-based nano particles with a structure-tunable encapsulation.

泊洛沙姆407涂覆的SWNT纳米棒悬浮液用样品制备过程（ 图4），其可分为两个重要工艺制造;关于使用超超声，以及使用离心捆绑聚集单独稳定的单壁碳纳米管的分馏工艺单壁碳纳米管表面泊洛沙姆407的物理吸附过程。 对于所制备的泊洛沙姆407 / SWNT / D得到SANS的散射强度2 O样品的温度范围内的5MS的在不存在（...

Watch this Scientific Journal Video about Functionalization of Single-walled Carbon Nanotubes with Thermo-reversible Block Copolymers and Characterization by Small-angle Neutron Scattering at JoVE.com

Functionalization of Single-walled Carbon Nanotubes with Thermo-reversible Block Copolymers and Characterization by Small-angle Neutron Scattering

A method for the functionalization of carbon nanotubes with structure-tunable polymeric encapsulation layers and structural characterization using small-angle neutron scattering is presented.

单壁碳纳米管与热可逆嵌段共聚物及表征功能化小角度中子散射

We demonstrate a protocol for single-walled carbon nanotube functionalization using thermo-sensitive PEO-PPO-PEO triblock copolymers in an aqueous ...

functionalization-single-walled-carbon-nanotubes-with-thermo

Research

JoVE Journal

Chemistry

9.1K 次观看.  Oak Ridge National Laboratory. A method for the functionalization of carbon nanotubes with structure-tunable polymeric encapsulation layers and structural characterization using small-angle neutron scattering is presented.

视频: Functionalization of Single-walled Carbon Nanotubes with Thermo-reversible Block Copolymers and Characterization by Small-angle Neutron Scattering

Template Directed Synthesis of Plasmonic Gold Nanotubes with Tunable IR Absorbance

A nearly parallel array of pores can be produced by anodizing aluminum foils in acidic environments1, 2. Applications of anodic aluminum oxide (AAO) membranes have been under development since the 1990's and have become a common method to template the synthesis of high aspect ratio nanostructures, mostly by electrochemical growth or pore-wetting. Recently, these membranes have become commercially available in a wide range of pore sizes and densities, leading to an extensive library of functional nanostructures being synthesized from AAO membranes. These include composite nanorods, nanowires and nanotubes made of metals, inorganic materials or polymers 3-10. Nanoporous membranes have been used to synthesize nanoparticle and nanotube arrays that perform well as refractive index sensors, plasmonic biosensors, or surface enhanced Raman spectroscopy (SERS) substrates 11-16, as well as a wide range of other fields such as photo-thermal heating 17, permselective transport 18, 19, catalysis 20, microfluidics 21, and electrochemical sensing 22, 23. Here, we report a novel procedure to prepare gold nanotubes in AAO membranes. Hollow nanostructures have potential application in plasmonic and SERS sensing, and we anticipate these gold nanotubes will allow for high sensitivity and strong plasmon signals, arising from decreased material dampening 15.

Solution-suspendable gold nanotubes with controlled dimensions can be synthesized by electrochemical deposition in porous anodic aluminum oxide (AAO) membranes using a hydrophobic polymer core. Gold nanotubes and nanotube arrays hold promise for applications in plasmonic biosensing, surface-enhanced Raman spectroscopy, photo-thermal heating, ionic and molecular transport, microfluidics, catalysis and electrochemical sensing.

的模板导演电浆黄金纳米管的合成与可调谐红外吸收

A nearly parallel array of pores can be produced by anodizing aluminum foils in acidic environments1, 2. Applications of anodic aluminum oxide (AAO) ...

科研

化学

Transport of Surface-modified Carbon Nanotubes through a Soil Column

Carbon nanotubes (CNTs) are widely manufactured nanoparticles, which are being utilized in a number of consumer products, such as sporting goods, electronics and biomedical applications. Due to their accelerating production and use, CNTs constitute a potential environmental risk if they are released to soil and groundwater systems. It is therefore essential to improve the current understanding of environmental fate and transport of CNTs. The transport and retention of CNTs in both natural and artificial media have been reported in literature, but the findings widely vary and are thus not conclusive. There are a number of physical and chemical parameters responsible for variation in retention and transport. In this study, a complete procedure of selected multiwalled carbon nanotubes (MWCNTs) is presented starting from their surface modification to a complete set of laboratory column experiments at critical physical and chemical scenarios. Results indicate that the stability of the commercially available MWCNTs are critical with their attached surface functional group which can also influence the transport and retention of MWCNT through the surrounding medium.

Surface properties of a nanoparticle are important for their interaction with the surrounding medium. Therefore the surface modification of carbon nanotubes can be critical for their transport and retention through porous media. Here, lab scale column experiments are used to understand the possible transport and retention of these nanoparticles.

表面修饰碳纳米管通过土柱运输

Carbon nanotubes (CNTs) are widely manufactured nanoparticles, which are being utilized in a number of consumer products, such as sporting goods, ...

Synthesis, Characterization, and Functionalization of Hybrid Au/CdS and Au/ZnS Core/Shell Nanoparticles

Plasmonic nanoparticles are an attractive material for light harvesting applications due to their easily modified surface, high surface area and large extinction coefficients which can be tuned across the visible spectrum. Research into the plasmonic enhancement of optical transitions has become popular, due to the possibility of altering and in some cases improving photo-absorption or emission properties of nearby chromophores such as molecular dyes or quantum dots. The electric field of the plasmon can couple with the excitation dipole of a chromophore, perturbing the electronic states involved in the transition and leading to increased absorption and emission rates. These enhancements can also be negated at close distances by energy transfer mechanism, making the spatial arrangement of the two species critical. Ultimately, enhancement of light harvesting efficiency in plasmonic solar cells could lead to thinner and, therefore, lower cost devices. The development of hybrid core/shell particles could offer a solution to this issue. The addition of a dielectric spacer between a gold nanoparticles and a chromophore is the proposed method to control the exciton plasmon coupling strength and thereby balance losses with the plasmonic gains. A detailed procedure for the coating of gold nanoparticles with CdS and ZnS semiconductor shells is presented. The nanoparticles show high uniformity with size control in both the core gold particles and shell species allowing for a more accurate investigation into the plasmonic enhancement of external chromophores.

The synthesis of uniform gold nanoparticles coated with semiconductor shells of CdS or ZnS is performed. The semiconductor coating is conducted by first depositing a silver sulfide shell and exchanging the silver cations for zinc or cadmium cations.

合成，表征和混合金/硫化镉和Au / ZnS核/壳纳米颗粒功能化

Plasmonic nanoparticles are an attractive material for light harvesting applications due to their easily modified surface, high surface area and large ...

Facile Preparation of Internally Self-assembled Lipid Particles Stabilized by Carbon Nanotubes

We present a facile method to prepare nanostructured lipid particles stabilized by carbon nanotubes (CNTs). Single-walled (pristine) and multi-walled (functionalized) CNTs are used as stabilizers to produce Pickering type oil-in-water (O/W) emulsions. Lipids namely, Dimodan U and Phytantriol are used as emulsifiers, which in excess water self-assemble into the bicontinuous cubic Pn3m phase. This highly viscous phase is fragmented into smaller particles using a probe ultrasonicator in presence of conventional surfactant stabilizers or CNTs as done here. Initially, the CNTs (powder form) are dispersed in water followed by further ultrasonication with the molten lipid to form the final emulsion. During this process the CNTs get coated with lipid molecules, which in turn are presumed to surround the lipid droplets to form a particulate emulsion that is stable for months. The average size of CNT-stabilized nanostructured lipid particles is in the submicron range, which compares well with the particles stabilized using conventional surfactants. Small angle X-ray scattering data confirms the retention of the original Pn3m cubic phase in the CNT-stabilized lipid dispersions as compared to the pure lipid phase (bulk state). Blue shift and lowering of the intensities in characteristic G and G&#39; bands of CNTs observed in Raman spectroscopy characterize the interaction between CNT surface and lipid molecules. These results suggest that the interactions between the CNTs and lipids are responsible for their mutual stabilization in aqueous solutions. As the concentrations of CNTs employed for stabilization are very low and lipid molecules are able to functionalize the CNTs, the toxicity of CNTs is expected to be insignificant while their biocompatibility is greatly enhanced. Hence the present approach finds a great potential in various biomedical applications, for instance, for developing hybrid nanocarrier systems for the delivery of multiple functional molecules as in combination therapy or polytherapy.

We report on a smart application of carbon nanotubes for kinetic stabilization of lipid particles that contain self-assembled nanostructures in their cores. The preparation of lipid particles requires rather low concentrations of carbon nanotubes permitting their use in biomedical applications such as drug delivery.

内部自组装脂质颗粒的简易制备碳纳米管稳定

We present a facile method to prepare nanostructured lipid particles stabilized by carbon nanotubes (CNTs). Single-walled (pristine) and multi-walled ...

Characterization, Quantification and Compound-specific Isotopic Analysis of Pyrogenic Carbon Using Benzene Polycarboxylic Acids (BPCA)

Fire-derived, pyrogenic carbon (PyC), sometimes called black carbon (BC), is the carbonaceous solid residue of biomass and fossil fuel combustion, such as char and soot. PyC is ubiquitous in the environment due to its long persistence, and its abundance might even increase with the projected increase in global wildfire activity and the continued burning of fossil fuel. PyC is also increasingly produced from the industrial pyrolysis of organic wastes, which yields charred soil amendments (biochar). Moreover, the emergence of nanotechnology may also result in the release of PyC-like compounds to the environment. It is thus a high priority to reliably detect, characterize and quantify these charred materials in order to investigate their environmental properties and to understand their role in the carbon cycle.
Here, we present the benzene polycarboxylic acid (BPCA) method, which allows the simultaneous assessment of PyC&#39;s characteristics, quantity and isotopic composition (13C and 14C) on a molecular level. The method is applicable to a very wide range of environmental sample materials and detects PyC over a broad range of the combustion continuum, i.e., it is sensitive to slightly charred biomass as well as high temperature chars and soot. The BPCA protocol presented here is simple to employ, highly reproducible, as well as easily extendable and modifiable to specific requirements. It thus provides a versatile tool for the investigation of PyC in various disciplines, ranging from archeology and environmental forensics to biochar and carbon cycling research.

Characterization, Quantification and Compound-specific Isotopic Analysis of Pyrogenic Carbon Using Benzene Polycarboxylic Acids BPCA

We present the benzene polycarboxylic acid (BPCA) method for assessing pyrogenic carbon (PyC) in the environment. The compound-specific approach uniquely provides simultaneous information about the characteristics, quantity and isotopic composition (13C and 14C) of PyC.

表征，气相炭用苯聚羧酸的定量和特定化合物同位素分析（BPCA）

Fire-derived, pyrogenic carbon (PyC), sometimes called black carbon (BC), is the carbonaceous solid residue of biomass and fossil fuel combustion, such as ...

Synthesis and Characterization of Fe-doped Aluminosilicate Nanotubes with Enhanced Electron Conductive Properties

The goal of the protocol is to synthesize Fe-doped aluminosilicate nanotubes of the imogolite type with the formula (OH)3Al2-xFexO3SiOH. Doping with Fe aims at lowering the band gap of imogolite, an insulator with the chemical formula (OH)3Al2O3SiOH, and at modifying its adsorption properties towards azo-dyes, an important class of organic pollutants of both wastewater and groundwater.
Fe-doped nanotubes are obtained in two ways: by direct synthesis, where FeCl3 is added to an aqueous mixture of the Si and Al precursors, and by post-synthesis loading, where preformed nanotubes are put in contact with a FeCl3&#8226;6H2O aqueous solution. In both synthesis methods, isomorphic substitution of Al3+ by Fe3+ occurs, preserving the nanotube structure. Isomorphic substitution is indeed limited to a mass fraction of ~1.0% Fe, since at a higher Fe content (i.e., a mass fraction of 1.4% Fe), Fe2O3 clusters form, especially when the loading procedure is adopted. The physicochemical properties of the materials are studied by means of X-ray powder diffraction (XRD), N2 sorption isotherms at -196 &#176;C, high resolution transmission electron microscopy (HRTEM), diffuse reflectance (DR) UV-Vis spectroscopy, and &#950;-potential measurements. The most relevant result is the possibility to replace Al3+ ions (located on the outer surface of the nanotubes) by post-synthesis loading on preformed imogolite without perturbing the delicate hydrolysis equilibria occurring during nanotube formation. During the loading procedure, an anionic exchange occurs, where Al3+ ions on the outer surface of the nanotubes are replaced by Fe3+ ions. In Fe-doped aluminosilicate nanotubes, isomorphic substitution of Al3+ by Fe3+ is found to affect the band gap of doped imogolite. Nonetheless, Fe3+ sites on the outer surface of nanotubes are able to coordinate organic moieties, like the azo-dye Acid Orange 7, through a ligand-displacement mechanism occurring in an aqueous solution.

Here, we present a protocol to synthesize and characterize Fe-doped aluminosilicate nanotubes. The materials are obtained by either sol-gel synthesis upon addition of FeCl3&#8226;6H2O to the mixture containing the Si and Al precursors or by post-synthesis ionic exchange of preformed aluminosilicate nanotubes.

以增强电子导电性能的合成与表征Fe掺杂碳纳米管硅铝的

The goal of the protocol is to synthesize Fe-doped aluminosilicate nanotubes of the imogolite type with the formula (OH)3Al2-xFexO3SiOH. Doping with Fe ...

Monitoring the Effects of Illumination on the Structure of Conjugated Polymer Gels Using Neutron Scattering

We demonstrate a protocol to effectively monitor the gelation process of a high concentration solution of conjugated polymer both in the presence and absence of white light exposure. By instituting a controlled temperature ramp, the gelation of these materials can be precisely monitored as they proceed through this structural evolution, which effectively mirrors the conditions experienced during the solution deposition phase of organic electronic device fabrication. Using small angle neutron scattering (SANS) and ultra-small angle neutron scattering (USANS) along with appropriate fitting protocols we quantify the evolution of select structural parameters throughout this process. Thorough analysis indicates that continued light exposure throughout the gelation process significantly alters the structure of the ultimately formed gel. Specifically, the aggregation process of poly(3-hexylthiophene-2,5-diyl) (P3HT) nano-scale aggregates is negatively affected by the presence of illumination, ultimately resulting in the retardation of growth in conjugated polymer microstructures and the formation of smaller scale macro-aggregate clusters.

A protocol for the analysis of gels formed from the optoelectronic conjugated polymer poly(3-hexylthiophene-2,5-diyl) (P3HT) using small and ultra-small angle neutron scattering in both the presence and absence of illumination is presented.

利用中子散射监测光照对共轭高分子凝胶结构的影响

We demonstrate a protocol to effectively monitor the gelation process of a high concentration solution of conjugated polymer both in the presence and ...

Grafting Multiwalled Carbon Nanotubes with Polystyrene to Enable Self-Assembly and Anisotropic Patchiness

We demonstrate a straightforward protocol to graft pristine multiwalled carbon nanotubes (MWCNTs) with polystyrene (PS) chains at the sidewalls through a free-radical polymerization strategy to enable the modulation of the nanotube surface properties and produce supramolecular self-assembly of the nanostructures. First, a selective hydroxylation of the pristine nanotubes through a biphasic catalytically mediated oxidation reaction creates superficially distributed reactive sites at the sidewalls. The latter reactive sites are subsequently modified with methacrylic moieties using a silylated methacrylic precursor to create polymerizable sites. Those polymerizable groups can address further polymerization of styrene to produce a hybrid nanomaterial containing PS chains grafted to the nanotube sidewalls. The polymer-graft content, amount of silylated methacrylic moieties introduced and hydroxylation modification of the nanotubes are identified and quantified by Thermogravimetric Analysis (TGA). The presence of reactive functional groups hydroxyl and silylated methacrylate are confirmed by Fourier Transform Infrared Spectroscopy (FT-IR). Polystyrene-grafted carbon nanotube solutions in tetrahydrofuran (THF) provide wall-to-wall collinearly self-assembled nanotubes when cast samples are analyzed by transmission electron microscopy (TEM). Those self-assemblies are not obtained when suitable blanks are similarly cast from analogous solutions containing non-grafted counterparts. Therefore, this method enables the modification of the nanotube anisotropic patchiness at the sidewalls which results into spontaneous auto-organization at the nanoscale.

A procedure for the synthesis of polystyrene-grafted multiwalled carbon nanotubes using successive chemical modification steps to selectively introduce the polymer chains to the sidewalls and their self-assembly via anisotropic patchiness is presented.

用聚苯乙烯接枝多壁纳米碳纳米管使自组装和各向异性斑块

We demonstrate a straightforward protocol to graft pristine multiwalled carbon nanotubes (MWCNTs) with polystyrene (PS) chains at the sidewalls through a ...

Time-resolved Photophysical Characterization of Triplet-harvesting Organic Compounds at an Oxygen-free Environment Using an iCCD Camera

Here, we present a sensible method of the acquisition and analysis of time-resolved photoluminescence using an ultrafast iCCD camera. This system enables the acquisition of photoluminescence spectra covering the time regime from nanoseconds up to 0.1 s. This enables us to follow the changes in the intensity (decay) and emission of the spectra over time. Using this method, it is possible to study diverse photophysical phenomena, such as the emission of phosphorescence, and the contributions of prompt and delayed fluorescence in molecules showing thermally activated delayed fluorescence (TADF). Remarkably, all spectra and decays are obtained in a single experiment. This can be done for solids (thin film, powder, crystal) and liquid samples, where the only limitations are the spectral sensitivity of the camera and the excitation wavelength (532 nm, 355 nm, 337 nm, and 266 nm). This technique is, thus, very important when investigating the excited state dynamics in organic emitters for their application in organic light-emitting diodes and other areas where triplet harvesting is of paramount importance. Since triplet states are strongly quenched by oxygen, emitters with efficient TADF luminescence, or those showing room temperature phosphorescence (RTP), must be correctly prepared in order to remove any dissolved oxygen from solutions and films. Otherwise, no long-lived emission will be observed. The method of degassing solid samples as presented in this work is basic and simple, but the degassing of liquid samples creates additional difficulties and is particularly interesting. A method of minimizing solvent loss and changing the sample concentration, while still enabling to remove oxygen in a very efficient and a repeatable manner, is presented in this work.

Here, we present a method of the spectroscopic characterization of organic molecules by means of time-resolved photoluminescence spectroscopy on the nanosecond-to-millisecond timescale in oxygen-free conditions. Methods to efficiently remove oxygen from the samples and, thus, limit luminescence quenching are also described.

利用 iccd 摄像机对无氧环境下的三重收集有机化合物进行光物理表征

Here, we present a sensible method of the acquisition and analysis of time-resolved photoluminescence using an ultrafast iCCD camera. This system enables ...

DNA-magnetic Particle Binding Analysis by Dynamic and Electrophoretic Light Scattering

Isolation of DNA using magnetic particles is a field of high importance in biotechnology and molecular biology research. This protocol describes the evaluation of DNA-magnetic particles binding via dynamic light scattering (DLS) and electrophoretic light scattering (ELS). Analysis by DLS provides valuable information on the physicochemical properties of particles including particle size, polydispersity, and zeta potential. The latter describes the surface charge of the particle which plays major role in electrostatic binding of materials such as DNA. Here, a comparative analysis exploits three chemical modifications of nanoparticles and microparticles and their effects on DNA binding and elution. Chemical modifications by branched polyethylenimine, tetraethyl orthosilicate and (3-aminopropyl)triethoxysilane are investigated. Since DNA exhibits a negative charge, it is expected that zeta potential of particle surface will decrease upon binding of DNA. Forming of clusters should also affect particle size. In order to investigate the efficiency of these particles in isolation and elution of DNA, the particles are mixed with DNA in low pH (~6), high ionic strength and dehydration environment. Particles are washed on magnet and then DNA is eluted by Tris-HCl buffer (pH = 8). DNA copy number is estimated using quantitative polymerase chain reaction (PCR). Zeta potential, particle size, polydispersity and quantitative PCR data are evaluated and compared. DLS is an insightful and supporting method of analysis that adds a new perspective to the process of screening of particles for DNA isolation.

This protocol describes the synthesis of magnetic particles and evaluation of their DNA-binding properties via dynamic and electrophoretic light scattering. This method focuses on monitoring changes in particle size, their polydispersity and zeta potential of particle surface which play major role in binding of materials such as DNA.

动态和电泳光散射的 DNA-磁性颗粒结合分析

Isolation of DNA using magnetic particles is a field of high importance in biotechnology and molecular biology research. This protocol describes the ...