Name: visible-light induced reduction of graphene oxide using plasmonic nanoparticle
Uploaded: 2015-09-22T16:00:00.000+00:00
Duration: 7 min 24 s
Description: Watch this Scientific Journal Video about Visible-light Induced Reduction of Graphene Oxide Using Plasmonic Nanoparticle at JoVE.com

这项工作是由韩国（2013R1A1A1061387）国家研究基金会和KU-KIST的研究基金的支持。

1.准备前兆<ol><li>制备氧化石墨烯（GO）的: <ol><li> GO准备采用改良悍马的方法14 <ol><li>添加3.0的克石墨片到浓缩的 H 2的混合物中的SO 4 / H 3 PO 4（360:40毫升）中于RT。 （注:特别注意有同时使用强酸H 2 SO 4和H 3 PO 4上当。） </li><li>加入高锰酸钾 （18.0克）在搅拌下缓慢冷却，在冰浴中以维持反应混合物在&lt;35℃的温度。 （溶液变得粘稠增加反应时间，需要用适当的方法来保持高效搅拌。）（注:特别注意具有同时加入高锰酸钾 ，由于放热反应才能作出。） </li><li>搅拌12小时，在50℃，然后冷却至室温，并倾倒反应混合物在冰（400ml）中含有30％的H 2 O 2（3毫升）中。 </li><li>滤波器第r反应的影响混合物使用金属美国标准测试筛（300微米）以除去未反应的石墨和离心机滤液（4722 xg离心速度为2小时），以除去上清液。 </li><li>再次重复离心步骤用200ml水，加入200ml 30％的HCl，200ml乙醇和蒸馏水，直到溶液的pH值范围在5.0-6.0。 </li><li>冻干最终的解决方案，以生产出蓬松GO粉末。 </li><li>为了使纳米尺寸的GO溶液，溶解在40ml的三次蒸馏水（&gt; 18兆欧）20毫克的GO粉末，然后通过延长超声处理（35％振幅，500瓦，2小时）剥离，直到整个尺寸分布变得低于150纳米，那么它离心两次（10625 XG的速度，15分钟）除去沉淀物（未剥离的大型GO张）。 </li></ol></li></ol></li><li>电浆纳米粒子的制备<ol><li>金纳米粒子的制备<ol><li>柠檬酸盐稳定的球形金纳米粒子（AUN为30nm的颗粒尺寸Ps的，OD = 1.0）用于R-GO还原。 </li></ol></li><li>的AuNRs 15制备<ol><li>通过添加硼氢化钠溶液（0.01M）新鲜制备的0.6毫升的冰冷溶液成以0.25ml氯金酸4（0.01M）和9.75毫升十六烷基三溴化铵（CTAB的含水混合物溶液撰写，0.1M制备种子溶液）。 </li><li>搅拌得到的混合物剧烈0.5分钟，然后将其保持在28℃下3小时。 </li><li>通过混合475毫升的CTAB（0.1M），将3ml的AgNO 3（0.01M）和20毫升氯金酸4（0.01M）制备的生长溶液。 </li><li>再加入新鲜制备的3.2毫升抗坏血酸（0.01 M），到接着加入0.8毫升的HCl水溶液（1.0M）溶液的混合物中。 </li><li>在最后的步骤中添加3.2毫升种子溶液的生长溶液在28 °C和服从反应混合物中快速反转的几秒钟。最后，柯EP所得混合物静置至少6小时。 </li><li>分析制备AuNRs用紫外-可见光谱的吸收最大值（λmax）和 TEM分析（通常为λ最大和纵横比被认为是730纳米和3.5，分别）。 </li></ol></li><li>的AuNSs 16准备 <ol><li>制备的4-（2-羟乙基）用100mM的浓度水溶液原液-1-哌嗪乙磺酸（HEPES），并通过添加1.0M的氢氧化钠溶液将pH调节至7.4，在25℃。 </li><li>拌20个ml的磷酸盐缓冲液（100毫摩尔）用30毫升的2- [4-（2-羟乙基）-1-哌嗪基]乙磺酸（100毫摩尔）。 </li><li>然后加入500μl的金（III）三水合物（20毫米）到上述混合物中，并保持在28.5℃下，在水浴30分钟。从淡黄色溶液颜色变成蓝绿色后，可以观察到30分钟。 </li><li>离心溶液在8928×g离心速度为30分钟，并分散沉淀在蒸馏水中。 </li><li>最后，分析所制备的AuNSs用紫外-可见光谱的吸收最大值（λmax）和 TEM分析为颗粒大小确认其被发现是分别740纳米和30纳米。 </li></ol></li></ol></li></ol> 2.制备R-GO利用可见光和金纳米粒子<ol><li>加入1毫升电浆纳米颗粒率（Abs 1.0在520nm为金纳米粒子，ABS 1.0原子，分别750纳米为AuNRs和ABS 1.0在730毫微米为AuNSs）和100微升的氢氧化铵（28％，重量/体积％），以将10ml GO溶液（OD 1.0在230nm，0.125毫克毫升-1）置于装有水的循环夹套的耐热玻璃反应器中。 </li><li>通过水循环夹套照射用氙灯（1.56W¯¯cm -2的功率密度）的混合物30分钟，用水循环，以保持温度在25℃，然后离心该溶液在10625×g离心速度进行15分钟至删除金纳米粒子。 </li><li>采取包含上清液中制备的r-GO与紫外可见分光光度计分析（R-GO应显示的独特吸收带在270nm处）在200-900纳米范围内。 </li></ol> 3.目标DNA检测使用R-GO解决方案17 <ol><li>对于荧光淬灭，加入20微升10 -6 M的Cy3修饰的单链DNA（5&#39;-ATC CTT ATC AAT ATT TAA CAA TAA TCC CTC-Cy3-3&#39;）到含有25微升GO GO的或R-GO解决方案（0.125毫克毫升-1）或1955微升的0.3M PBS溶液（10mM磷酸盐缓冲液，0.3M NaCl）中的r-GO（0.125毫克毫升-1），并孵育在室温10分钟。 </li><li>测量这些样品用荧光分光光度计（λ= 前 529纳米）的荧光强度。 </li><li>对于目标检测，在三种不同浓度（10 -6 &lt;加入200微升目标寡核苷酸溶液（5&#39;-GAG GGA TTA TTG TTA AAT ATT GAT AAG GAT- 3&#39;）的/ SUP&gt;男，10 -7 M，10 -8 M）为含有20微升10 -6 M单链DNA的Cy3，25微升GO或R-GO的GO或R-GO解决方案（0.125毫克毫升-1）和1755微升0.3M的PBS的荧光恢复实验。17 注意事项: 光源及反应器 可见光（400-780 nm）的来源。可见光照射通过含有用Xe灯（1.56瓦/厘米2的功率）GO溶液的Pyrex玻璃制反应器（窗口直径为1.1厘米）。施加到反应器中的光子能量被计算为4.8×10 21光子每分钟（ 图2A-2C）。 近红外（NIR）激光。近红外激光（窗口直径= 13.2厘米）与0.36瓦/厘米2的功率密度，和808的工作波长处已被用作近红外光为GO还原反应（图2E）的来源。光子能量计算为每分钟2.43×10 21光子。 REAC器:耐热玻璃反应器（直径窗口= 1.1的厘米;反应体积= 10毫升）配备有水夹套循环同时用于可见光和NIR光照射的GO还原反应（图2F）。 </li></ol>

<ol>
	<li>Novoselov, K. 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=Electric+Field+Effect+in+Atomically+Thin+Carbon+Films.">Electric Field Effect in Atomically Thin Carbon Films.</a> Science. 306 (5696), 666-669 (2004).</li><li>Obraztsov, 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+Vapour+Deposition+Making+Graphene+on+a+Large+Scale.">Chemical Vapour Deposition Making Graphene on a Large Scale.</a> Nat Nanotechnol. 4 (4), 212-213 (2009).</li><li>Choi, W., Lahiri, I., Seelaboyina, R., Kang, Y. S. <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+Graphene+and+Its+Applications+A+Review.">Synthesis of Graphene and Its Applications A Review.</a> Crit Rev Solid State Mater Sci. 35 (1), 52-71 (2010).</li><li>Zhou, Y., 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=Microstructuring+of+Graphene+Oxide+Nanosheets+Using+Direct+Laser+Writing.">Microstructuring of Graphene Oxide Nanosheets Using Direct Laser Writing.</a> Adv Mater. 22 (1), 67-71 (2010).</li><li>Stankovich, 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=Graphene+Based+Composite+Materials.">Graphene Based Composite Materials.</a> Nature. 442 (7100), 282-286 (2006).</li><li>Becerril, H. 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=Evaluation+of+Solution-Processed+Reduced+Graphene+Oxide+Films+as+Transparent+Conductors.">Evaluation of Solution-Processed Reduced Graphene Oxide Films as Transparent Conductors.</a> ACS Nano. 2 (3), 463-470 (2008).</li><li>Wang, X., Zhi, L., M&#252;llen, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Transparent+Conductive+Graphene+Electrodes+for+Dye+Sensitized+Solar+Cells.">Transparent Conductive Graphene Electrodes for Dye Sensitized Solar Cells.</a> Nano Lett. 8 (1), 323-327 (2007).</li><li>Sungjin, P., Ruoff, R. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Chemical+Methods+for+the+Production+of+Graphenes.">Chemical Methods for the Production of Graphenes.</a> Nat Nanotechnol. 4 (4), 217-224 (2009).</li><li>Akhavan, O., Ghaderi, E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Photocatalytic+Reduction+of+Graphene+Oxide+Nanosheets+on+TiO2+Thin+Film+for+Photoinactivation+of+Bacteria+in+Solar+Light+Irradiation.">Photocatalytic Reduction of Graphene Oxide Nanosheets on TiO2 Thin Film for Photoinactivation of Bacteria in Solar Light Irradiation.</a> J Phys Chem C. 113 (47), 20214-20220 (2009).</li><li>Huang, L., 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=Pulsed+Laser+Assisted+Reduction+of+Graphene+Oxide.">Pulsed Laser Assisted Reduction of Graphene Oxide.</a> Carbon. 49 (7), 2431-2436 (2011).</li><li>Cote, L. J., Cruz-Silva, R., Huang, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Flash+Reduction+and+Patterning+of+Graphite+Oxide+and+Its+Polymer.">Flash Reduction and Patterning of Graphite Oxide and Its Polymer.</a> Composite. J. Am. Chem. Soc. 131 (31), 11027-11032 (2009).</li><li>Wu, 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=Surface+plasmon+resonance-induced+visible+light+photocatalytic+reduction+of+graphene+oxide:+Using+Ag+nanoparticles+as+a+plasmonic+photocatalyst.">Surface plasmon resonance-induced visible light photocatalytic reduction of graphene oxide: Using Ag nanoparticles as a plasmonic photocatalyst.</a> Nanoscale. 3 (5), 2142-2144 (2011).</li><li>Kumar, D., Kaur, S., Lim, D. K., 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=Plasmon-assisted+and+visible-light+induced+graphene+oxide+reduction+and+efficient+fluorescence+quenching.">Plasmon-assisted and visible-light induced graphene oxide reduction and efficient fluorescence quenching.</a> Chem. Commun. 50 (88), 13481-13484 (2014).</li><li>Gilje, 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=Photothermal+Deoxygenation+of+Graphene+Oxide+for+Patterning+and+Distributed+Ignition+Applications.">Photothermal Deoxygenation of Graphene Oxide for Patterning and Distributed Ignition Applications.</a> Adv. Mater. 22 (3), 419-423 (2010).</li><li>Cote, L. J., Kim, F., Huang, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Langmuir&#8722;Blodgett+Assembly+of+Graphite+Oxide+Single+Layers.">Langmuir&#8722;Blodgett Assembly of Graphite Oxide Single Layers.</a> J. Am. Chem. Soc. 131 (3), 1043-1049 (2008).</li><li>Ming, 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=Experimental+Evidence+of+Plasmophores:+Plasmon-Directed+Polarized+Emission+from+Gold+Nanorod&#8211;Fluorophore+Hybrid+Nanostructures.">Experimental Evidence of Plasmophores: Plasmon-Directed Polarized Emission from Gold Nanorod&#8211;Fluorophore Hybrid Nanostructures.</a> Nano Lett. 11 (6), 2296-2303 (2011).</li><li>Xie, J., Lee, J. Y., Seedless Wang, D. I. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Surfactantless,+High-Yield+Synthesis+of+Branched+Gold+Nanocrystals+in+HEPES+Buffer+Solution.">Surfactantless, High-Yield Synthesis of Branched Gold Nanocrystals in HEPES Buffer Solution.</a> Chem. Mater. 19 (11), 2823-2830 (2007).</li><li>Ferrari, A. C., Robertson, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Resonant+Raman+spectroscopy+of+disordered,+amorphous,+and+diamond+like+carbon.">Resonant Raman spectroscopy of disordered, amorphous, and diamond like carbon.</a> Phys. Rev. B. 64 (7), 075414-1-075414-13 (2000).</li><li>Tian, J., 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=One&#8211;pot+green+hydrothermal+synthesis+of+CuO&#8211;Cu2O&#8211;Cu+nanorod&#8211;decorated+reduced+graphene+oxide+composites+and+their+application+in+photocurrent+generation.">One&#8211;pot green hydrothermal synthesis of CuO&#8211;Cu2O&#8211;Cu nanorod&#8211;decorated reduced graphene oxide composites and their application in photocurrent generation.</a> Catal. Sci. Technol. 2 (11), 2227-2230 (2012).</li><li>Liu, S., Tian, J., Wang, L., Sun, X. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+method+for+the+production+of+reduced+graphene+oxide+using+benzylamine+as+a+reducing+and+stabilizing+agent+and+its+subsequent+decoration+with+Ag+nanoparticles+for+enzymeless+hydrogen+peroxide+detection.">A method for the production of reduced graphene oxide using benzylamine as a reducing and stabilizing agent and its subsequent decoration with Ag nanoparticles for enzymeless hydrogen peroxide detection.</a> CARBON. 49 (10), 3158-3164 (2011).</li><li>Tian, J., 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=Environmentally+Friendly,+One&#8211;Pot+Synthesis+of+Ag+Nanoparticle+Decorated+Reduced+Graphene+Oxide+Composites+and+Their+Application+to+Photocurrent+Generation.">Environmentally Friendly, One&#8211;Pot Synthesis of Ag Nanoparticle Decorated Reduced Graphene Oxide Composites and Their Application to Photocurrent Generation.</a> Inorg. Chem. 51 (8), 4742-4746 (2012).</li><li>Tian, J., 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=Three&#8211;Dimensional+Porous+Supramolecular+Architecture+from+Ultrathin+gC3N4+Nanosheets+and+Reduced+Graphene+Oxide:+Solution+Self-Assembly+Construction+and+Application+as+a+Highly+Efficient+Metal&#8211;Free+Electrocatalyst+for+Oxygen+Reduction+Reaction.">Three&#8211;Dimensional Porous Supramolecular Architecture from Ultrathin gC3N4 Nanosheets and Reduced Graphene Oxide: Solution Self-Assembly Construction and Application as a Highly Efficient Metal&#8211;Free Electrocatalyst for Oxygen Reduction Reaction.</a> ACS Appl. Mater. Interfaces. 6 (2), 1011-1017 (2014).</li><li>Liu, 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=Stable+Aqueous+Dispersion+of+Graphene+Nanosheets:+Noncovalent+Functionalization+by+a+Polymeric+Reducing+Agent+and+Their+Subsequent+Decoration+with+Ag+Nanoparticles+for+Enzymeless+Hydrogen+Peroxide+Detection.">Stable Aqueous Dispersion of Graphene Nanosheets: Noncovalent Functionalization by a Polymeric Reducing Agent and Their Subsequent Decoration with Ag Nanoparticles for Enzymeless Hydrogen Peroxide Detection.</a> Macromolecules. 43 (23), 10078-10083 (2010).</li><li>Li, H., 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=Photocatalytic+synthesis+of+highly+dispersed+Pd+nanoparticles+on+reduced+graphene+oxide+and+their+application+in+methanol+electro&#8211;oxidation.">Photocatalytic synthesis of highly dispersed Pd nanoparticles on reduced graphene oxide and their application in methanol electro&#8211;oxidation.</a> Catal. Sci. Technol. 2 (6), 1153-1156 (2012).</li></ol>

我们什么都没有透露。

可见光照射到30分钟与金粒子（AuNPs，AuNSs＆AuNRs）GO溶液显示从浅黄棕色至黑的颜色（ 图1）的快速颜色变化。为了获得高纯度的R-GO产品的高收益，有两个重要的因素需要遵循。一种是使用金纳米粒子作为有效的等离子体激元催化剂，因为金纳米粒子可以强烈地吸收其它结构（即，AuNRs，AuNSs）之间的可见光。另一种是利用纳米GO解决方案，以获得纳米颗粒无高纯度的R-GO产品。所...

<html>第一开发苏格兰胶带基于方法1和化学气相沉积2分别以产生石墨烯的原始状态优良的方法，但与广域表面上的大型的石墨烯合成或石墨烯层的形成已被视为一个关键限制以前的方法。对于大规模的r-GO合成将湿化学合成的方法，该方法首先需要与强氧化剂，广泛物理处理如超声处理的反应，以产生GO片，和氧功能，例如最后的减少可能的解决方案3的一个如羟基，环氧基和羰基在GO是为了恢复其原有的物理性能是必不可少的。4晴，GO为还原，进行与使用的肼或其衍生物5或通过热处理方法或者化学方法（550-1,100° C）在惰性气氛或还原气氛。6 jove_content"&gt;这些方法需要有毒的化学物质，反应时间长，高温而增加了的r-GO合成总的能源需求。7虽然光照射还原过程，如紫外线引起，8光热过程使用脉冲氙闪光，9脉冲激光辅助10和光热相机闪光灯11也有报道用于制备加热的r-GO，在通常情况下，光诱导方法转换效率低传播到利用紫外线或脉冲的激光照射，可提供高光子能量。可见光的低光子能量限制了它的使用，而不是引起了对于R-GO合成。电​​浆纳米颗粒的优异的光吸收特性中的可见和/或近红外区域可以大大改善目前的缺点12,13温和的反应条件，反应时间短，限制使用有毒通道的使用可见光为R-GO合成。emicals可以使可见光诱导等离子体辅助光催化还原GO作为一种有用的替代方法。 在本方法中，我们使用电浆纳米粒子和可见光描述了高效和简单的R-GO合成方法。反应进程被发现是强烈地依赖于电浆纳米颗粒的结构，例如球形金粒子（AuNPs），金纳米棒（AuNRs）和金纳米星（AuNSs）。使用金纳米粒子表现出最有效的减少的GO和纳米颗粒是易于拆卸和可循环用于重复使用（ 图1）。在R-GO使用可见光合成金纳米粒子表现出几乎相同的品质与相比R-GO准备知名化学法（肼）就证明了利用各种分析测量和荧光猝灭/恢复基于DNA的检测方法。

<table><tbody><tr><td>Cy3 modifeid ssDNA</td><td>IDT(Iowa, USA)</td><td></td><td>HPLC purified by IDT</td></tr><tr><td>Gold nanoparticles (30&amp;#160;nm)</td><td>Ted Pella, Inc(Redding, CA, USA).</td><td>15706-20</td><td>colloidal solution</td></tr><tr><td>4-(2-hydroxyethyl)-1-piperazineethane sulfonic acid (HEPES) (99.5%)</td><td>Sigma-Aldrich (St. Louis, MO, USA)</td><td>7365-45-9</td><td></td></tr><tr><td>Gold(III) Chloride Hydrate (99.999%)</td><td>Sigma-Aldrich (St. Louis, MO, USA)</td><td>&amp;nbsp;27988-77-8</td><td>strongly hygroscopic</td></tr><tr><td>Sodium Borohydride (99.99%)</td><td>Sigma-Aldrich (St. Louis, MO, USA)</td><td>16940-66-2</td><td></td></tr><tr><td>Hexadecyltrimethylammonium bromide (&amp;ge;99%)</td><td>Sigma-Aldrich (St. Louis, MO, USA)</td><td>57-09-0</td><td></td></tr><tr><td>L-Ascorbic Acid(&amp;ge;99.0%)</td><td>Sigma-Aldrich (St. Louis, MO, USA)</td><td>50-81-7</td><td></td></tr><tr><td>Sodium Chloride (99.5%)</td><td>Sigma-Aldrich (St. Louis, MO, USA)</td><td>7647-14-5</td><td></td></tr><tr><td>Silver Nitrate&amp;nbsp; (&amp;ge;99.0%)</td><td>Sigma-Aldrich (St. Louis, MO, USA)</td><td>7761-88-8</td><td></td></tr><tr><td>Graphite</td><td>Sigma-Aldrich (St. Louis, MO, USA)</td><td>7782-42-5</td><td></td></tr><tr><td>Sulfuric acid</td><td>Sigma-Aldrich (St. Louis, MO, USA)</td><td>7664-93-9</td><td></td></tr><tr><td>Phophoric acid</td><td>Sigma-Aldrich (St. Louis, MO, USA)</td><td>7664-38-2</td><td></td></tr><tr><td>Potassium permanganate</td><td>Sigma-Aldrich (St. Louis, MO, USA)</td><td>7722-64-7</td><td></td></tr><tr><td>Hydrogen peroxide</td><td>JUNSEI</td><td>23150-0350</td><td></td></tr><tr><td>Ammonium hydroxide</td><td>Sigma-Aldrich (St. Louis, MO, USA)</td><td>1336-21-6</td><td></td></tr><tr><td>Xe-lamp</td><td>&amp;nbsp;Cermax, Waltham, USA</td><td></td><td></td></tr><tr><td>NIR Laser</td><td>Class-IV, Sanctity Laser, Shanghai, China&amp;nbsp;</td><td></td><td>6W (output power)</td></tr><tr><td>UV-Vis spectrophotometer&amp;nbsp;</td><td>S-3100, SINCO, South Korea</td><td></td><td></td></tr><tr><td>Transmission Electron Microscopy</td><td>H-7650, Hitachi, Japan</td><td></td><td></td></tr><tr><td>Spectro Fluorometer</td><td>Jasco FP-6500, Tokyo, Japan</td><td></td><td></td></tr><tr><td>X-ray Photoelectron Spectrometer</td><td>AXIS&amp;ndash;NOVA, KRATOS Inc., UK</td><td></td><td></td></tr></tbody></table>

visible-light induced reduction of graphene oxide using plasmonic nanoparticle

目前的工作证明了简单，无化学，快速，高效节能利用可见光照射电浆纳米颗粒在室温下制造减少了石墨烯氧化物（R-GO）溶液方法。电浆纳米颗粒用于改进GO为还原效率。只需要30分钟，在RT下通过照射用氙灯的解决方案中，R-GO的解决方案可以通过简单的离心步骤完全除去金纳米颗粒而获得。球形金粒子（AuNPs）相比于其它纳米结构是最合适的电浆纳米结构物的R-GO制剂。所述还原的石墨烯氧化物制备使用可见光和金纳米粒子同样定性化学还原的石墨烯氧化物，其通过诸如UV-Vis光谱，拉曼光谱，粉末XRD和XPS各种分析技术的支持。制备的可见光减少的氧化石墨烯显示在氟优良的淬特性修改后的单链DNA和优良的荧光恢复的目标DNA检测escent分子。制备纳米金回收The-Go的r被认为是相同的质量与化学还原R-GO的。与电浆纳米粒子的使用可见光演示了R-GO合成好的替代方法。

图1示出了用于可见光和电浆纳米颗粒基的r-GO还原反应的总体方案。 图2示出了仪器设置的新的反应。反应后，需要离心步骤以除去所用的光催化剂（AuNSs，AuNRs，或金纳米粒子），如图3A所示。高分辨的分析表明，在上清液（R-GO）（图3B），这也是可能的，以确认，用紫外-可见分析，如图3C所示，吸收带从第...

Watch this Scientific Journal Video about Visible-light Induced Reduction of Graphene Oxide Using Plasmonic Nanoparticle at JoVE.com

Visible-light Induced Reduction of Graphene Oxide Using Plasmonic Nanoparticle

一个简单的协议，用于石墨烯氧化物减少使用可见光和电浆纳米粒子的制备描述。

可见光诱导的还原氧化石墨烯的使用电浆纳米粒子

Present work demonstrates the simple, chemical free, fast, and energy efficient method to produce reduced graphene oxide (r-GO) solution at RT using ...

visible-light-induced-reduction-graphene-oxide-using-plasmonic

Universidad San Sebastian

Research

JoVE Journal

Engineering

14.4K 次观看.  Korea University. 一个简单的协议，用于石墨烯氧化物减少使用可见光和电浆纳米粒子的制备描述。 

视频: Visible-light Induced Reduction of Graphene Oxide Using Plasmonic Nanoparticle

Template Directed Synthesis of Plasmonic Gold Nanotubes with Tunable IR Absorbance

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

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

的模板导演电浆黄金纳米管的合成与可调谐红外吸收

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

科研

化学

Evaluating Plasmonic Transport in Current-carrying Silver Nanowires

Plasmonics is an emerging technology capable of simultaneously transporting a plasmonic signal and an electronic signal on the same information support1,2,3. In this context, metal nanowires are especially desirable for realizing dense routing networks4. A prerequisite to operate such shared nanowire-based platform relies on our ability to electrically contact individual metal nanowires and efficiently excite surface plasmon polaritons5 in this information support. In this article, we describe a protocol to bring electrical terminals to chemically-synthesized silver nanowires6 randomly distributed on a glass substrate7. The positions of the nanowire ends with respect to predefined landmarks are precisely located using standard optical transmission microscopy before encapsulation in an electron-sensitive resist. Trenches representing the electrode layout are subsequently designed by electron-beam lithography. Metal electrodes are then fabricated by thermally evaporating a Cr/Au layer followed by a chemical lift-off. The contacted silver nanowires are finally transferred to a leakage radiation microscope for surface plasmon excitation and characterization8,9. Surface plasmons are launched in the nanowires by focusing a near infrared laser beam on a diffraction-limited spot overlapping one nanowire extremity5,9. For sufficiently large nanowires, the surface plasmon mode leaks into the glass substrate9,10. This leakage radiation is readily detected, imaged, and analyzed in the different conjugate planes in leakage radiation microscopy9,11. The electrical terminals do not affect the plasmon propagation. However, a current-induced morphological deterioration of the nanowire drastically degrades the flow of surface plasmons. The combination of surface plasmon leakage radiation microscopy with a simultaneous analysis of the nanowire electrical transport characteristics reveals the intrinsic limitations of such plasmonic circuitry.

Silver nanowires can simultaneously transport electrons and optical information in the form of surface plasmons. A procedure is described here to realize such a shared circuitry and the limitations at propagating both information carriers are evaluated.

Plasmonics is an emerging technology capable of simultaneously transporting a plasmonic signal and an electronic signal on the same information ...

工程学

Utilization of Plasmonic and Photonic Crystal Nanostructures for Enhanced Micro- and Nanoparticle Manipulation

A method to manipulate the position and orientation of submicron particles nondestructively would be an incredibly useful tool for basic biological research. Perhaps the most widely used physical force to achieve noninvasive manipulation of small particles has been dielectrophoresis(DEP).1 However, DEP on its own lacks the versatility and precision that are desired when manipulating cells since it is traditionally done with stationary electrodes. Optical tweezers, which utilize a three dimensional electromagnetic field gradient to exert forces on small particles, achieve this desired versatility and precision.2 However, a major drawback of this approach is the high radiation intensity required to achieve the necessary force to trap a particle which can damage biological samples.3 A solution that allows trapping and sorting with lower optical intensities are optoelectronic tweezers (OET) but OET's have limitations with fine manipulation of small particles; being DEP-based technology also puts constraint on the property of the solution.4,5
This video article will describe two methods that decrease the intensity of the radiation needed for optical manipulation of living cells and also describe a method for orientation control. The first method is plasmonic tweezers which use a random gold nanoparticle (AuNP) array as a substrate for the sample as shown in Figure 1. The AuNP array converts the incident photons into localized surface plasmons (LSP) which consist of resonant dipole moments that radiate and generate a patterned radiation field with a large gradient in the cell solution. Initial work on surface plasmon enhanced trapping by Righini et al and our own modeling have shown the fields generated by the plasmonic substrate reduce the initial intensity required by enhancing the gradient field that traps the particle.6,7,8 The plasmonic approach allows for fine orientation control of ellipsoidal particles and cells with low optical intensities because of more efficient optical energy conversion into mechanical energy and a dipole-dependent radiation field. These fields are shown in figure 2 and the low trapping intensities are detailed in figures 4 and 5. The main problems with plasmonic tweezers are that the LSP's generate a considerable amount of heat and the trapping is only two dimensional. This heat generates convective flows and thermophoresis which can be powerful enough to expel submicron particles from the trap.9,10 The second approach that we will describe is utilizing periodic dielectric nanostructures to scatter incident light very efficiently into diffraction modes, as shown in figure 6.11 Ideally, one would make this structure out of a dielectric material to avoid the same heating problems experienced with the plasmonic tweezers but in our approach an aluminum-coated diffraction grating is used as a one-dimensional periodic dielectric nanostructure. Although it is not a semiconductor, it did not experience significant heating and effectively trapped small particles with low trapping intensities, as shown in figure 7. Alignment of particles with the grating substrate conceptually validates the proposition that a 2-D photonic crystal could allow precise rotation of non-spherical micron sized particles.10 The efficiencies of these optical traps are increased due to the enhanced fields produced by the nanostructures described in this paper.

Plasmonic tweezers and photonic crystal nanostructures are shown to produce useful enhancements in the efficiency and orientation control of optically trapping micro- and nano-particles.

为增强微型和纳米操纵利用电浆和光子晶体纳米结构

A method to manipulate the position and orientation of submicron particles nondestructively would be an incredibly useful tool for basic biological ...

生物工程

Multifunctional Hybrid Fe2O3-Au Nanoparticles for Efficient Plasmonic Heating

One of the most widely used methods for manufacturing colloidal gold nanospherical particles involves the reduction of chloroauric acid (HAuCl4) to neutral gold Au(0) by reducing agents, such as sodium citrate or sodium borohydride. The extension of this method to decorate iron oxide or similar nanoparticles with gold nanoparticles to create multifunctional hybrid Fe2O3-Au nanoparticles is straightforward. This approach yields fairly good control over Au nanoparticle dimensions and loading onto Fe2O3. Additionally, the Au metal size, shape, and loading can easily be tuned by changing experimental parameters (e.g., reactant concentrations, reducing agents, surfactants, etc.). An advantage of this procedure is that the reaction can be done in air or water, and, in principle, is amenable to scaling up. The use of such optically tunable Fe2O3-Au nanoparticles for hyperthermia studies is an attractive option as it capitalizes on plasmonic heating of gold nanoparticles tuned to absorb light strongly in the VIS-NIR region. In addition to its plasmonic effects, nanoscale Au provides a unique surface for interesting chemistries and catalysis. The Fe2O3 material provides additional functionality due to its magnetic property. For example, an external magnetic field could be used to collect and recycle the hybrid Fe2O3-Au nanoparticles after a catalytic experiment, or alternatively, the magnetic Fe2O3 can be used for hyperthermia studies through magnetic heat induction. The photothermal experiment described in this report measures bulk temperature change and nanoparticle solution mass loss as functions of time using infrared thermocouples and a balance, respectively. The ease of sample preparation and the use of readily available equipment are distinct advantages of this technique. A caveat is that these photothermal measurements assess the bulk solution temperature and not the surface of the nanoparticle where the heat is transduced and the temperature is likely to be higher.

Multifunctional Hybrid Fe2O3-Au Nanoparticles for Efficient Plasmonic Heating

We describe the synthesis and properties of multifunctional Fe2O3-Au nanoparticles produced by a wet chemical approach and investigate their photothermal properties using laser irradiation. The composite Fe2O3-Au nanoparticles retain the properties of both materials, creating a multifunctional structure with excellent magnetic and plasmonic properties.

多功能混合铁<sub&gt; 2</sub&gt; 0<sub&gt; 3</sub&gt; -Au纳米粒子高效的电浆暖气

One of the most widely used methods for manufacturing colloidal gold nanospherical particles involves the reduction of chloroauric acid (HAuCl4) to ...

In Situ Synthesis of Gold Nanoparticles without Aggregation in the Interlayer Space of Layered Titanate Transparent Films

Combinations of metal oxide semiconductors and gold nanoparticles (AuNPs) have been investigated as new types of materials. The in situ synthesis of AuNPs within the interlayer space of semiconducting layered titania nanosheet (TNS) films was investigated here. Two types of intermediate films (i.e., TNS films containing methyl viologen (TNS/MV2+) and 2-ammoniumethanethiol (TNS/2-AET+)) were prepared. The two intermediate films were soaked in an aqueous tetrachloroauric(III) acid (HAuCl4) solution, whereby considerable amounts of Au(III) species were accommodated within the interlayer spaces of the TNS films. The two types of obtained films were then soaked in an aqueous sodium tetrahydroborate (NaBH4) solution, whereupon the color of the films immediately changed from colorless to purple, suggesting the formation of AuNPs within the TNS interlayer. When only TNS/MV2+ was used as the intermediate film, the color of the film gradually changed from metallic purple to dusty purple within 30 min, suggesting that aggregation of AuNPs had occurred. In contrast, this color change was suppressed by using the TNS/2-AET+ intermediate film, and the AuNPs were stabilized for over 4 months, as evidenced by the characteristic extinction (absorption and scattering) band from the AuNPs.

In Situ Synthesis of Gold Nanoparticles without Aggregation in the Interlayer Space of Layered Titanate Transparent Films

Here, we present a protocol for the in situ synthesis of gold nanoparticles (AuNPs) within the interlayer space of layered titanate films without the aggregation of AuNPs. No spectral change was observed even after 4 months. The synthesized material has expected applications in catalysis, photo-catalysis, and the development of cost-effective plasmonic devices.

在没有聚集的层状钛酸盐薄膜透明的层间金纳米粒子的原位合成

Combinations of metal oxide semiconductors and gold nanoparticles (AuNPs) have been investigated as new types of materials. The in situ synthesis of AuNPs ...

Fabrication of Periodic Gold Nanocup Arrays Using Colloidal Lithography

Within recent years, the field of plasmonics has exploded as researchers have demonstrated exciting applications related to chemical and optical sensing in combination with new nanofabrication techniques. A plasmon is a quantum of charge density oscillation that lends nanoscale metals such as gold and silver unique optical properties. In particular, gold and silver nanoparticles exhibit localized surface plasmon resonances-collective charge density oscillations on the surface of the nanoparticle-in the visible spectrum. Here, we focus on the fabrication of periodic arrays of anisotropic plasmonic nanostructures. These half-shell (or nanocup) structures can exhibit additional unique light-bending and polarization-dependent optical properties that simple isotropic nanostructures cannot. Researchers are interested in the fabrication of periodic arrays of nanocups for a wide variety of applications such as low-cost optical devices, surface-enhanced Raman scattering, and tamper indication. We present a scalable technique based on colloidal lithography in which it is possible to easily fabricate large periodic arrays of nanocups using spin-coating and self-assembled commercially available polymeric nanospheres. Electron microscopy and optical spectroscopy from the visible to near-infrared (near-IR) was performed to confirm successful nanocup fabrication. We conclude with a demonstration of the transfer of nanocups to a flexible, conformal adhesive film.

We demonstrate the fabrication of periodic gold nanocup arrays using colloidal lithographic techniques and discuss the importance of nanoplasmonic films.

用胶体光刻制备周期性金 Nanocup 阵列

Within recent years, the field of plasmonics has exploded as researchers have demonstrated exciting applications related to chemical and optical sensing ...

Determination of the Excitation and Coupling Rates Between Light Emitters and Surface Plasmon Polaritons

We have developed a unique method to measure the excitation and coupling rates between the light emitters and surface plasmon polaritons (SPPs) arising from metallic periodic arrays without involving time-resolved techniques. We have formulated the rates by quantities that can be measured by simple optical measurements. The instrumentation based on angle- and polarization-resolved reflectivity and photoluminescence spectroscopy will be described in detail here. Our approach is intriguing due to its simplicity, which requires routine optics and several mechanical stages, and thus is highly affordable to most of the research laboratories.

This protocol describes the instrumentation for determining the excitation and coupling rates between light emitters and Bloch-like surface plasmon polaritons arising from periodic arrays.

光发射器与表面等离子体极化激元的激发和耦合速率的测定

We have developed a unique method to measure the excitation and coupling rates between the light emitters and surface plasmon polaritons (SPPs) arising ...

Performing Spectroscopy on Plasmonic Nanoparticles with Transmission-Based Nomarski-Type Differential Interference Contrast Microscopy

Differential interference contrast (DIC) microscopy is a powerful imaging tool that is most commonly employed for imaging microscale objects using visible-range light. The purpose of this protocol is to detail a proven method for preparing plasmonic nanoparticle samples and performing single particle spectroscopy on them with DIC microscopy. Several important steps must be followed carefully in order to perform repeatable spectroscopy experiments. First, landmarks can be etched into the sample substrate, which aids in locating the sample surface and in tracking the region of interest during experiments. Next, the substrate must be properly cleaned of debris and contaminants that can otherwise hinder or obscure examination of the sample. Once a sample is properly prepared, the optical path of the microscope must be aligned, using Kohler Illumination. With a standard Nomarski style DIC microscope, rotation of the sample may be necessary, particularly when the plasmonic nanoparticles exhibit orientation-dependent optical properties. Because DIC microscopy has two inherent orthogonal polarization fields, the wavelength-dependent DIC contrast pattern reveals the orientation of rod-shaped plasmonic nanoparticles. Finally, data acquisition and data analyses must be carefully performed. It is common to represent DIC-based spectroscopy data as a contrast value, but it is also possible to present it as intensity data. In this demonstration of DIC for single particle spectroscopy, the focus is on spherical and rod-shaped gold nanoparticles.

The goal of this protocol is to detail a proven approach for the preparation of plasmonic nanoparticle samples and for performing single particle spectroscopy on them with differential interference contrast (DIC) microscopy.

基于传输的野武学型差分干涉对比显微镜对等离子体纳米粒子的光谱处理

Differential interference contrast (DIC) microscopy is a powerful imaging tool that is most commonly employed for imaging microscale objects using ...

Photodeposition of Pd onto Colloidal Au Nanorods by Surface Plasmon Excitation

A protocol is described to photocatalytically guide Pd deposition onto Au nanorods (AuNR) using surface plasmon resonance (SPR). Excited plasmonic hot electrons upon SPR irradiation drive reductive deposition of Pd on colloidal AuNR in the presence of [PdCl4]2-. Plasmon-driven reduction of secondary metals potentiates covalent, sub-wavelength deposition at targeted locations coinciding with electric field &#8220;hot-spots&#8221; of the plasmonic substrate using an external field (e.g., laser). The process described herein details a solution-phase deposition of a catalytically-active noble metal (Pd) from a transition metal halide salt (H2PdCl4) onto aqueously-suspended, anisotropic plasmonic structures (AuNR). The solution-phase process is amenable to making other bimetallic architectures. Transmission UV-vis monitoring of the photochemical reaction, coupled with ex situ XPS and statistical TEM analysis, provide immediate experimental feedback to evaluate properties of the bimetallic structures as they evolve during the photocatalytic reaction. Resonant plasmon irradiation of AuNR in the presence of [PdCl4]2- creates a thin, covalently-bound Pd0 shell without any significant dampening effect on its plasmonic behavior in this representative experiment/batch. Overall, plasmonic photodeposition offers an alternative route for high-volume, economical synthesis of optoelectronic materials with sub-5 nm features (e.g., heterometallic photocatalysts or optoelectronic interconnects).

A protocol for anisotropic photodeposition of Pd onto aqueously-suspended Au nanorods via localized surface plasmon excitation is presented.

通过表面等离子体激发将 Pd 光沉积到胶体 Au 纳米棒上

A protocol is described to photocatalytically guide Pd deposition onto Au nanorods (AuNR) using surface plasmon resonance (SPR). Excited plasmonic hot ...

Graphene-Assisted Quasi-van der Waals Epitaxy of AlN Film on Nano-Patterned Sapphire Substrate for Ultraviolet Light Emitting Diodes

This protocol demonstrates a method for graphene-assisted quick growth and coalescence of AlN on nano-pattened sapphire substrate (NPSS). Graphene layers are directly grown on NPSS using catalyst-free atmospheric-pressure chemical vapor deposition (APCVD). By applying nitrogen reactive ion etching (RIE) plasma treatment, defects are introduced into the graphene film to enhance chemical reactivity. During metal-organic chemical vapor deposition (MOCVD) growth of AlN, this N-plasma treated graphene buffer enables AlN quick growth, and coalescence on NPSS is confirmed by cross-sectional scanning electron microscopy (SEM). The high quality of AlN on graphene-NPSS is then evaluated by X-ray rocking curves (XRCs) with narrow (0002) and (10-12) full width at half-maximum (FWHM) as 267.2 arcsec and 503.4 arcsec, respectively. Compared to bare NPSS, AlN growth on graphene-NPSS shows significant reduction of residual stress from 0.87 GPa to 0.25 Gpa, based on Raman measurements. Followed by AlGaN multiple quantum wells (MQWS) growth on graphene-NPSS, AlGaN-based deep ultraviolet light-emitting-diodes (DUV LEDs) are fabricated. The fabricated DUV-LEDs also demonstrate obvious, enhanced luminescence performance. This work provides a new solution for the growth of high quality AlN and fabrication of high performance DUV-LEDs using a shorter process and less costs.

A protocol for graphene-assisted growth of high-quality AlN films on nano-patterned sapphire substrate is presented.

紫外发光二极管纳米图案蓝宝石基板的AlN薄膜的石墨烯辅助准范德瓦尔斯皮Taxy

This protocol demonstrates a method for graphene-assisted quick growth and coalescence of AlN on nano-pattened sapphire substrate (NPSS). Graphene layers ...