我们要感谢墨西哥国立自治大学的 PAIP 和 DGAPA-PAPIIT 项目 (赠款5000-9158、5000-9156、IA205616 和 IA205316) 和国家科学技术委员会从墨西哥-CONACYT-(赠款编号251533)。

警告: 使用前请查阅所有相关的材料安全数据表 (MSDS)。本议定书中使用的几种化学品具有剧毒和致癌性。与其他传统的散装碳同素异形体相比, 碳纳米管衍生物可能有额外的呼吸危险。据怀疑, 气溶胶中的碳纳米管对肺部的影响可能与石棉类似, 但至今尚未完全阐明其致癌性质。在执行化学反应和产品处理步骤时, 请使用所有适当的安全做法, 包括使用油烟机和个人防护设备 (实验室大衣、手套、安全眼镜、封闭式鞋、全长长裤), 同时适用过滤面罩呼吸器应特别使用时, 可能产生的潜在的纳米管粉尘 (NIOSH 批准 N95 模型, 或欧洲 EN 149 认证 FFP3 版本)。以下过程的部分涉及标准的惰性大气处理技术。24
1. 多壁纳米碳纳米管选择性羟基化的研究22
<ol><li>双向催化介导的 MWCNTs 氧化反应
	<ol>
<li>
有机相的制备
		<ol>
<li>将2.5 克的原始 MWCNTs 添加到手表玻璃、培养皿或烧杯中。</li>
			<li>将容器移动到80摄氏度真空烤箱中, 用合适的手表玻璃盖住。打开烤箱的真空泵, 将系统设置为ca 200 mmHg。</li>
			<li>在真空烤箱中把纳米管干燥12小时。在此步骤之后, MWCNTs 中的含水量将被消除。</li>
			<li>将干燥的 MWCNTs 倒入一个100毫升的圆底烧瓶, 用一个玻璃漏斗和一把铲子, 然后把漏斗取出。</li>
			<li>在圆底烧瓶中引入磁性搅拌棒, 用烧杯将50毫升99% 二氯甲烷添加到烧瓶中。用搅拌板搅拌60转, 直到团聚消失。</li>
			<li>如果在搅拌10分钟后, 团聚保持在溶液中, 将烧瓶移动到超声波浴中, 并打开系统5分钟. 如有必要, 重复超声波。该溶液将是氧化反应阶段的有机相。</li>
		</ol>
</li>
		<li>
水相的制备
		<ol>
<li>在25毫升烧杯中, 使用磁性搅拌棒和搅拌板, 在5毫升蒸馏水中溶解0.6 克铵溴 (TPABr)。</li>
			<li>在10毫升容积烧瓶中, 在蒸馏水 (0.16 米溶液) 中溶解0.253 克 KMnO4 , 并将溶液保存在手上的烧杯中。此解决方案将在步骤1.1.2.4 中使用。</li>
			<li>取5毫升的冰川醋酸 (HOAc), 将体积降为 TPABr 溶液。使用一个毕业的吸管和不断搅拌在冰浴可能是有益的。 注: 混合物过程是放热的, 因此, 增加应该慢慢地执行, 以避免可能的损伤由投射的水滴或过度变暖。</li>
			<li>将0.16 米 KMnO4水溶液的5毫升整除转移到酸化 TPABr 溶液中。使用干净的毕业吸管和搅拌可能会有帮助。</li>
			<li>保持以前的解决方案覆盖的手表玻璃, 直到需要。该溶液将是氧化反应阶段的水相。</li>
		</ol>
</li>
		<li>
氧化反应
		<ol>
<li>将水相倒入含有有机相的圆底烧瓶中。这种混合物将是两相反应混合物。</li>
			<li>使用搅拌板, 以 80 rpm 或更多的双相系统搅拌, 使混合料在室温下搅拌24小时。经过这段时间后, 紫水相变淡粉红色, 纳米管变成羟基 (MWCNT-OH)。</li>
		</ol>
</li>
	</ol></li>
	<li>MWCNT 的纯化-OH
	<ol>
<li>
液-液萃取
		<ol>
<li>将两相反应混合物转化为150毫升或200毫升部位漏斗, 旋塞阀在闭合位置。如果需要, 可以使用玻璃漏斗和刮刀。</li>
			<li>使用毕罗吸管, 一个巴斯德吸管与橡胶灯泡连接或烧杯, 添加〜0.25 毫升浓缩盐酸到部位漏斗。</li>
			<li>使用部位漏斗。<ol>
<li>关闭部位漏斗与聚四氟乙烯塞子 (不要使用玻璃塞子为碳纳米管), 并大力鼓动 5 s 在一个通风罩与窗扇窗口向下。在搅拌过程中, 要用一只手紧紧地握住漏斗, 用另一手抓住旋塞阀。</li>
				<li>搅拌一步后, 立即将漏斗翻转, 并通过各自的手打开旋塞阀释放压力积聚。 注意: 一定要解决的压力方向的通风食品的后方。</li>
				<li>重复最后两个搅拌/压力释放步骤的周期为 3-5。</li>
				<li>一旦最后一个周期完成, 立即删除塞子和离开漏斗夹紧和不受干扰, 直到相分离是明显的。液-液分离后, 水相保持在有机相的上方。MWCNT-OH 将保持在有机阶段。</li>
			</ol>
</li>
			<li>如果不发生相分离, 将 1-5 毫升盐水 (水中的 10-20% 氯化钠) 添加到部位漏斗上, 使用毕罗吸管或巴斯德吸管, 轻轻混合, 使混合物不受干扰, 直到相分离。重复, 直到需要。</li>
			<li>在150毫升烧杯上恢复有机相, 保持旋塞阀打开, 直到相边界到达旋塞阀位置。150毫升锥形瓶可交替用于恢复有机相;然而, 从这种容器类型中提取纳米管通常更为困难。</li>
			<li>将已恢复的解决方案与监视玻璃保持保护, 直到过滤。</li>
			<li>适当地丢弃水相。</li>
		</ol>
</li>
		<li>
真空过滤系统的设置
		<ol>
<li>设置真空过滤系统, 阀塞和底座牢固地固定在夹紧的北瓶的颈部。</li>
			<li>保持47毫米直径的膜过滤器在手边, 并根据膜材料和制造商的指示, 可选择地遵循这一步骤和未来两个 (步骤 1.2.2.2-1.2.2.4)。准备一个100毫米直径培养皿与乙醇 (乙醇) 灌装50% 的容量。</li>
			<li>用平滑尖端钳, 将47毫米直径的膜过滤器放置在培养皿上, 乙醇。将膜留在乙醇中 2-5 分钟. 确保使用具有孔隙大小 0.45-20 µm 的膜. 较小的孔径会堵塞过滤, 而较大的则会降低过滤效率。</li>
			<li>使用平滑尖端钳从乙醇中取出膜。</li>
			<li>将膜放在过滤支承表面的烧结玻璃区域上, 从膜的边缘开始。与乙醇的可选润湿可以促进这一步骤。</li>
			<li>将漏斗的法兰放在组件顶部的中间。请勿打扰膜。将漏斗和底座与弹簧钳锁在一起。</li>
			<li>将系统连接到真空源。在需要的时候不要打开真空。</li>
		</ol>
</li>
		<li>
过滤 MWCNT-哦
		<ol>
<li>将回收的有机相倒入玻璃棒辅助的真空过滤漏斗中。应用真空过滤样品直到干燥。</li>
			<li>使用洗涤瓶清洗固体与 40-50 毫升95% 甲醇 (甲醇)。使用玻璃棒可能有助于这项工作。重复此过程至少5次。在此步骤中保持真空。</li>
			<li>清洗后, 将系统置于真空状态下, 用玻璃表覆盖20分钟以烘干固体。</li>
			<li>为了从膜中恢复固体, 请按照下一步 1.2.3.5 1.2.3.8。</li>
			<li>小心, 取下弹簧钳, 然后垂直移除漏斗, 不干扰膜和固体。</li>
			<li>非常小心, 去除膜与固体从过滤器支持表面帮助下铲和光滑尖端钳。</li>
			<li>将膜与固体转移到一个直径为100毫米的培养皿或手表玻璃上。</li>
			<li>辅以两个平滑尖端钳和铲, 从膜表面恢复固体, 直到所有的产品都存放在培养皿/手表玻璃。</li>
		</ol>
</li>
		<li>
MWCNT 的干燥与贮存-哦
		<ol>
<li>覆盖培养皿/手表玻璃与一个合适的手表玻璃 (更大的直径是必需的)。 注: 请勿使用密封膜, 避免静电充电。</li>
			<li>将培养皿/手表玻璃引入加热在80摄氏度的真空烤箱中。打开烤箱的真空泵, 将系统设置为ca 200 毫米汞。</li>
			<li>将固体干燥24小时。在此步骤后, 产品中的溶剂含量将被淘汰。如果不立即使用该产品, 请将该实体存储在干燥中, 直到需要为止。</li>
		</ol>
</li>
	</ol></li>
</ol>2. 接枝 MWCNT-OH 与聚苯乙烯链22,23
<ol><li>
硅烷化甲基丙烯酸基团改性 MWCNT-OH 的研究
	<ol>
<li>用玻璃漏斗和刮刀将2.5 克 MWCNT 和5克的氢醌倒入干净的100毫升 Schlenk 瓶中, 取下漏斗, 引入磁性搅拌棒。</li>
		<li>根据以下指示将 Schlenk 瓶设置为回流模式:<ol>
<li>将 Schlenk 烧瓶连接到真空/惰性气体歧管系统, 使用连接到烧瓶玻璃接头的合适的橡胶管。把瓶子的歧管闭上。</li>
			<li>使用合适的橡胶管将合适的冷凝器连接到自来水系统, 确保通过靠近男性接头的玻璃接头设置水的收入。</li>
			<li>润滑的冷凝器的男性接头与均匀应用的细层真空润滑脂。 注: 接头不应过度润滑以避免产品污染。</li>
			<li>将冷凝器的雄性接头连接到 Schlenk 烧瓶的颈部。用橡胶塞子关闭冷凝器的母接头。</li>
			<li>小心, 打开瓶子到真空。确保在这个过程中, 纳米管不会被吸进真空线。</li>
			<li>用 N2气体填充 Schlenk 烧瓶。</li>
			<li>重复最后两个步骤两次。</li>
			<li>将系统保持在正 N2气体流量之下。</li>
		</ol>
</li>
		<li>辅以干净的套管和适当的注射器, 慢慢地通过橡胶塞子注入50毫升干甲苯。</li>
		<li>使用搅拌板和热浴, 搅拌在 80 rpm 或更多的混合物, 并使混合物在室温下搅拌 5-10 分钟。</li>
		<li>使用干净的套管和注射器, 通过橡胶塞子注入5毫升的 TMSPMA。</li>
		<li>将温度设置为100摄氏度, 并使反应在回流和搅拌12小时。在此之后, 硅烷化甲基丙烯酸基团是化学上的一对羟基组在 MWCNTs (即 MWCNT O TMSPMA)。</li>
		<li>一旦反应结束, 小心地卸下橡胶塞子, 关闭 N2流, 等待, 直到瓶在室温下。</li>
		<li>设置真空过滤系统 (步骤 1.2.2)。</li>
		<li>筛选实心 (步骤 1.2.3)。用甲醇洗。</li>
		<li>干燥并储存 MWCNT TMSPMA (步骤 1.2.4)。</li>
	</ol>
</li>
	<li>
改性 MWCNTs 苯乙烯的聚合研究
	<ol>
<li>将2.5 克的 MWCNT TMSPMA 和75毫克的 azobisisobutyronitrile (AIBN) 倒入一个干净的100毫升 Schlenk 瓶使用玻璃漏斗和铲, 并删除漏斗。 注意: AIBN 粉末不应暴露于热或强氧化剂, 因为它可能自发爆炸。</li>
		<li>在 Schlenk 瓶中引入磁性搅拌棒。</li>
		<li>将 Schlenk 瓶设置为回流模式 (步骤 2.1.2)。</li>
		<li>使用干净的套管和注射器, 通过橡胶塞子注入50毫升干甲苯。</li>
		<li>使用搅拌板和热浴, 搅拌在 80 rpm 或更多的混合物, 并使混合物在室温下搅拌 5-10 分钟。</li>
		<li>辅以干净的套管和注射器, 通过塞子注入7.5 毫升苯乙烯。</li>
		<li>将温度设置为70摄氏度, 并在反流、搅拌和 N2中保持 12 h 的反应。此后, PS 链被接上纳米管壁 (MWCNT-ps)。</li>
		<li>将系统打开到空气中, 关闭 N2流, 并将烧瓶冷却到室温。</li>
		<li>设置真空过滤系统 (步骤 1.2.2)。</li>
		<li>过滤和洗涤固体 (步骤 1.2.3)。在洗涤步骤中使用丙酮代替甲醇。用20毫升 THF 清洗固体五倍, 去除未结聚苯乙烯。</li>
		<li>干燥并贮存 MWCNT (步 1.2.4)。 注: 在聚合过程中, 通过改变甲苯中苯乙烯的浓度, 可以调节接枝纳米管的聚合物链的长度;低浓度产生短链。聚合反应时间可用于调整高分子链的尺寸;缩短了反应时间, 缩短了链条的长度。有关详细信息, 请参阅参考资料22和23。</li>
	</ol>
</li>
</ol>

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M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Perspectives+in+Chemistry+-+Steps+towards+Complex+Matter.">Perspectives in Chemistry - Steps towards Complex Matter.</a> Angew. Chem. Int. Ed. 52, 2836-2850 (2013).</li><li>Mattia, E., Otto, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Supramolecular+Systems+Chemistry.">Supramolecular Systems Chemistry.</a> Nat. Nanotechnol. 10, 111-119 (2015).</li><li>Leh, J. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Supramolecular Chemistry: Concepts and Perspectives. , (1995).</li><li>Esc&#225;rcega-Bobadilla, M. V., 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=Nanorings+and+Rods+Interconnected+by+Self-Assembly+Mimicking+an+Artificial+Network+of+Neurons.">Nanorings and Rods Interconnected by Self-Assembly Mimicking an Artificial Network of Neurons.</a> Nat. Commun. 4, 2648 (2013).</li><li>Gegenhuber, T., 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=Noncovalent+Grafting+of+Carbon+Nanotubes+with+Triblock+Terpolymers:+Toward+Patchy+1D+Hybrids.">Noncovalent Grafting of Carbon Nanotubes with Triblock Terpolymers: Toward Patchy 1D Hybrids.</a> Macromolecules. 48, 1767-1776 (2015).</li><li>Peng, H., Alemany, L. B., Margrave, J. L., Khabashesku, V. N. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Sidewall+Carboxylic+Acid+Functionalization+of+Single-Walled+Carbon+Nanotubes.">Sidewall Carboxylic Acid Functionalization of Single-Walled Carbon Nanotubes.</a> J. Am. Chem. Soc. 125, 15174-15182 (2003).</li><li>Furtado, C. A., Kim, U. J., Gutierrez, H. R., Pan, L., Dickey, E. C., Ecklund, P. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Debundling+and+Dissolution+of+Single-Walled+Carbon+Nanotubes+in+Amide+Solvents.">Debundling and Dissolution of Single-Walled Carbon Nanotubes in Amide Solvents.</a> J. Am. Chem. Soc. 126, 6095-6105 (2004).</li><li>Jeon, J. H., Lim, J. H., Kim, K. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Fabrication+of+Hybrid+Nanocomposites+with+Polystyrene+and+Multiwalled+Carbon+Nanotubes+with+Well-Defined+Polystyrene+via+Multiple+Atom+Transfer+Radical+Polymerization.">Fabrication of Hybrid Nanocomposites with Polystyrene and Multiwalled Carbon Nanotubes with Well-Defined Polystyrene via Multiple Atom Transfer Radical Polymerization.</a> Polymer. 50, 4488-4495 (2009).</li><li>Kim, M., Hong, C. K., Choe, S., Shim, S. E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+of+Polystyrene+Brush+on+Multiwalled+Carbon+Nanotubes+Treated+with+KMnO4+in+the+Presence+of+a+Phase-Transfer+Catalyst.">Synthesis of Polystyrene Brush on Multiwalled Carbon Nanotubes Treated with KMnO4 in the Presence of a Phase-Transfer Catalyst.</a> J. Polym. Sci. Pol. Chem. 45, 4413-4420 (2007).</li><li>Oliveira, E. Y. S., Bode, R., Esc&#225;rcega-Bobadilla, M. V., Zelada-Guill&#233;n, G. A., Maier, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Polymer+Nanocomposites+from+Self-Assembled+Polystyrene-Grafted+Carbon+Nanotubes.">Polymer Nanocomposites from Self-Assembled Polystyrene-Grafted Carbon Nanotubes.</a> New J. Chem. 40, 4625-4634 (2016).</li><li>Shriver, D. F., Drezdzon, M. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> The Manipulation of Air-Sensitive Compounds. , (1986).</li><li>Bressy, C., Ngo, V. 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作者没有什么可透露的。

在这种方法中, 有一些步骤对保证嫁接过程的成功至关重要。首先, 采用两相催化介导的氧化反应 (步骤 1.1), 用最近分散的碳纳米管 (步骤 1.1.1.5) 进行。如果色散结果难以为继根据协议中的建议, 使用超声波尖端 sonicator 将有助于如果使用相同的迹象 (步骤 1.1.1.6)。使用较短的 MWCNTs 也可能有助于解决色散问题。其次, 真空过滤系统的设置是净化效率的关键 (步骤 1.2.2)。从这个意义上说, 在过滤器支撑...

自发现单壁碳纳米管 (SWCNTs)、1、2以来, 科学界已将其优异的电气、机械和热性能应用于各种尖端的3 。应用程序通过调制其表面属性通过共价键4和非共价键5策略。这些应用程序的例子包括: 传感器中的传感器、6、7在太阳能电池中的电极、8在催化中的异构支持、9 nanoreactors 合成、10防污在保护膜中的代理,11复合材料中的填料,12等。然而, 调整其更健壮, 但在工业上可用的多壁纳米对应物的表面性质的可能性, 即 MWCNTs, 以控制其在纳米尺度上的非共价键相互作用的方向性, 仍然是一个困难的任务到目前为止。13
分子积木的超分子自组装是控制纳米尺度物质组织的最通用的策略之一。14,15在这种意义上, 超分子相互作用涉及定向、短程和中距离非共价键相互作用, 如 H 键、范德华、偶极子、离子偶极、偶极子诱导偶极、ππ叠加、阳离子π、负离子π、库仑、等。16不幸的是, 像 MWCNTs 这样的大型结构自组装的方向性不是自发的, 通常需要外部动力 (例如模板或耗能系统)。17最近的一份报告使用了非共价键包装的纳米管与量身定做的共同聚合物来追求后者的目标,18但使用共价键战略提供新的替代办法来解决这个问题还没有得到探讨。
碳纳米管的化学修饰可以有选择地进行, 以引入不同的功能组到总站或壁。19,20在碳纳米结构中调整表面性能最有用的方法之一是通过标准聚合路线进行高分子接枝。通常, 这些方法包括对聚合或启动器组 (丙烯酸、乙烯基、等) 的初步介绍. 纳米结构表面及其与合适单体的连续聚合。21在 MWCNTs 的情况下, 壁中的聚合物链的共价引入以各向异性的方式控制其斑块仍然是一个挑战。
在这里, 我们将展示如何一系列直接的化学修改步骤22,23可以应用于插入 PS 链上的壁 MWCNTs, 以修改其表面斑块和促进其各向异性在纳米尺度上的自组装23 。在修改路线, 第一步允许选择性羟基化的原始 MWCNTs 在壁通过遵循双向催化介导的氧化反应, 以产生羟基对应, MWCNT-哦。第二步使用 3-(trimethoxysilyl) 甲基丙烯酸丙酯 (TMSPMA), 向先前产生的羟基 (MWCNT O TMSPMA) 引入硅烷化甲基丙烯酸基团。当苯乙烯单体从甲基丙烯酸酯基团聚合, 从而产生接枝到纳米管壁的聚合物链 (即MWCNT-PS) 时, 这些刀片将提供表面活性点。

<table><tbody><tr><td>Tetrapropylammonium bromide, 99 % (TPABr)</td><td>Sigma-Aldrich</td><td>88104</td><td>Irritant, toxic</td></tr><tr><td>Potassium permanganate, 99 % (KMnO&lt;sub&gt;4&lt;/sub&gt;)</td><td>Sigma-Aldrich</td><td>223468</td><td></td></tr><tr><td>Acetic acid, 99.5 %</td><td>Sigma-Aldrich</td><td>45726</td><td></td></tr><tr><td>Pristine multiwalled carbon nanotubes, 99 % (MWCNTs)</td><td>Bayer Technology Services</td><td>Donated sample</td><td>Harmful dusts. &gt;1 micrometer in length and 13&amp;ndash;16 nm in outer diameter. Alternative supplier: Nanocyl, Catalog N. NC7000, website: http://www.nanocyl.com/</td></tr><tr><td>Sodium Chloride, 98 % (NaCl)</td><td>Sigma-Aldrich</td><td>S3014</td><td>Technical grade can also be used</td></tr><tr><td>Ethanol, 99.8 % (EtOH)</td><td>Sigma-Aldrich</td><td>32221</td><td>Technical grade can also be used</td></tr><tr><td>Methanol, 99.8 % (MeOH)</td><td>Sigma-Aldrich</td><td>322415</td><td>Highly toxic. Technical grade can also be used</td></tr><tr><td>Hydroquinone, 99 %</td><td>Sigma-Aldrich</td><td>H9003</td><td></td></tr><tr><td>Toluene, 99.8 %</td><td>Sigma-Aldrich</td><td>244511</td><td>Anhydrous</td></tr><tr><td>3-(Trimethoxysilyl)propyl methacrylate, 98 % (TMSPMA)</td><td>Sigma-Aldrich</td><td>440159</td><td>Air sensitive, toxic</td></tr><tr><td>Azobisisobutyronitrile, 99 % (AIBN)</td><td>Sigma-Aldrich</td><td>755745</td><td>Explosive</td></tr><tr><td>Styrene, 99 %</td><td>Sigma-Aldrich</td><td>S4972</td><td>Purified using an alumina gel preparative column and stored at 4 &amp;deg;C</td></tr><tr><td>Acetone, 99.5 %</td><td>Sigma-Aldrich</td><td>179124</td><td>Technical grade can also be used</td></tr><tr><td>Tetrahydrofuran, 99.9 % (THF)</td><td>Sigma-Aldrich</td><td>494461</td><td></td></tr><tr><td>Dichloromethane, 99.5 %</td><td>Sigma-Aldrich</td><td>443484</td><td>Highly toxic</td></tr><tr><td>Hydrochloric acid, 37 %</td><td>Sigma-Aldrich</td><td>435570</td><td>Harmful fumes</td></tr></tbody></table>

grafting multiwalled carbon nanotubes with polystyrene to enable self-assembly and anisotropic patchiness

我们展示了一个直接的协议, 以移植原始的多壁纳米碳纳米管 (MWCNTs) 与聚苯乙烯 (PS) 链在壁通过自由基聚合战略, 以使纳米管表面性能的调制和生产纳米结构的超分子自组装。首先, 通过双相催化介导的氧化反应, 对原始纳米管进行选择性羟基化, 在壁产生表面分布的活性点。后反应站点随后用甲基丙烯酸基团改性, 使用硅烷化甲基丙烯酸前驱体创建聚合点。这些聚合组可以解决苯乙烯的进一步聚合, 以产生含有 PS 链的混合纳米材料, 接枝到纳米管壁。通过热重分析, 确定了聚合物接枝的含量、硅烷化甲基丙烯酸基团的用量以及纳米管的羟基化改性。用傅里叶变换红外光谱 (IR) 证实了活性官能团羟基和硅烷化甲基丙烯酸酯的存在。用透射电镜分析了铸造样品时, 在四氢呋喃 (THF) 中的聚苯乙烯接枝碳纳米管溶液提供了壁壁 collinearly 自组装纳米管。当适当的空白类似于含有非接枝对应的类似溶液时, 就无法获得这些自组装。因此, 该方法能够在壁上对纳米管各向异性斑块进行修正, 从而使其在纳米尺度上产生自发的自动组织。

从原始的纳米管、羟基纳米管、用硅烷化甲基丙烯酸基团和聚苯乙烯接枝纳米管改性的纳米管(图 1) 中收集了 TGA 数据。通过硅烷化甲基丙烯酸基团(图 2) 修饰的羟基纳米管和纳米管收集红外光谱结果。TEM 图像是从原始的纳米管和聚苯乙烯接枝纳米管收集的 (图 3)。在质量上的 TGA 下降用于计算纳米管化学?...

Watch this Scientific Journal Video about Grafting Multiwalled Carbon Nanotubes with Polystyrene to Enable Self-Assembly and Anisotropic Patchiness at JoVE.com

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

采用连续化学改性的方法合成聚苯乙烯接枝多壁纳米碳纳米管, 选择性地将聚合物链引入壁及其自组装通过各向异性斑块是提出.

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 ...

grafting-multiwalled-carbon-nanotubes-with-polystyrene-to-enable-self

Universidad San Sebastian

Research

JoVE Journal

Chemistry

8.0K 次观看.  National Autonomous University of Mexico. 采用连续化学改性的方法合成聚苯乙烯接枝多壁纳米碳纳米管, 选择性地将聚合物链引入壁及其自组装通过各向异性斑块是提出.

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

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

Manufacturing of Three-dimensionally Microstructured Nanocomposites through Microfluidic Infiltration

Microstructured composite beams reinforced with complex three-dimensionally (3D) patterned nanocomposite microfilaments are fabricated via nanocomposite in&#64257;ltration of 3D interconnected microfluidic networks. The manufacturing of the reinforced beams begins with the fabrication of microfluidic networks, which involves layer-by-layer deposition of fugitive ink filaments using a dispensing robot, filling the empty space between filaments using a low viscosity resin, curing the resin and finally removing the ink.&#160;Self-supported 3D structures with other geometries and many layers (e.g.&#160;a few hundreds layers) could be built using this method. The resulting tubular micro&#64258;uidic networks are then infiltrated with thermosetting nanocomposite suspensions containing nanofillers (e.g.&#160;single-walled carbon nanotubes), and subsequently cured. The infiltration is done by applying a pressure gradient between two ends of the empty network (either by applying a vacuum or vacuum-assisted microinjection). Prior to the infiltration, the nanocomposite suspensions are prepared by dispersing nanofillers into polymer matrices using ultrasonication and three-roll mixing methods. The nanocomposites (i.e.&#160;materials infiltrated) are then solidified under UV exposure/heat cure, resulting in a 3D-reinforced composite structure. The technique presented here enables the design of functional nanocomposite macroscopic products for microengineering applications such as actuators and sensors.

Three-dimensional (3D) microstructured composite beams are fabricated through the directed and localized infiltration of nanocomposites into 3D porous microfluidic networks. The flexibility of this manufacturing method enables the utilization of different thermosetting materials and nanofillers in order to achieve a variety of functional 3D reinforced nanocomposite macroscopic products.

通过微流体渗透制备三维微结构纳米复合材料的制造

Microstructured composite beams reinforced with complex three-dimensionally (3D) patterned nanocomposite microfilaments are fabricated via nanocomposite ...

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 ...

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.

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 ...

Self-assembling Morphologies Obtained from Helical Polycarbodiimide Copolymers and Their Triazole Derivatives

A facile method for the preparation of polycarbodiimide-based secondary structures (e.g., nano-rings, &#34;craters,&#34; fibers, looped fibers, fibrous networks, ribbons, worm-like aggregates, toroidal structures, and spherical particles) is described. These aggregates are morphologically influenced by extensive hydrophobic side chain-side chain interactions of the singular polycarbodiimide strands, as inferred by atomic force microscopy (AFM) and scanning electron microscopy (SEM) techniques. Polycarbodiimide-g-polystyrene copolymers (PS-PCDs) were prepared by a combination of synthetic methods, including coordination-insertion polymerization, copper(I)-catalyzed azide alkyne cycloaddition (CuAAC) &#34;click&#34; chemistry, and atom transfer radical polymerization (ATRP). PS-PCDs were found to form specific toroidal architectures at low concentrations in CHCl3. To determine the influence of a more polar solvent medium (i.e., THF and THF/EtOH) on polymer aggregation behavior, a number of representative PS-PCD composites have been tested to show discrete concentration-dependent spherical particles. These fundamental studies are of practical interest to the development of experimental procedures for desirable architectures by directed self-assembly in thin film. These architectures may be exploited as drug carriers, whereas other morphological findings represent certain interest in the area of novel functional materials.

Here, we present a protocol to prepare and visualize secondary structures (e.g., fibers, toroidal architectures, and nano-spheres) derived from helical polycarbodiimides. The morphology characterized by both atomic force microscopy (AFM) and scanning electron microscopy (SEM) was shown to depend on molecular structure, concentration, and the solvent of choice.

从螺旋聚碳化二亚胺共聚物及其三唑衍生物获得自组装形貌

A facile method for the preparation of polycarbodiimide-based secondary structures (e.g., nano-rings, &#34;craters,&#34; fibers, looped fibers, fibrous ...

Precision Milling of Carbon Nanotube Forests Using Low Pressure Scanning Electron Microscopy

A nanoscale fabrication technique appropriate for milling carbon nanotube (CNT) forests is described. The technique utilizes an environmental scanning electron microscope (ESEM) operating with a low pressure water vapor ambient. In this technique, a portion of the electron beam interacts with the water vapor in the vicinity of the CNT sample, dissociating the water molecules into hydroxyl radicals and other species by radiolysis. The remainder of the electron beam interacts with the CNT forest sample, making it susceptible to oxidation from the chemical products of radiolysis. This technique may be used to trim a selected region of an individual CNT, or it may be used to remove hundreds of cubic microns of material by adjusting ESEM parameters. The machining resolution is similar to the imaging resolution of the ESEM itself. The technique produces only small quantities of carbon residue along the boundaries of the cutting zone, with minimal effect on the native structural morphology of the CNT forest.

Low pressure scanning electron microscopy in a water vapor ambient is used to machine nanoscale to microscale features in carbon nanotube forests.

碳纳米管森林精密铣床使用低压扫描电子显微镜

A nanoscale fabrication technique appropriate for milling carbon nanotube (CNT) forests is described. The technique utilizes an environmental scanning ...

Fabrication of a Bioactive, PCL-based "Self-fitting" Shape Memory Polymer Scaffold

Tissue engineering has been explored as an alternative strategy for the treatment of critical-sized cranio-maxillofacial (CMF) bone defects. Essential to the success of this approach is a scaffold that is able to conformally fit within an irregular defect while also having the requisite biodegradability, pore interconnectivity and bioactivity. By nature of their shape recovery and fixity properties, shape memory polymer (SMP) scaffolds could achieve defect &#8220;self-fitting.&#8221; In this way, following exposure to warm saline (~60 &#186;C), the SMP scaffold would become malleable, permitting it to be hand-pressed into an irregular defect. Subsequent cooling (~37 &#186;C) would return the scaffold to its relatively rigid state within the defect. To meet these requirements, this protocol describes the preparation of SMP scaffolds prepared via the photochemical cure of biodegradable polycaprolactone diacrylate (PCL-DA) using a solvent-casting particulate-leaching (SCPL) method. A fused salt template is utilized to achieve pore interconnectivity. To realize bioactivity, a polydopamine coating is applied to the surface of the scaffold pore walls. Characterization of self-fitting and shape memory behaviors, pore interconnectivity and in vitro bioactivity are also described.

Scaffolds capable of fitting within cranio-maxillofacial (CMF) bone defects while exhibiting osteoconductivity and bioactivity are of interest. This protocol describes the preparation of a shape memory scaffold based on polycaprolactone diacrylate (PCL-DA) using a solvent-casting particulate-leaching (SCPL) method employing a fused salt template and application of a bioactive polydopamine coating.

生物活性，PCL为基础的"自我装配"形状记忆聚合物支架的制备

Tissue engineering has been explored as an alternative strategy for the treatment of critical-sized cranio-maxillofacial (CMF) bone defects. Essential to ...

生物工程

Multiscale Structures Aggregated by Imprinted Nanofibers for Functional Surfaces

Multiscale surface structures have attracted increasing interest owing to several potential applications in surface devices. However, an existing challenge in the field is the fabrication of hybrid micro-nano structures using a facile, cost-effective, and high-throughput method. To overcome these challenges, this paper proposes a protocol to fabricate multiscale structures using only an imprint process with an anodic aluminum oxide (AAO) filter and an evaporative self-aggregation process of nanofibers. Unlike previous attempts that have aimed to straighten nanofibers, we demonstrate a unique fabrication method for multiscale aggregated nanofibers with high aspect ratios. Furthermore, the surface morphology and wettability of these structures on various liquids were investigated to facilitate their use in multifunctional surfaces.

Presented is an easy method to fabricate nano-micro multiscale structures, for functional surfaces, by aggregating nanofibers fabricated using an anodic aluminum oxide filter.

功能表面用印迹纳米纤维聚合的多尺度结构

Multiscale surface structures have attracted increasing interest owing to several potential applications in surface devices. However, an existing ...

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 ...