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><tbody><tr><td>HiPco Single-walled carbon nanotubes</td><td>Unidym</td><td>P2771</td><td></td></tr><tr><td>Pluronic F127</td><td>BASF</td><td>9003-11-6</td><td>Mw = 12.6 kg/mol</td></tr><tr><td>5-methylsalicylic acid</td><td>TCI America</td><td>C0410</td><td></td></tr><tr><td>Ultrasonic processor</td><td>Cole-Parmer</td><td>ML-04714-52</td><td></td></tr><tr><td>Sorvall 6 plus centrifuge</td><td>Thermo Scientific</td><td>46910</td><td></td></tr><tr><td>Innova AFM</td><td>Bruker</td><td></td><td></td></tr><tr><td>Si-wafer</td><td>Silicon Quest International</td><td></td><td>150 mm in diameter; N type &amp;lt;1-1-1&gt; cut; 1-10&amp;nbsp;Ohm/cm; Single-side polyshed (675 &amp;#177; 25 &amp;#956;m); Diced (12&amp;nbsp;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

Universidad de Cartagena UDEC

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

Fabrication, Densification, and Replica Molding of 3D Carbon Nanotube Microstructures

The introduction of new materials and processes to microfabrication has, in large part, enabled many important advances in microsystems, lab-on-a-chip devices, and their applications. In particular, capabilities for cost-effective fabrication of polymer microstructures were transformed by the advent of soft lithography and other micromolding techniques 1, 2, and this led a revolution in applications of microfabrication to biomedical engineering and biology. Nevertheless, it remains challenging to fabricate microstructures with well-defined nanoscale surface textures, and to fabricate arbitrary 3D shapes at the micro-scale. Robustness of master molds and maintenance of shape integrity is especially important to achieve high fidelity replication of complex structures and preserving their nanoscale surface texture. The combination of hierarchical textures, and heterogeneous shapes, is a profound challenge to existing microfabrication methods that largely rely upon top-down etching using fixed mask templates. On the other hand, the bottom-up synthesis of nanostructures such as nanotubes and nanowires can offer new capabilities to microfabrication, in particular by taking advantage of the collective self-organization of nanostructures, and local control of their growth behavior with respect to microfabricated patterns. 
Our goal is to introduce vertically aligned carbon nanotubes (CNTs), which we refer to as CNT "forests", as a new microfabrication material. We present details of a suite of related methods recently developed by our group: fabrication of CNT forest microstructures by thermal CVD from lithographically patterned catalyst thin films; self-directed elastocapillary densification of CNT microstructures; and replica molding of polymer microstructures using CNT composite master molds. In particular, our work shows that self-directed capillary densification ("capillary forming"), which is performed by condensation of a solvent onto the substrate with CNT microstructures, significantly increases the packing density of CNTs. This process enables directed transformation of vertical CNT microstructures into straight, inclined, and twisted shapes, which have robust mechanical properties exceeding those of typical microfabrication polymers. This in turn enables formation of nanocomposite CNT master molds by capillary-driven infiltration of polymers. The replica structures exhibit the anisotropic nanoscale texture of the aligned CNTs, and can have walls with sub-micron thickness and aspect ratios exceeding 50:1. Integration of CNT microstructures in fabrication offers further opportunity to exploit the electrical and thermal properties of CNTs, and diverse capabilities for chemical and biochemical functionalization 3.

We present methods for fabrication of patterned microstructures of vertically aligned carbon nanotubes (CNTs), and their use as master molds for production of polymer microstructures with organized nanoscale surface texture. The CNT forests are densified by condensation of solvent onto the substrate, which significantly increases their packing density and enables self-directed formation of 3D shapes.

制备，致密，副本三维碳纳米管微结构成型

The introduction of new materials and processes to microfabrication has, in large part, enabled many important advances in microsystems, lab-on-a-chip ...

科研

工程学

Gyroid Nickel Nanostructures from Diblock Copolymer Supramolecules

Nanoporous metal foams possess a unique combination of properties - they are catalytically active, thermally and electrically conductive, and furthermore, have high porosity, high surface-to-volume and strength-to-weight ratio. Unfortunately, common approaches for preparation of metallic nanostructures render materials with highly disordered architecture, which might have an adverse effect on their mechanical properties. Block copolymers have the ability to self-assemble into ordered nanostructures and can be applied as templates for the preparation of well-ordered metal nanofoams. Here we describe the application of a block copolymer-based supramolecular complex - polystyrene-block-poly(4-vinylpyridine)(pentadecylphenol) PS-b-P4VP(PDP) - as a precursor for well-ordered nickel nanofoam. The supramolecular complexes exhibit a phase behavior similar to conventional block copolymers and can self-assemble into the bicontinuous gyroid morphology with two PS networks placed in a P4VP(PDP) matrix. PDP can be dissolved in ethanol leading to the formation of a porous structure that can be backfilled with metal. Using electroless plating technique, nickel can be inserted into the template&#39;s channels. Finally, the remaining polymer can be removed via pyrolysis from the polymer/inorganic nanohybrid resulting in nanoporous nickel foam with inverse gyroid morphology.

This article describes the preparation of well-ordered nickel nanofoams via electroless metal deposition onto nanoporous templates obtained from self-assembled diblock copolymer based supramolecules.

Gyroid镍纳米结构的嵌段共聚物超分子

Nanoporous metal foams possess a unique combination of properties - they are catalytically active, thermally and electrically conductive, and furthermore, ...

化学

Synthesis and Functionalization of Nitrogen-doped Carbon Nanotube Cups with Gold Nanoparticles as Cork Stoppers

Nitrogen-doped carbon nanotubes consist of many cup-shaped graphitic compartments termed as nitrogen-doped carbon nanotube cups (NCNCs). These as-synthesized graphitic nanocups from chemical vapor deposition (CVD) method were stacked in a head-to-tail fashion held only through noncovalent interactions. Individual NCNCs can be isolated out of their stacking structure through a series of chemical and physical separation processes. First, as-synthesized NCNCs were oxidized in a mixture of strong acids to introduce oxygen-containing defects on the graphitic walls. The oxidized NCNCs were then processed using high-intensity probe-tip sonication which effectively separated the stacked NCNCs into individual graphitic nanocups. Owing to their abundant oxygen and nitrogen surface functionalities, the resulted individual NCNCs are highly hydrophilic and can be effectively functionalized with gold nanoparticles (GNPs), which preferentially fit in the opening of the cups as cork stoppers. These graphitic nanocups corked with GNPs may find promising applications as nanoscale containers and drug carriers.

We discussed the synthesis of individual graphitic nanocups using a series of techniques including chemical vapor deposition, acid oxidation and probe-tip sonication. By citrate reduction of HAuCl4, the graphitic nanocups were effectively corked with gold nanoparticles due to the chemically reactive edges of the cups.

黄金纳米粒子作为软木塞氮掺杂碳纳米管杯的合成与功能构造

Nitrogen-doped carbon  nanotubes consist of many cup-shaped graphitic compartments termed as  nitrogen-doped carbon nanotube cups (NCNCs).  These ...

Using Polystyrene-block-poly(acrylic acid)-coated Metal Nanoparticles as Monomers for Their Homo- and Co-polymerization

We present a template-free method for &#8220;polymerizing&#8221; nanoparticles into long chains without side branches. A variety of nanoparticles are encapsulated in polystyrene-block-poly(acrylic acid) (PSPAA) shells and then used as monomers for their self-assembly. Spherical PSPAA micelles upon acid treatment are known to assemble into cylindrical micelles. Exploiting this tendency, the core-shell nanoparticles are induced to aggregate, coalesce, and then transform into long chains. When more than one type of nanoparticles are used, random and block &#8220;copolymers&#8221; of nanoparticles can be obtained. Detailed procedures are reported for the PSPAA encapsulation of nanoparticles, homo- and co-polymerization of the core-shell nanoparticles, separation and purification of the resulting nanoparticle chains. Transformations of single-line chains into double- and triple-line chains are also presented. The synergy between the polymer shell and the embedded nanoparticles leads to an unusual chain-growth polymerization mode, giving long nanoparticle chains that are distinct from the products of the traditional step-growth aggregation process.

Using Polystyrene-block-polyacrylic acid-coated Metal Nanoparticles as Monomers for Their Homo- and Co-polymerization

We report protocols for &#8220;polymerizing&#8221; various types of polymer-encapsulated metal nanoparticles into long chains of &#8220;homo-&#8220; and &#8220;co-polymers&#8221;.

使用聚苯乙烯<em&gt;块</em&gt; - 聚（丙烯酸）涂层的金属纳米颗粒作为单体他们均聚物和共聚物聚合

We present a template-free method for &#8220;polymerizing&#8221; nanoparticles into long chains without side branches. A variety of nanoparticles are ...

Preparation of Carbon Nanosheets at Room Temperature

Amphiphilic molecules equipped with a reactive, carbon-rich "oligoyne" segment consisting of conjugated carbon-carbon triple bonds self-assemble into defined aggregates in aqueous media and at the air-water interface. In the aggregated state, the oligoynes can then be carbonized under mild conditions while preserving the morphology and the embedded chemical functionalization. This novel approach provides direct access to functionalized carbon nanomaterials. In this article, we present a synthetic approach that allows us to prepare hexayne carboxylate amphiphiles as carbon-rich siblings of typical fatty acid esters through a series of repeated bromination and Negishi-type cross-coupling reactions. The obtained compounds are designed to self-assemble into monolayers at the air-water interface, and we show how this can be achieved in a Langmuir trough. Thus, compression of the molecules at the air-water interface triggers the film formation and leads to a densely packed layer of the molecules. The complete carbonization of the films at the air-water interface is then accomplished by cross-linking of the hexayne layer at room temperature, using UV irradiation as a mild external stimulus. The changes in the layer during this process can be monitored with the help of infrared reflection-absorption spectroscopy and Brewster angle microscopy. Moreover, a transfer of the carbonized films onto solid substrates by the Langmuir-Blodgett technique has enabled us to prove that they were carbon nanosheets with lateral dimensions on the order of centimeters.

We present the synthesis of an amphiphilic hexayne and its use in the preparation of carbon nanosheets at the air-water interface from a self-assembled monolayer of these reactive, carbon-rich molecular precursors.

碳纳米片在室温下准备

Amphiphilic molecules equipped with a reactive, carbon-rich "oligoyne" segment consisting of conjugated carbon-carbon triple bonds self-assemble into ...

Functionalization and Dispersion of Carbon Nanomaterials Using an Environmentally Friendly Ultrasonicated Ozonolysis Process

Functionalization of carbon nanomaterials is often a critical step that facilitates their integration into larger material systems and devices. In the as-received form, carbon nanomaterials, such as carbon nanotubes (CNTs) or graphene nanoplatelets (GNPs), may contain large agglomerates. Both agglomerates and impurities will diminish the benefits of the unique electrical and mechanical properties offered when CNTs or GNPs are incorporated into polymers or composite material systems. Whilst a variety of methods exist to functionalize carbon nanomaterials and to create stable dispersions, many the processes use harsh chemicals, organic solvents, or surfactants, which are environmentally unfriendly and may increase the processing burden when isolating the nanomaterials for subsequent use. The current research details the use of an alternative, environmentally friendly technique for functionalizing CNTs and GNPs. It produces stable, aqueous dispersions free of harmful chemicals. Both CNTs and GNPs can be added to water at concentrations up to 5 g/L and can be recirculated through a high-powered ultrasonic cell. The simultaneous injection of ozone into the cell progressively oxidizes the carbon nanomaterials, and the combined ultrasonication breaks down agglomerates and immediately exposes fresh material for functionalization. The prepared dispersions are ideally suited for the deposition of thin films onto solid substrates using electrophoretic deposition (EPD). CNTs and GNPs from the aqueous dispersions can be readily used to coat carbon- and glass-reinforcing fibers using EPD for the preparation of hierarchical composite materials.

Here, a novel method for the functionalization and stable dispersion of carbon nanomaterials in aqueous environments is described. Ozone is injected directly into an aqueous dispersion of carbon nanomaterial that is continuously recirculated through a high-powered ultrasonic cell.

碳纳米材料的功能化和分散使用环境友好的超声波臭氧分解过程

Functionalization of carbon nanomaterials is often a critical step that facilitates their integration into larger material systems and devices. In the ...

环境科学

Nanosponge Tunability in Size and Crosslinking Density

We describe a protocol for the synthesis of linear polyesters containing pendant epoxide functionality and their incorporation into a nanosponge with controlled dimensions. This approach begins with synthesis of a functionalized lactone which is key to the pendant functionalization of the resulting polymer. Valerolactone (VL) and allyl-valerolactone (AVL) are then copolymerized using ring-opening polymerization. Post-polymerization modification is then used to install an epoxide moiety on some or all of the pendant allyl groups. Epoxy-amine chemistry is employed to form nanoparticles in a dilute solution of both polymer and small molecule diamine crosslinker based on the desired nanosponge size and crosslinking density. Nanosponge sizes can be characterized by transmission electron microscopy (TEM) imaging to determine the dimension and distribution. This method provides a pathway by which highly tunable polyesters can create tunable nanoparticles, which can be used for small molecule drug encapsulation. Due to the nature of the backbone, these particles are hydrolytically and enzymatically degradable for a controlled release of a wide range of hydrophobic small molecules.

This article describes a process for tuning the size and crosslinking density of covalently crosslinked nanoparticles from linear polyesters containing pendant functionality. By tailoring synthesis parameters (polymer molecular weight, pendant functionality incorporation, and crosslinker equivalents), a desired nanoparticle size and crosslinking density can be achieved for drug delivery applications.

Nanosponge 可调大小和交联密度

We describe a protocol for the synthesis of linear polyesters containing pendant epoxide functionality and their incorporation into a nanosponge with ...

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 ...

Synthesis of Monodisperse Cylindrical Nanoparticles via Crystallization-driven Self-assembly of Biodegradable Block Copolymers

The production of monodisperse cylindrical micelles is a significant challenge in polymer chemistry. Most cylindrical constructs formed from diblock copolymers are produced by one of three techniques: thin film rehydration, solvent switching or polymerization-induced self-assembly, and produce only flexible, polydisperse cylinders. Crystallization-driven self-assembly (CDSA) is a method which can produce cylinders with these properties, by stabilizing structures of a lower curvature due to the formation of a crystalline core. However, the living polymerization techniques by which most core-forming blocks are formed are not trivial processes and the CDSA process may yield unsatisfactory results if carried out incorrectly. Here, the synthesis of cylindrical nanoparticles from simple reagents is shown. The drying and purification of reagents prior to a ring-opening polymerization of &#949;-caprolactone catalyzed by diphenyl phosphate is described. This polymer is then chain extended by methyl methacrylate (MMA) followed by N,N-dimethyl acrylamide (DMA) using reversible addition&#8722;fragmentation chain-transfer (RAFT) polymerization, affording a triblock copolymer that can undergo CDSA in ethanol. The living CDSA process is outlined, the results of which yield cylindrical nanoparticles up to 500 nm in length and a length dispersity as low as 1.05. It is anticipated that these protocols will allow others to produce cylindrical nanostructures and elevate the field of CDSA in the future.

Crystallization-driven self-assembly (CDSA) displays the unique ability to fabricate cylindrical nanostructures of narrow length distributions. The organocatalyzed ring-opening polymerization of &#949;-caprolactone and subsequent chain extensions of methyl methacrylate and N,N-dimethyl acrylamide are demonstrated. A living CDSA protocol that produces monodisperse cylinders up to 500 nm in length is outlined.

通过结晶驱动生物降解块共聚物的自组装合成单分散圆柱状纳米粒子

The production of monodisperse cylindrical micelles is a significant challenge in polymer chemistry. Most cylindrical constructs formed from diblock ...

Engineering Molecular Recognition with Bio-mimetic Polymers on Single Walled Carbon Nanotubes

Semiconducting single-wall carbon nanotubes (SWNTs) are a class of optically active nanomaterial that fluoresce in the near infrared, coinciding with the optical window where biological samples are most transparent. Here, we outline techniques to adsorb amphiphilic polymers and polynucleic acids onto the surface of SWNTs to engineer their corona phases and create novel molecular sensors for small molecules and proteins. These functionalized SWNT sensors are both biocompatible and stable. Polymers are adsorbed onto the nanotube surface either by direct sonication of SWNTs and polymer or by suspending SWNTs using a surfactant followed by dialysis with polymer. The fluorescence emission, stability, and response of these sensors to target analytes are confirmed using absorbance and near-infrared fluorescence spectroscopy. Furthermore, we demonstrate surface immobilization of the sensors onto glass slides to enable single-molecule fluorescence microscopy to characterize polymer adsorption and analyte binding kinetics.

We present a protocol for engineering the corona phase of near infrared fluorescent single walled carbon nanotubes (SWNTs) using amphiphilic polymers and DNA to develop sensors for molecular targets without known recognition elements.

工程分子识别与单壁碳纳米管仿生聚合物

Semiconducting single-wall carbon nanotubes (SWNTs) are a class of optically active nanomaterial that fluoresce in the near infrared, coinciding with the ...