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>

<ol>
	<li>Iijima, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Helical+Microtubules+of+Graphitic+Carbon.">Helical Microtubules of Graphitic Carbon.</a> Nature. 354, 56-58 (1991).</li><li>Iijima, S., Ichihashi, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Single-Shell+Carbon+Nanotubes+of+1-nm+Diameter.">Single-Shell Carbon Nanotubes of 1-nm Diameter.</a> Nature. 363, 603-605 (1993).</li><li>Dai, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Carbon+Nanotubes:+Synthesis,+Integration+and+Properties.">Carbon Nanotubes: Synthesis, Integration and Properties.</a> Acc. Chem. Res. 35, 1035-1044 (2002).</li><li>Karousis, N., Tagmatarchis, N. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Current+Progress+on+the+Chemical+Modification+of+Carbon+Nanotubes.">Current Progress on the Chemical Modification of Carbon Nanotubes.</a> Chem. Rev. 110, 5366-5397 (2010).</li><li>Zhao, Y. L., Stoddart, J. F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Noncovalent+Functionalization+of+Single-Walled+Carbon+Nanotubes.">Noncovalent Functionalization of Single-Walled Carbon Nanotubes.</a> Acc. Chem. Res. 42, 1161-1171 (2009).</li><li>Zelada-Guill&#233;n, G. A., Riu, J., D&#252;zg&#252;n, A., Rius, F. X. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Immediate+Detection+of+Living+Bacteria+at+Ultralow+Concentrations+Using+a+Carbon+Nanotube+Based+Potentiometric+Aptasensor.">Immediate Detection of Living Bacteria at Ultralow Concentrations Using a Carbon Nanotube Based Potentiometric Aptasensor.</a> Angew. Chem. Int. Ed. 48, 7334-7337 (2009).</li><li>Zelada-Guill&#233;n, G. A., Blondeau, P., Rius, F. X., Riu, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Carbon+Nanotube-Based+Aptasensors+for+the+Rapid+and+Ultrasensitive+Detection+of+Bacteria.">Carbon Nanotube-Based Aptasensors for the Rapid and Ultrasensitive Detection of Bacteria.</a> Methods. 63, 233-238 (2013).</li><li>Jung, Y., Li, X., Rajan, N. K., Taylor, A. D., Reed, 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=Record+High+Efficiency+Single-Walled+Carbon+Nanotube/Silicon+p-n+Junction+Solar+Cells.">Record High Efficiency Single-Walled Carbon Nanotube/Silicon p-n Junction Solar Cells.</a> Nano Lett. 13, 95-99 (2013).</li><li>Esc&#225;rcega-Bobadilla, M. V., Rodr&#237;guez-P&#233;rez, L., Teuma, E., Serp, P., Masdeu-Bult&#243;, A. M., G&#243;mez, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Rhodium+Complexes+Containing+Chiral+P-Donor+Ligands+as+Catalysts+for+Asymmetric+Hydrogenation+in+Non+Conventional+Media.">Rhodium Complexes Containing Chiral P-Donor Ligands as Catalysts for Asymmetric Hydrogenation in Non Conventional Media.</a> Chem. Soc. Rev. 141, 808-816 (2011).</li><li>Miners, S. A., Rance, G. A., Khlobystov, A. N. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Chemical+Reactions+Confined+within+Carbon+Nanotubes.">Chemical Reactions Confined within Carbon Nanotubes.</a> Chem. Soc. Rev. 45, 4727-4746 (2016).</li><li>Rege, K., Raravikar, N. R., Kim, D. Y., Schadler, L. S., Ajayan, P. M., Dordick, J. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Enzyme-Polymer-Single+Walled+Carbon+Nanotube+Composites+as+Biocatalytic+Films.">Enzyme-Polymer-Single Walled Carbon Nanotube Composites as Biocatalytic Films.</a> Nano Lett. 3, 829-832 (2003).</li><li>Ma, R., Menamparambath, M. M., Nikolaev, P., Baik, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Transparent+Stretchable+Single-Walled+Carbon+Nanotube-Polymer+Composite+Films+with+Near-Infrared+Fluorescence.">Transparent Stretchable Single-Walled Carbon Nanotube-Polymer Composite Films with Near-Infrared Fluorescence.</a> Adv. Mater. 25, 2548-2553 (2013).</li><li>De Volder, M. F. L., Tawfick, S. H., Baughman, R. H., Hart, A. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Carbon+Nanotubes:+Present+and+Future+Commercial+Applications.">Carbon Nanotubes: Present and Future Commercial Applications.</a> Science. 339, 535-539 (2013).</li><li>Lehn, 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=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. G., Ziarelli, F., Margaillan, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=New+Insights+into+the+Adsorption+of+3-(Trimethoxysilyl)-propylmethacrylate+on+Hydroxylated+ZnO+Nanopowders.">New Insights into the Adsorption of 3-(Trimethoxysilyl)-propylmethacrylate on Hydroxylated ZnO Nanopowders.</a> Langmuir. 28, 3290-3297 (2012).</li><li>Wu, X., Qiu, J., Liu, P., Sakai, E., Lei, L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Polystyrene+Grafted+Carbon+Black+Synthesis+via+in+situ+Solution+Radical+Polymerization+in+Ionic+Liquid.">Polystyrene Grafted Carbon Black Synthesis via in situ Solution Radical Polymerization in Ionic Liquid.</a> J. Polym. Res. 20, 167 (2013).</li></ol>

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 border="0" cellpadding="0" cellspacing="0" width="1573">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:379px;">Tetrapropylammonium bromide, 99 % (TPABr)</td>
			<td style="width:181px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">88104</td>
			<td style="width:895px;">Irritant, toxic</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:379px;">Potassium permanganate, 99 % (KMnO4)</td>
			<td style="width:181px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">223468</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:379px;">Acetic acid, 99.5 %</td>
			<td style="width:181px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">45726</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:379px;">Pristine multiwalled carbon nanotubes, 99 % (MWCNTs)</td>
			<td style="width:181px;">Bayer Technology Services</td>
			<td style="width:119px;">Donated sample</td>
			<td>Harmful dusts. &#62;1 mm in length and 13&#8211;16 nm in outer diameter. Alternative supplier: Nanocyl, Catalog N. NC7000, website: http://www.nanocyl.com/</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:379px;">Sodium Chloride, 98 % (NaCl)</td>
			<td style="width:181px;">Sigma-Aldrich</td>
			<td style="width:119px;">S3014</td>
			<td>Technical grade can also be used</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:379px;">Ethanol, 99.8 % (EtOH)</td>
			<td style="width:181px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">32221</td>
			<td>Technical grade can also be used</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:379px;">Methanol, 99.8 % (MeOH)</td>
			<td style="width:181px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">322415</td>
			<td>Highly toxic. Technical grade can also be used</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:379px;">Hydroquinone, 99 %</td>
			<td style="width:181px;">Sigma-Aldrich</td>
			<td style="width:119px;">H9003</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:379px;">Toluene, 99.8 %</td>
			<td style="width:181px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">244511</td>
			<td>Anhydrous</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:379px;">3-(Trimethoxysilyl)propyl methacrylate, 98 % (TMSPMA)</td>
			<td style="width:181px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">440159</td>
			<td>Air sensitive, toxic</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:379px;">Azobisisobutyronitrile, 99 % (AIBN)</td>
			<td style="width:181px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">755745</td>
			<td>Explosive</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:379px;">Styrene, 99 %</td>
			<td style="width:181px;">Sigma-Aldrich</td>
			<td style="width:119px;">S4972</td>
			<td>Purified using an alumina gel preparative column and stored at 4 &#176;C</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:379px;">Acetone, 99.5 %</td>
			<td style="width:181px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">179124</td>
			<td>Technical grade can also be used</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:379px;">Tetrahydrofuran, 99.9 % (THF)</td>
			<td style="width:181px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">494461</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:379px;">Dichloromethane, 99.5 %</td>
			<td style="width:181px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">443484</td>
			<td>Highly toxic</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:379px;">Hydrochloric acid, 37 %</td>
			<td style="width:181px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">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 de Cartagena UDEC

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

Origami Inspired Self-assembly of Patterned and Reconfigurable Particles

There are numerous techniques such as photolithography, electron-beam lithography and soft-lithography that can be used to precisely pattern two dimensional (2D) structures. These technologies are mature, offer high precision and many of them can be implemented in a high-throughput manner. We leverage the advantages of planar lithography and combine them with self-folding methods1-20 wherein physical forces derived from surface tension or residual stress, are used to curve or fold planar structures into three dimensional (3D) structures. In doing so, we make it possible to mass produce precisely patterned static and reconfigurable particles that are challenging to synthesize.
In this paper, we detail visualized experimental protocols to create patterned particles, notably, (a) permanently bonded, hollow, polyhedra that self-assemble and self-seal due to the minimization of surface energy of liquefied hinges21-23 and (b) grippers that self-fold due to residual stress powered hinges24,25. The specific protocol described can be used to create particles with overall sizes ranging from the micrometer to the centimeter length scales. Further, arbitrary patterns can be defined on the surfaces of the particles of importance in colloidal science, electronics, optics and medicine. More generally, the concept of self-assembling mechanically rigid particles with self-sealing hinges is applicable, with some process modifications, to the creation of particles at even smaller, 100 nm length scales22, 26 and with a range of materials including metals21, semiconductors9 and polymers27. With respect to residual stress powered actuation of reconfigurable grasping devices, our specific protocol utilizes chromium hinges of relevance to devices with sizes ranging from 100 &mu;m to 2.5 mm. However, more generally, the concept of such tether-free residual stress powered actuation can be used with alternate high-stress materials such as heteroepitaxially deposited semiconductor films5,7 to possibly create even smaller nanoscale grasping devices.

We describe experimental details of the synthesis of patterned and reconfigurable particles from two dimensional (2D) precursors. This methodology can be used to create particles in a variety of shapes including polyhedra and grasping devices at length scales ranging from the micro to centimeter scale.

折纸灵感的图案和可重构颗粒自组装

There are numerous techniques such as photolithography, electron-beam lithography and soft-lithography that can be used to precisely pattern two ...

科研

化学

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) ...

Formation of Ordered Biomolecular Structures by the Self-assembly of Short Peptides

In nature, complex functional structures are formed by the self-assembly of biomolecules under mild conditions. Understanding the forces that control self-assembly and mimicking this process in vitro will bring about major advances in the areas of materials science and nanotechnology. Among the available biological building blocks, peptides have several advantages as they present substantial diversity, their synthesis in large scale is straightforward, and they can easily be modified with biological and chemical entities1,2. Several classes of designed peptides such as cyclic peptides, amphiphile peptides and peptide-conjugates self-assemble into ordered structures in solution. Homoaromatic dipeptides, are a class of short self-assembled peptides that contain all the molecular information needed to form ordered structures such as nanotubes, spheres and fibrils3-8. A large variety of these peptides is commercially available.
This paper presents a procedure that leads to the formation of ordered structures by the self-assembly of homoaromatic peptides. The protocol requires only commercial reagents and basic laboratory equipment. In addition, the paper describes some of the methods available for the characterization of peptide-based assemblies. These methods include electron and atomic force microscopy and Fourier-Transform Infrared Spectroscopy (FT-IR). Moreover, the manuscript demonstrates the blending of peptides (coassembly) and the formation of a &#34;beads on a string&#34;-like structure by this process.9 The protocols presented here can be adapted to other classes of peptides or biological building blocks and can potentially lead to the discovery of new peptide-based structures and to better control of their assembly.

This paper describes the formation of highly ordered peptide-based structures by the spontaneous process of self-assembly. The method utilizes commercially available peptides and common lab equipment. This technique can be applied to a large variety of peptides and may lead to the discovery of new peptide-based assemblies.

生物分子有序结构由短肽的自组装形成

In nature, complex functional structures are formed by the self-assembly of biomolecules under mild conditions. Understanding the forces that control ...

Self-assembly of Complex Two-dimensional Shapes from Single-stranded DNA Tiles

Current methods in DNA nano-architecture have successfully engineered a variety of 2D and 3D structures using principles of self-assembly. In this article, we describe detailed protocols on how to fabricate sophisticated 2D shapes through the self-assembly of uniquely addressable single-stranded DNA tiles which act as molecular pixels on a molecular canvas. Each single-stranded tile (SST) is a 42-nucleotide DNA strand composed of four concatenated modular domains which bind to four neighbors during self-assembly. The molecular canvas is a rectangle structure self-assembled from SSTs. A prescribed complex 2D shape is formed by selecting the constituent molecular pixels (SSTs) from a 310-pixel molecular canvas and then subjecting the corresponding strands to one-pot annealing. Due to the modular nature of the SST approach we demonstrate the scalability, versatility and robustness of this method. Compared with alternative methods, the SST method enables a wider selection of information polymers and sequences through the use of de novo designed and synthesized short DNA strands.

DNA tiling is an effective approach to make programmable nanostructures. We describe the protocols to construct complex two-dimensional shapes by the self-assembly of single-stranded DNA tiles.

复杂的二维形状的从单链DNA的瓷砖自组装

Current methods in DNA nano-architecture have successfully engineered a variety of 2D and 3D structures using principles of self-assembly. In this ...

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, ...

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 ...

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 ...

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 ...

Facet-to-facet Linking of Shape-anisotropic Colloidal Cadmium Chalcogenide Nanostructures

Here, we describe a protocol that allows for shape-anisotropic cadmium chalcogenide nanocrystals (NCs), such as nanorods (NRs) and tetrapods (TPs), to be covalently and site-specifically linked via their end facets, resulting in polymer-like linear or branched chains. The linking procedure begins with a cation-exchange process in which the end facets of the cadmium chalcogenide NCs are first converted to silver chalcogenide. This is followed by the selective removal of ligands at their surface. This results in cadmium chalcogenide NCs with highly reactive silver chalcogenide end facets that spontaneously fuse upon contact with each other, thereby establishing an interparticle facet-to-facet attachment. Through the judicious choice of precursor concentrations, an extensive network of linked NCs can be produced. Structural characterization of the linked NCs is carried out via low- and high-resolution transmission electron microscopy (TEM), as well as energy-dispersive X-ray spectroscopy, which confirm the presence of silver chalcogenide domains between chains of cadmium chalcogenide NCs.

A protocol detailing how shape-anisotropic colloidal cadmium chalcogenide nanocrystals can be covalently linked via their end facets is presented here.

形状-各向异性胶体镉硫纳米结构的 Facet-to-facet 连接

Here, we describe a protocol that allows for shape-anisotropic cadmium chalcogenide nanocrystals (NCs), such as nanorods (NRs) and tetrapods (TPs), to be ...

Liquid-cell Transmission Electron Microscopy for Tracking Self-assembly of Nanoparticles

Drying a nanoparticle dispersion is a versatile way to create self-assembled structures of nanoparticles, but the mechanism of this process is not fully understood. We have traced the trajectories of individual nanoparticles using liquid-cell transmission electron microscopy (TEM) to investigate the mechanism of the assembly process. Herein, we present the protocols used for liquid-cell TEM studies of the self-assembly mechanism. First, we introduce the detailed synthetic protocols used to produce uniformly sized platinum and lead selenide nanoparticles. Next, we present the microfabrication processes used to produce liquid cells with silicon nitride or silicon windows and then describe the loading and imaging procedures of the liquid-cell TEM technique. Several notes are included to provide helpful tips for the entire process, including how to manage the fragile cell windows. The individual motions of nanoparticles tracked by liquid-cell TEM revealed that changes in the solvent boundaries caused by evaporation affected the self-assembly process of nanoparticles. The solvent boundaries drove nanoparticles to primarily form amorphous aggregates, followed by flattening of the aggregates to produce a 2-dimensional (2D) self-assembled structure. These behaviors are also observed for different nanoparticle types and different liquid-cell compositions.

Here we introduce experimental protocols for the real-time observation of a self-assembly process using liquid-cell transmission electron microscopy.

用于跟踪纳米粒子自组装的液体细胞透射电子显微镜

Drying a nanoparticle dispersion is a versatile way to create self-assembled structures of nanoparticles, but the mechanism of this process is not fully ...