这项工作是由加拿大多伦多大学，自然科学和工程研究理事会，加拿大创新基金会，加拿大，安大略省研究基金支持。 DSS的早期研究者奖感谢安大略省。

1。形成的银工作电极<ol><li> AAO膜基片的顶侧固定在玻璃板上，使用2 - 双面粘合。注意:与粘合剂接触的膜面积最小化，因为它会堵塞毛孔。 </li><li>成的金属蒸发器的基板保持器，安装在玻璃板，关闭的腔室，并撤离到压力低于1.0μTorr。 </li><li>使用一个电阻源，蒸发到衬底上的银颗粒（纯度&gt; 99.99％），直到达到的层厚度为100nm，然后在0.8埃/秒的速率增加的蒸发速率的最终厚度为1.5埃/秒，直到达到250纳米。 </li><li>释放的阳极氧化铝膜的粘接剂层用二氯甲烷溶解粘合剂润湿，用棉签擦拭。 </li></ol> 2。电铜和镍<ol><li>步骤2-3使用一个自定义的两片式开面铁氟龙电化学电池，持有阳极氧化铝膜接触的，作为工作电极（ 图2）用导电性箔。的小区设计的细节可以在别处找到45。清洁特氟隆细胞漂洗3×10秒，然后，丙酮，乙醇，18.2MΩ的去离子水。让干细胞在实验室环境空气。 </li><li>膜侧银放置到一块光滑铝箔在特氟隆电化学电池，密封的工作电极的面积与氟橡胶O形环（ 图2）。 </li><li>加入3.0毫升的无电镀铜溶液（0.95米的CuSO 4（5H 2 O），0.21 MH 2 SO 4）的Teflon小区。连接铂计数器电极，参考电极水溶液与铝箔到恒电位仪使用常规的3电极设置工作电极。 15分钟-90毫伏vs.Ag / AgCl的施加电势。 </li><li>断开和删除的参考和辅助电极，保持两件CE11和AAO膜完好，箔，运行18.2MΩ的去离子水，然后用清水冲洗下的单元格。让细胞5毫升18.2兆欧的去离子水浸泡30分钟以除去过量的铜电镀液从毛孔内的。 </li><li>清空的单元格，以及商业镀镍溶液中的3.0毫升（瓦特镍纯从Technic INC。）添加并连接计数器的参考，和步骤2.3中所描述的工作电极。应用的电位为-900毫伏vs.Ag / AgCl的20分钟。 </li><li>断开并取下两片电池和AAO膜和金属箔完整的参考和辅助电极保持。 18.2MΩ的去离子水冲洗细胞3×10秒，然后让它在5毫升18.2MΩ的去离子水浸泡30分钟，以去除多余的电镀液从毛孔。让细胞彻底干燥，在实验室环境空气中过夜。 </li></ol> 3。电聚合的聚合物电芯<ol><li>把完整的特氟纶细胞总成在惰性气氛的手套式操作箱配有外部连接到恒电位仪，Y到。 </li><li>准备的30mM 3 - 己基噻吩的溶液在3.0毫升46％的三氟化硼乙醚，并把它添加到特氟隆电化学电池。 </li><li>计数器连接到恒电位仪的工作电极，如步骤2.3中描述。加入的Ag / AgNO 3的乙腈中的参考电极和连接步骤2.3中描述。应用1500毫伏相对于Ag / AgNO 3的 10分钟的电位。电流上的顺序0.1毫安表明一个成功的沉积（ 图3）。 </li><li>断开并删除的参考电极和辅助电极保持的两件式的细胞和AAO膜和箔完整并冲洗细胞与5毫升乙腈中的手套箱中，以除去过量的三氟化硼。从手套箱中取出细胞，并用5毫升等分的乙醇冲洗，然后使该细胞在新鲜的乙醇中浸泡20分钟。再次冲洗细胞用5ml英里<html> LLI-Q 18.2MΩ的去离子水，然后让细胞在18.2MΩ的去离子水浸泡20分钟。允许它在实验室环境空气干燥。 </li></ol> 4。电金壳<ol><li>加入3.0毫升的商业镀金溶液（Orotemp 24 RTU从Technic公司）特氟隆细胞，混合，用移液管，持续2分钟，以允许镀金溶液完全渗透毛孔和诱导聚合物芯的疏水崩溃。 </li><li>工作电极，反电极和参考电极水溶液在步骤2.3到恒电位连接，并适用于-920毫伏vs.Ag / AgCl的不同时间（5分钟至5小时）。电流上的顺序0.5毫安表明一个成功的沉积（ 图3）。黄金碳纳米管的长度确定的沉积时间（ 图4）。 </li><li> 18.2兆欧的去离子水的流下冲洗细胞，并让其干燥。 </li></ol>文件"&gt; 5。删除牺牲材料和隔离的黄金纳米管<ol><li>取出的膜从Teflon单元组件，并用几滴浓溶解的银，铜和镍。硝酸（&gt; 68％）的银涂层的一面。除去酸和18.2兆欧的去离子水冲洗膜3×10秒。 </li><li>蚀刻聚合物芯膜浸渍过夜，以3:1体积/体积的硫酸溶液和30％的过氧化氢（注意！此解决方案是一种强氧化剂，应小心处理）。 </li><li>除去酸溶液和18.2mΩ的去离子水的流下冲洗膜。打破膜切成小块，地点在3.0 mL离心瓶，并加入2毫升的水3.0 M NaOH溶液。搅动小瓶操作加热的混合器中以1,000 rpm和40℃下进行3小时或，直到膜溶解。 </li><li>离心混合物在21,000 xg离心10分钟，除去上层液体，并更换Ë它用18.2MΩ的去离子水。重复这个周期的3倍。现在的小瓶含有温和的超声的黄金纳米管可以暂停。经超声和悬挂系统的解决方案应该出现浅紫色。 </li></ol> 6。黄金纳米管的光学特性<ol><li>要测量光谱，离心21000×g离心10分钟，在的黄金纳米管的解决方案，除去上层液体，取而代之的是与D 2 O。重复此过程3次。 </li><li>超声混合物，持续30秒，直到溶液变得清晰，将溶液转移到一个1毫升的石英比色皿。 </li><li>获取的消光光谱紫外/可见分光光度计在200nm至2,000 nm的，在双光束模式操作，与D 2 O作为基准单元使用一个反应杯中。两个吸光度应该存在，相应的横向和纵向的等离激元模式（ 图5）。 </li><li>为了测量固态光谱，proceed到步骤5.2。停止并放置在载玻片上的完整的包膜。 </li><li>湿膜和载玻片与D 2 O，以提高透明度。 </li><li>将膜固定在载玻片上，将其安装在一个薄膜样本保持器的紫外/可见分光光度计。工作在双光束模式下，得到的消光光谱从200nm至1,300 nm的作为基准使用的玻璃滑动。 </li></ol>

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R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Template-Fabricated+Gold+Nanowires+and+Nanotubes.">Template-Fabricated Gold Nanowires and Nanotubes.</a> Advanced Materials. 15 (5), 455-458 (2003).</li><li>Sehayek, T., Lahav, M., Popovitz-Biro, R., Vaskevich, A., Rubinstein, I. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Template+Synthesis+of+Nanotubes+by+Room-Temperature+Coalescence+of+Metal+Nanoparticles.">Template Synthesis of Nanotubes by Room-Temperature Coalescence of Metal Nanoparticles.</a> Chemistry of Materials. 17 (14), 3743-3748 (2005).</li><li>Lahav, M., Sehayek, T., Vaskevich, A., Rubinstein, I. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nanoparticle+Nanotubes.">Nanoparticle Nanotubes.</a> Angewandte Chemie (International ed. in English). 42 (45), 5576-5579 (2003).</li><li>Hua, Z., Yang, S., 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=Metal+nanotubes+prepared+by+a+sol-gel+method+followed+by+a+hydrogen+reduction+procedure.">Metal nanotubes prepared by a sol-gel method followed by a hydrogen reduction procedure.</a> Nanotechnology. 17 (20), 5106-5110 (2006).</li><li>Lee, W., Scholz, R., Nielsch, K., G&#246;sele, U. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+Template-Based+Electrochemical+Method+for+the+Synthesis+of+Multisegmented+Metallic+Nanotubes.">A Template-Based Electrochemical Method for the Synthesis of Multisegmented Metallic Nanotubes.</a> Angewandte Chemie (International ed. in English). 44 (37), 6050-6054 (2005).</li><li>Cui, C. -. H., Li, H. -. H., Yu, S. -. H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+general+approach+to+electrochemical+deposition+of+high+quality+free-standing+noble+metal+(Pd,+Pt,+Au,+Ag)+sub-micron+tubes+composed+of+nanoparticles+in+polar+aprotic+solvent.">A general approach to electrochemical deposition of high quality free-standing noble metal (Pd, Pt, Au, Ag) sub-micron tubes composed of nanoparticles in polar aprotic solvent.</a> Chemical Communications. 46 (6), 940 (2010).</li><li>Han, X. -. F., Shamaila, S., Sharif, R., Chen, J. -. Y., Liu, H. -. R., Liu, D. -. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Structural+and+Magnetic+Properties+of+Various+Ferromagnetic+Nanotubes.">Structural and Magnetic Properties of Various Ferromagnetic Nanotubes.</a> Advanced Materials. 21 (45), 4619-4624 (2009).</li><li>Hendren, W. R., Murphy, A., 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=Fabrication+and+optical+properties+of+gold+nanotube+arrays.">Fabrication and optical properties of gold nanotube arrays.</a> Journal of Physics: Condensed Matter. 20 (36), 362203 (2008).</li><li>Lahav, M., Weiss, E. A., Xu, Q., Whitesides, G. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Core-Shell+and+Segmented+Polymer-Metal+Composite+Nanostructures.">Core-Shell and Segmented Polymer-Metal Composite Nanostructures.</a> Nano Letters. 6 (9), 2166-2171 (2006).</li><li>Chen, X., Li, S., Xue, C., Banholzer, M. J., Schatz, G. C., Mirkin, C. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Plasmonic+Focusing+in+Rod-Sheath+Heteronanostructures.">Plasmonic Focusing in Rod-Sheath Heteronanostructures.</a> ACS Nano. 3 (1), 87-92 (2009).</li><li>Banholzer, M. J., Qin, L., Millstone, J. E., Osberg, K. D., Mirkin, C. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=On-wire+lithography:+synthesis,+encoding+and+biological+applications.">On-wire lithography: synthesis, encoding and biological applications.</a> Nature Protocols. 4 (6), 838-848 (2009).</li></ol>

AAO膜纳米棒的模板合成已成为越来越流行，但是合成的纳米棒往往是对材料和合成条件的细微变化非常敏感。在这里，采用AAO膜的优点和局限性，列出一个全面的了解，以及使用阳极氧化铝膜的电化学合成纳米结构的一般准则。 购买AAO膜时，一般有两种类型可供选择:非对称和对称。非对称膜的有孔的直径从顶部向底部变化的。模板的底部通常包含支链的网络的孔，最终导致...

当它们的尺寸接近的光的穿透深度（约50 nm的纳米级），贵金属，和最重要的是金的，表现出精致的大小，形状和环境依赖性的光学特性24，25。在这个规模，直接照射会导致表面等离子体共振（SPR）被称为传导电子的相干振荡。 SPR是高度依赖于纳米结构的大小，形状，和周围介质的介电性能。有极大的兴趣特征SPR特性，在新材料，SPR为基础的设备不断涌现在亚波长光学，SERS基板，超灵敏的光学传感器，11-16，26-29。因此，开发的计算方法，更准确地预测规模和结构可以改变电浆反应仍然是一个主要的目标。 AAO膜的使用提供了一个方便的方式来改变颗粒的直径或长度，和几个重要的研究，使用此关联我消化率和计算的等离激元具有不同颗粒直径，长度，和纵横比为30，31的响应。也许最研究，并成功地利用电浆材料的折射率传感器。对于这一点，在红色，近红外（NIR）范围内（〜800 - 1300纳米）的共振是可取的，因为它们是更敏感的折射率变化，以及在于"水窗"，使得它们通过水和发送人体组织。在此范围内开放有趣的可能性， 在体内电浆生物传感与SPR峰的解决方案-悬浮纳米结构。 多孔阳极氧化铝已通过电化学合成或模板润湿用于制备聚合物纳米管或纳米线，并证明是适用于各种各样的材料。 AAO膜现在正在使用的综合解决方案悬浮的高纵横比的纳米棒和纳米结构阵列作为高性能电浆生物传感器或SER小号基板。虽然阳极氧化铝膜，大多被用作模板，用于合成固体棒，在某些情况下，它可能是可取的是中空的结构。电浆和SERS传感应用中，例如，基于表面，并具有大的表面面积与体积比的中空结构，可能会导致产生更强的信号和更高的灵敏度14，15，32。相对于这个已被合成，黄金碳纳米管从各种方法，包括电镀，无电解电镀34，35，模板孔隙36的表面变形，37次 ，溶胶-凝胶的方法38，和电沉积39-41银纳米棒33上的置换反应。这些合成通常留下不好的，多孔管或允许几乎没有控制权的大小和形态。的合成也有报道，其特征在于，淀积在金属壳在AAO膜42，43中的聚合物的核心。这些合成离开金nanotubes绑定到基板，并依赖于模板的蚀刻，以允许周围的聚合物增长的黄金，因此它们不能在溶液中进行研究。此外，模板刻蚀有一些潜在的缺点。首先，非均匀的孔蚀刻沿模板壁可能导致非均匀的金壳厚度。二，显着的蚀刻（ 即很厚的壁管）完全溶解毛孔壁。 最近，桥梁等人报道的腐蚀剂自由方法合成金的纳米管在阳极氧化铝膜，使用的牺牲的聚（3 -己基）噻吩的核心和产量溶液悬浮黄金碳纳米管具有非常高的折射率灵敏度15。从该和随后的工作中，它被发现未经化学蚀刻以沉积金壳聚合物纤芯周围，聚合物必须是管状的，例如，有它折叠的内部空间，并且该聚合物必须是疏水性的，使得其将关口失效到本身，而不是坚持的模板孔壁16。当亲水性聚合物的使用，一金"鞘"部分地覆盖的聚合物芯的观察，表明聚合物芯附着金沉积期间44的模板的壁之一。这里，中空黄金碳纳米管的合成，它允许长度和直径的控制协议，用于详细描述（ 图1）。这些解决方案悬浮的黄金纳米管是为广泛的应用，包括电浆生物感测或SERS衬底材料。

<table border="1"><tbody><tr><td></td><td></td><td></td><td> 试剂/材料 </td></tr><tr><td> UniKera标准膜</td><td> Synkera科技有限公司</td><td> SM-XY-13 </td><td>各种孔径大小范围为13 - 150nm的阳极氧化铝膜是可从synkera，从50到100微米的厚度。我们使用50微米的。它们是对称的，这意味着从顶部到底部是均匀的孔径。 </td></tr><tr><td> Anopore无机膜</td><td> Whatman公司</td><td> 6809-7023 </td><td> 13毫米直径，200 nm的孔径。这些膜是很脆弱的。的孔的直径是不统一的，所以重要的是要始终使用该膜作为工作电极底部</td></tr><tr><td>银颗粒％，99.99 </td><td>科特•莱思科</td><td> EVMAG40EXE-D </td><td></td></tr><tr><td>铜（II）五水硫酸铜&lt;/ TD&gt; <td> Sigma-Aldrich公司</td><td> 209189 </td><td></td></tr><tr><td>硫酸</td><td> ACP </td><td> S8780 </td><td>注意:腐蚀性液体。 </td></tr><tr><td>过氧化氢（30％） </td><td> ACP </td><td> H7000 </td><td>注意:氧化性液体</td></tr><tr><td>硝酸</td><td> ACP </td><td> N2800 </td><td>注意:腐蚀性的发烟液体， </td></tr><tr><td>氢氧化钠</td><td> Fisher Scientific则</td><td> S318-1 </td><td>注意:腐蚀性的粉末</td></tr><tr><td>瓦特镍纯</td><td>工艺公司</td><td> 130859 </td><td>产品不再是可以从Technic公司。，但是将其他商业nickelplating解决方案。 </td></tr><tr><td>技术黄金434HS </td><td>工艺公司</td><td> X6763600 </td><td>含有氰化物，​​不酸化</td></tr><tr><td>三氟化硼乙醚</td><td>西格玛-Aldrich公司</td><td> 175501-100ML </td><td>必须存储并在惰性气氛下使用</td></tr><tr><td> 3 - 己基噻吩</td><td> Sigma-Aldrich公司</td><td> 399051-5G </td><td></td></tr><tr><td>氧化氘</td><td> Sigma-Aldrich公司</td><td> 151880-100G </td><td></td></tr><tr><td>乙腈（无水） </td><td> Sigma-Aldrich公司</td><td> 271004 </td><td></td></tr><tr><td>乙醇（无水） </td><td>克力实验室</td><td> 1500年1月5日</td><td></td></tr><tr><td></td><td></td><td></td><td> 设备 </td></tr><tr><td> EC小量电位/恒电流</td><td>巴斯（生物分析系统公司） </td><td> N / A </td><td>参比电极和铂丝与恒电位仪，，和更换是从巴斯<a href="http://www.basinc.com/products/ec/epsilon/features.html" target="_blank">HTTP的</a> purchaes <a href="http://www.basinc.com/products/ec/epsilon/features.html" target="_blank">:</a><html> / / www.basinc.com的/产品/ EC /ε/ features.html </td></tr><tr><td> Cary 5000型紫外 - 可见 - 近红外分光光度计</td><td>安捷伦科技公司</td><td> N / A </td><td> </td></tr><tr><td>恒温ŕ </td><td> Eppendorf公司</td><td> N / A </td><td> <a href="http://www.eppendorf.com/int/index.php?action=products&amp;contentid=1&amp;catalognode=9832" target="_blank">http://www.eppendorf.com/int/index.php?action=products&amp;contentid=1&amp;catalognode=9832</a> </td></tr><tr><td>布兰森2510超声波清洗机</td><td> Bransonic </td><td> Z244810（来自Sigma Aldrich） </td><td>/ aldrich/Z244910？LANG = EN＆地区= CA"目标="_blank"&gt; http://www.sigmaaldrich.com/catalog/product/aldrich/Z244910?lang=en&amp;region=CA </td></tr><tr><td> COVAP 2热蒸发器</td><td>埃工程</td><td> N / A </td><td> <a href="http://www.angstromengineering.com/covap.html" target="_blank">http://www.angstromengineering.com/covap.html</a> </td></tr><tr><td> Millipore公司协同水净化系统</td><td>密理博</td><td> N / A </td><td> <a href="http://www.millipore.com/catalogue/module/c9209" target="_blank">http://www.millipore.com/catalogue/module/c9209</a> </td></tr></tbody></table>

template directed synthesis of plasmonic gold nanotubes with tunable ir absorbance

可以产生一个几乎平行阵列的孔，通过阳极氧化在酸性环境中1，2的铝箔。自1990年以来一直在开发的阳极氧化铝（AAO）膜的应用和模板合成的高宽比的纳米结构，主要是通过电化学增长或孔隙的润湿已成为一种常见的方法。最近，这些膜已成为市售在很宽的范围内的孔的尺寸和密度，从而导致被从阳极氧化铝膜的合成功能的纳米结构的一个广泛的图书馆。这些包括复合材料制成的金属，无机材料或聚合物3-10纳米棒，纳米线和纳米管的。纳米多孔膜已被用于合成纳米粒子和纳米管阵列，执行以及折射率传感器，电浆生物传感器，表面增强拉曼光谱（SERS）基板11-16，以及广泛的其他领域，如光热加热17日 ，:选择渗透运输18，19 20，催化，微流体21，和电化学传感器22，23。在这里，我们提出了一种新颖的程序，准备金的纳米管在AAO膜。空心纳米结构具有潜在的应用电浆和表面增强拉曼光谱感应，我们预计这些黄金纳米管将允许产生的高灵敏度和强大的等离子激元的信号，减少材料阻尼15。

每个步骤之后，人们可以明显地确定是否合成是成功的，通过观察该膜的颜色。沉积铜（2.3）后的模板将出现紫色。在沉积镍（2.5）的模板会慢慢变成黑色。后的聚合物淀积（步骤3.3）模板应显得更暗紫色/黑色和更有光泽（ 图2）。成功聚合物和金的典型chronoapmerograms包括（ 图3）。在最后的蚀刻工序（5.2），该模板应出现紫色的和不透明的（ 图2），由于黄?...

Watch this Scientific Journal Video about Template Directed Synthesis of Plasmonic Gold Nanotubes with Tunable IR Absorbance at JoVE.com

Template Directed Synthesis of Plasmonic Gold Nanotubes with Tunable IR Absorbance

解决方案悬浮黄金碳纳米管具有受控的尺寸，可以合成由电化学沉积在多孔阳极氧化铝（AAO）膜使用的疏水性聚合物的芯。黄金纳米管和纳米管阵列有希望在电浆生物传感，表面增强拉曼光谱，光热加热，离子和分子运输，微流体，催化和电化学传感应用。

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) ...

template-directed-synthesis-plasmonic-gold-nanotubes-with-tunable-ir

Research

JoVE Journal

Chemistry

16.1K 次观看.  University of Toronto. 解决方案悬浮黄金碳纳米管具有受控的尺寸，可以合成由电化学沉积在多孔阳极氧化铝（AAO）膜使用的疏水性聚合物的芯。黄金纳米管和纳米管阵列有希望在电浆生物传感，表面增强拉曼光谱，光热加热，离子和分子运输，微流体，催化和电化学传感应用。

视频: Template Directed Synthesis of Plasmonic Gold Nanotubes with Tunable IR Absorbance

Synthesis of Immunotargeted Magneto-plasmonic Nanoclusters

Magnetic and plasmonic properties combined in a single nanoparticle provide a synergy that is advantageous in a number of biomedical applications including contrast enhancement in novel magnetomotive imaging modalities, simultaneous capture&#160;and detection of circulating tumor cells (CTCs),&#160;and multimodal molecular imaging combined with photothermal therapy of cancer cells. These applications have stimulated significant interest in development of protocols for synthesis of magneto-plasmonic nanoparticles with optical absorbance in the near-infrared (NIR) region and a strong magnetic moment. Here, we present a novel protocol for synthesis of such hybrid nanoparticles that is based on an oil-in-water microemulsion method. The unique feature of the protocol described herein is synthesis of magneto-plasmonic nanoparticles of various sizes from primary blocks which also have magneto-plasmonic characteristics. This approach yields nanoparticles with a high density of magnetic and plasmonic functionalities which are uniformly distributed throughout the nanoparticle volume. The hybrid nanoparticles can be easily functionalized by attaching antibodies through the Fc moiety leaving the Fab portion that is responsible for antigen binding available for targeting.

Here, we describe a protocol for synthesis of magneto-plasmonic nanoparticles with a strong magnetic moment and a strong near-infrared (NIR) absorbance. The protocol also includes antibody conjugation to the nanoparticles through the Fc moiety for various biomedical applications which require molecular specific targeting.

Immunotargeted的合成磁等离子团簇

Magnetic and plasmonic properties combined in a single nanoparticle provide a synergy that is advantageous in a number of biomedical applications ...

科研

化学

Synthesis and Catalytic Performance of Gold Intercalated in the Walls of Mesoporous Silica

As a promising catalytically active nano reactor, gold nanoparticles intercalated in mesoporous silica (GMS) were successfully synthesized and properties of the materials were investigated. We used a one pot sol-gel approach to intercalate gold nano particles in the walls of mesoporous silica. To start with the synthesis, P123 was used as template to form micelles. Then TESPTS was used as a surface modification agent to intercalate gold nano particles. Following this process, TEOS was added in as a silica source which underwent a polymerization process in acid environment. After hydrothermal processing and calcination, the final product was acquired. Several techniques were utilized to characterize the porosity, morphology and structure of the gold intercalated mesoporous silica. The results showed a stable structure of mesoporous silica after gold intercalation. Through the oxidation of benzyl alcohol as a benchmark reaction, the GMS materials showed high selectivity and recyclability.

Here, we present a protocol with a sol-gel process to synthesize gold intercalated in the walls of mesoporous materials (GMS), which is confirmed to possess a mesoporous matrix with gold intercalated in the walls imparting great stability and recyclability.

合成和金插在介孔二氧化硅的墙壁催化性能

As a promising catalytically active nano reactor, gold nanoparticles intercalated in mesoporous silica (GMS) were successfully synthesized and properties ...

A Simple Method for the Size Controlled Synthesis of Stable Oligomeric Clusters of Gold Nanoparticles under Ambient Conditions

Reducing dilute aqueous HAuCl4 with sodium thiocyanate (NaSCN) under alkaline conditions produces 2 to 3 nm diameter nanoparticles. Stable grape-like oligomeric clusters of these yellow nanoparticles of narrow size distribution are synthesized under ambient conditions via two methods. The delay-time method controls the number of subunits in the oligoclusters by varying the time between the addition of HAuCl4 to alkaline solution and the subsequent addition of reducing agent, NaSCN. The yellow oligoclusters produced range in size from ~3 to ~25 nm. This size range can be further extended by an add-on method utilizing hydroxylated gold chloride (Na+[Au(OH4-x)Clx]-) to auto-catalytically increase the number of subunits in the as-synthesized oligocluster nanoparticles, providing a total range of 3 nm to 70 nm. The crude oligocluster preparations display narrow size distributions and do not require further fractionation for most purposes. The oligoclusters formed can be concentrated &#62;300 fold without aggregation and the crude reaction mixtures remain stable for weeks without further processing. Because these oligomeric clusters can be concentrated before derivatization they allow expensive derivatizing agents to be used economically. In addition, we present two models by which predictions of particle size can be made with great accuracy.

We describe a simple method for producing highly stable oligomeric clusters of gold nanoparticles via the reduction of chloroauric acid (HAuCl4) with sodium thiocyanate (NaSCN). The oligoclusters have a narrow size distribution and can be produced with a wide range of sizes and surface coats.

根据环境条件的金纳米粒子的稳定低聚簇的大小控制合成的一种简便方法

Reducing dilute aqueous HAuCl4 with sodium thiocyanate (NaSCN) under alkaline conditions produces 2 to 3 nm diameter nanoparticles. Stable grape-like ...

Hydroquinone Based Synthesis of Gold Nanorods

Gold nanorods are an important kind of nanoparticles characterized by peculiar plasmonic properties. Despite their widespread use in nanotechnology, the synthetic methods for the preparation of gold nanorods are still not fully optimized. In this paper we describe a new, highly efficient, two-step protocol based on the use of hydroquinone as a mild reducing agent. Our approach allows the preparation of nanorods with a good control of size and aspect ratio (AR) simply by varying the amount of hexadecyl trimethylammonium bromide (CTAB) and silver ions (Ag+) present in the "growth solution". By using this method, it is possible to markedly reduce the amount of CTAB, an expensive and cytotoxic reagent, necessary to obtain the elongated shape. Gold nanorods with an aspect ratio of about 3 can be obtained in the presence of just 50 mM of CTAB (versus 100 mM used in the standard protocol based on the use of ascorbic acid), while shorter gold nanorods are obtained using a concentration as low as 10 mM.

This paper describes a protocol for the synthesis of gold nanorods, based on the use of hydroquinone as reducing agent, plus the different mechanisms for controlling their size and aspect ratio.

金纳米棒基于对苯二酚合成

Gold nanorods are an important kind of nanoparticles characterized by peculiar plasmonic properties. Despite their widespread use in nanotechnology, the ...

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 ...

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 ...

Rapid Nanoprobe Signal Enhancement by In Situ Gold Nanoparticle Synthesis

The use of nanoprobes such as gold, silver, silica or iron-oxide nanoparticles as detection reagents in bioanalytical assays can enable high sensitivity and convenient colorimetric readout. However, high densities of nanoparticles are typically needed for detection. The available synthesis-based enhancement protocols are either limited to gold and silver nanoparticles or rely on precise enzymatic control and optimization. Here, we present a protocol to enhance the colorimetric readout of gold, silver, silica, and iron oxide nanoprobes. It was observed that the colorimetric signal can be improved by up to a 10000-fold factor. The basis for such signal enhancement strategies is the chemical reduction of Au3+ to Au0. There are several chemical reactions that enable the reduction of Au3+ to Au0. In the protocol, Good&#39;s buffers and H2O2 are used and it is possible to favor the deposition of Au0 onto the surface of existing nanoprobes, in detriment of the formation of new gold nanoparticles. The protocol consists of the incubation of the microarray with a solution consisting of chloroauric acid and H2O2 in 2-(N-morpholino)ethanesulfonic acid pH 6 buffer following the nanoprobe-based detection assay. The enhancement solution can be applied to paper and glass-based sensors. Moreover, it can be used in commercially available immunoassays as demonstrated by the application of the method to a commercial allergen microarray. The signal development requires less than 5 min of incubation with the enhancement solution and the readout can be assessed by naked eye or low-end image acquisition devices such as a table-top scanner or a digital camera.

Rapid Nanoprobe Signal Enhancement by In Situ Gold Nanoparticle Synthesis

In this work, a protocol for signal enhancement of nanoprobe-based biosensing is presented. The protocol is based on the reduction of chloroauric acid onto the surface of existing nanoprobes that consist of gold, silver, silica or iron-oxide nanoparticles.

原位金纳米粒子合成快速 Nanoprobe 信号增强

The use of nanoprobes such as gold, silver, silica or iron-oxide nanoparticles as detection reagents in bioanalytical assays can enable high sensitivity ...

Synthesis and Characterization of Amphiphilic Gold Nanoparticles

Gold nanoparticles covered with a mixture of 1-octanethiol (OT) and 11-mercapto-1-undecane sulfonic acid (MUS) have been extensively studied because of their interactions with cell membranes, lipid bilayers, and viruses. The hydrophilic ligands make these particles colloidally stable in aqueous solutions and the combination with hydrophobic ligands creates an amphiphilic particle that can be loaded with hydrophobic drugs, fuse with the lipid membranes, and resist nonspecific protein adsorption. Many of these properties depend on nanoparticle size and the composition of the ligand shell. It is, therefore, crucial to have a reproducible synthetic method and reliable characterization techniques that allow the determination of nanoparticle properties and the ligand shell composition. Here, a one-phase chemical reduction, followed by a thorough purification to synthesize these nanoparticles with diameters below 5 nm, is presented. The ratio between the two ligands on the surface of the nanoparticle can be tuned through their stoichiometric ratio used during synthesis. We demonstrate how various routine techniques, such as transmission electron microscopy (TEM), nuclear magnetic resonance (NMR), thermogravimetric analysis (TGA), and ultraviolet-visible (UV-Vis) spectrometry, are combined to comprehensively characterize the physicochemical parameters of the nanoparticles.

Amphiphilic gold nanoparticles can be used in many biological applications. A protocol to synthesize gold nanoparticles coated by a binary mixture of ligands and a detailed characterization of these particles is presented.

两栖金纳米粒子的合成与表征

Gold nanoparticles covered with a mixture of 1-octanethiol (OT) and 11-mercapto-1-undecane sulfonic acid (MUS) have been extensively studied because of ...

Assembly of Gold Nanorods into Chiral Plasmonic Metamolecules Using DNA Origami Templates

The inherent addressability of DNA origami structures makes them ideal templates for the arrangement of metal nanoparticles into complex plasmonic nanostructures. The high spatial precision of a DNA origami-templated assembly allows controlling the coupling between plasmonic resonances of individual particles and enables tailoring optical properties of the constructed nanostructures. Recently, chiral plasmonic systems attracted a lot of attention due to the strong correlation between the spatial configuration of plasmonic assemblies and their optical responses (e.g., circular dichroism [CD]). In this protocol, we describe the whole workflow for the generation of DNA origami-based chiral assemblies of gold nanorods (AuNRs). The protocol includes a detailed description of the design principles and experimental procedures for the fabrication of DNA origami templates, the synthesis of AuNRs, and the assembly of origami-AuNR structures. In addition, the characterization of structures using transmission electron microscopy (TEM) and CD spectroscopy is included. The described protocol is not limited to chiral configurations and can be adapted for the construction of various plasmonic architectures.

We describe the detailed protocol for the DNA origami-based assembly of gold nanorods into chiral plasmonic metamolecules with strong chiroptical responses. The protocol is not limited to chiral configurations and can be easily adapted for the fabrication of various plasmonic architectures.

利用 dna 折纸模板将金纳米产物组装成手性质浆细胞分裂体

The inherent addressability of DNA origami structures makes them ideal templates for the arrangement of metal nanoparticles into complex plasmonic ...

Synthesis of Information-bearing Peptoids and their Sequence-directed Dynamic Covalent Self-assembly

This protocol presents the use of Lewis acidic multi-role reagents to circumvent kinetic trapping observed during the self-assembly of information-encoded oligomeric strands mediated by paired dynamic covalent interactions in a manner mimicking the thermal cycling commonly employed for the self-assembly of complementary nucleic acid sequences. Primary amine monomers bearing aldehyde and amine pendant moieties are functionalized with orthogonal protecting groups for use as dynamic covalent reactant pairs. Using a modified automated peptide synthesizer, the primary amine monomers are encoded into oligo(peptoid) strands through solid-phase submonomer synthesis. Upon purification by high-performance liquid chromatography (HPLC) and characterization by electrospray ionization mass spectrometry (ESI-MS), sequence-specific oligomers are subjected to high-loading of a Lewis acidic rare-earth metal triflate which both deprotects the aldehyde moieties and affects the reactant pair equilibrium such that strands completely dissociate. Subsequently, a fraction of the Lewis acid is extracted, enabling annealing of complementary sequence-specific strands to form information-encoded molecular ladders characterized by matrix assisted laser desorption/ionization mass spectrometry (MALDI-MS). The simple procedure outlined in this report circumvents kinetic traps commonly experienced in the field of dynamic covalent assembly and serves as a platform for the future design of robust, complex architectures.

A protocol is presented for the synthesis of information-encoded peptoid oligomers and for the sequence-directed self-assembly of these peptoids into molecular ladders using amines and aldehydes as dynamic covalent reactant pairs and Lewis acidic rare-earth metal triflates as multi-role reagents.

信息承载Peptoids及其序列定向动态共价自组装的合成

This protocol presents the use of Lewis acidic multi-role reagents to circumvent kinetic trapping observed during the self-assembly of information-encoded ...