The authors acknowledge financial support from the Engineering and Physical Sciences Research Council, UK under the Program Grant 'Supercritical Fluid Electrodeposition' (EP/J016276/1). J.S. and R.J.K. are indebted to the Warwick Centre for Analytical Science (EPSRC funded Grant EP/F034210/1). Additionally, we are indebted to Drs. Zheng Liu and Kazu Suenaga who provided the top right part of Panel d of Figure 1, which originally appeared in Microsc. Semicond. Mater. 2008, 120, 213-216 (used with permission).

1.样品制备:单壁碳纳米管的熔体充实的碲化汞（HGTE）和其他材料注意:在本协议中使用的一些化学物质会危害健康。请咨询相关的材料安全数据表的任何化学反应发生之前。利用适当的个人防护装备（实验室外套，护目镜等 ）和工程控制（ 如手套箱，通风柜等 ）处理碳纳米管和碲化汞的时候。 <ol><li>预热〜50毫克的单壁碳纳米管〜400℃在干燥空气或500℃真空 。 注意:如果使用干燥的空气，可以存在的单壁碳纳米管的量的一些损失，典型地20-40％。之前以这种方式填充的单壁碳纳米管的预热已报道提高填充有分子或晶体12的单壁碳纳米管的比例。 </li><li>在氩手套箱碾〜20毫克预热的单壁碳纳米管26与等体积的填充材料（在这种情况下，汞德lluride），用于使用玛瑙研钵和研杵，将力施加到产生的紧密混合物&gt; 20分钟。 </li><li>同时仍然在手套箱中，单壁碳纳米管的/全部量的填充材料的混合物转移到一个8-10毫米（内径），在一端密封，并开在其另一6-10厘米长的二氧化硅石英安瓿中。 注:滤纸的漏斗是1.3有用的。不要使用普通的实验室玻璃安瓿瓶作为本级玻璃可能熔化并损坏炉。 </li><li>内手套箱临时密封与转移到真空管线的塑料薄膜的安瓿的开口端。一旦它被固定到真空管线取出胶片。 </li></ol> 2.疏散和填充步骤<ol><li>密封安瓿含有单壁碳纳米管/真空适中（一般0.1〜帕）下填充复合材料。 </li><li>在可编程管或马弗炉，加热该密封的安瓿在〜5℃分钟-1至〜100℃&gt;熔化填充的点（MP）的升温速率在为+/- 100℃的温度下进行48小时的总时间12小时期间用热循环ING。 </li><li>冷却在炉至室温安瓿的速率不超过5℃分钟更大-1之前破开和存储。 危害:砸开安瓿可能会导致割伤或可破灭，呈现出显著的眼睛影响的危险。眼睛防护和安全手套在操作过程中佩戴。安瓿可通过第一得分在用玻璃划线中心安全地打破了安瓿，然后在此位置通过在硬布包裹破，然后同时施加弯曲压力的得分点的任一侧。 </li></ol> 3.样本清洁<ol><li>浓HCl和HNO 3（总体积50ml）中的〜1小时1混合物:由以1轻轻回流除去样品中的外部化合物的单壁碳纳米管。 </li><li>使用可控孔径f。洗涤用去离子水和过滤器的样品ILTER具有〜0.22微米的孔尺寸。 </li></ol> 4.高分辨透射电镜分析样品（HRTEM） <ol><li>以750瓦在2秒的尖端超声波仪功率的大约20％的分散开/关脉冲在〜5毫升用声处理乙醇〜5毫克的样品。 </li><li>将分散的1-2滴上3.05毫米花边涂碳高分辨透射电子显微镜标本电网。 </li><li>在80千伏像差校正的HRTEM执行HRTEM 27,29成像和装有4,008点¯x2672像素的电荷耦合器件（CCD）。 </li><li> Precalibrate CCD的在相同的放大倍数也可以用于使用分散金纳米粒子的（111）晶格面（由0.235毫微米分隔）成像纳米线/碳纳米管复合材料。 </li><li>在至少60万次和最佳施科泽散焦成像条件下的倍率得到的离散填充SWNT样品的图像。 </li><li>确认通过能量分散型X射线显微馅料的组合物（EDX） <sup&gt; 28,29理想地使用相同的HRTEM作为用于成像。使用聚焦在单壁碳纳米管填充包了〜1纳米电子探针。 </li></ol> 5.确认单壁碳纳米管的嵌入式至尊纳米线由高分辨图像模拟的微观结构注:对于图像的模拟标准多层图像仿真包，如SimulaTEM可用于产生可直接比较的位图图像（* .BMP）模拟。有关通过各种平台的软件操作具体细节，请按照制造商的协议。 <ol><li>选择无漂移，并与沿〜5纳米的单壁碳纳米管的距离清晰可见解决原子列的纳米线的高分辨图像。纳米线/纳米管复合材料的长轴应正交相对于所述电子束。 </li><li>通过使用校准图像（步骤4.4）直接绘制原子的位置上原子列的一个高晶体对称性S上的情况下，产生原子坐标。8tructure;单个图像需要11。加在突起2-3原子层到模型以完成结构。为一个低对称模型，从两个或多个在两个单独的纳米管10的两个或更多晶体相同片段的不同突起解决的晶体结构。 </li><li>生成名为* .xyz碳纳米管坐标使用根据关系确定的合适的程序（ 例如 TubeGen 3.4）适当直径的纳米管。 <img alt="式（1）" src="/files/ftp_upload/53434/53434eq1.jpg" /> 其中d是直径， 一个是CC键距（0.246纳米），n和m管构象。纳米管应该足够容纳从步骤5.2考虑到纳米管的壁（0.17纳米）的碳原子的范德华半径产生的晶体的外部体积大。 </li><li>从纳米线/纳米管compos组装复合原子坐标伊特使用使得1D晶体插入并沿纳米管的公共中心轴线对齐，然后保存在* .xyx或*的.pdb格式最终模型坐标一个合适的结构处理程序（ 例如 CrystalMaker软件）。 </li><li>生产使用使用5.3产生的原子坐标标准多层模拟协议（ 如 SimulaTEM）纳米线/碳纳米管复合材料的图像模拟。 </li><li>模拟的初步定向的复合物，使得该复合材料的长轴垂直于电子束。使用模拟参数与加速电压一致（ 如 80千伏）和球面像差系数（CS; 例如 0.001毫米）用高分辨仪器一致。 </li><li>目测比较仿真的图像的外观。如果未获得良好的视觉匹配通过合适的间隔（ 例如绕极端纳米线/纳米管复合材料的长轴片段。克10°），然后重新模拟。重复此步骤为复合的完整180°旋转。 </li><li>如果怀疑该实验成像片段相对于倾斜的理想正交取向，重复步骤5.5至5.7为±10°的倾斜，直到获得良好的匹配。 </li></ol> 6.样品制备适合于拉曼光谱危险:纳米管溶液的超声处理可能能够形成含有管或填充管的气雾剂和如果样品随后不正确地处理可能会导致在纳米管或填充碳纳米管操作呼吸。 <ol><li>放置20毫克碳纳米管产物到小瓶，加入20毫升乙醇中并密封盖子。 </li><li>在槽式声波和超声药瓶放置在20瓦的约20分钟，直到液体变黑。离开〜5小时，使纳米管小瓶解决了雾化。 </li><li>轻轻旋转小瓶如果存在鼓动下悬挂。 </l我&gt; <li>使用移液管，滴涂层10-20微升悬浮液的上氧化物涂覆的硅基片（5毫米×10毫米），并允许乙醇蒸发。 </li></ol> 7.安装在样品低温恒温器<ol><li>放置在低温恒温器冷指金属导电漆（约2 平方毫米）的液滴，并轻轻地放在硅样品上滴漆，让干〜2小时。 </li><li>低温恒温器密封按照制造商的协议和螺栓低温恒温器到XYZ阶段，并使用无油泵泵低温恒温器，以10-6毫巴。 </li></ol> 8.初始设置和拉曼系统优化注:请参考阅读该协议的以下部分之前在图10中呈现的实验原理图。 <ol><li>采用可调谐激光光源根据制造商的协议集入射光波长为需要的值（ 如 800纳米）。 </li><li>调整激光预过滤器（C 如图10 </strong&gt;）按照生产商的方案，通过过滤器，以最大限度地提高激光功率的传输。如果使用批量布拉格光栅（VBG）修改光设立按照图10并使用以下子过程。 <ol><li>旋转VBG围绕垂直轴通过VBG减少激光的发射。微调使用VBG镜子坐骑。 </li><li>镜子的位置进入布拉格反射光束和逆向反射光束返回到VBG。调整镜子通过VBG打压回射光束的传输。 </li><li>通过测量虹膜1发射激光功率和微调VBG和后向反射镜以最大限度地提高激光能量的传输。 </li></ol></li><li>调整后的过滤器（C）的反射镜（M1和M2）通过重新定位来自相关分束器（BP1和BP2）反射到两个梁观测摄像机（C1和C2），以激光束返回到预定路径。 </li><li>通过间接散射光谱仪将激光测量光子能量。 ðO不可直接散射光进入光谱仪，因为这可能会损坏敏感光谱相机。 </li><li>调整半波片（HWP1）设置电源事件在客观（和PM2）以约1毫瓦。 </li><li>使用光学成像（ 图10:蓝色虚线），检查样本图像，并确保激光点是在没有stigmation所需位置（8.3优化如果有）。 注:接下来的10个步骤最初用于保证激光有效地耦合到光谱仪。一旦完成这些步骤并不需要重复，直到显著的变化在光学装置进行。 </li><li>调整样品位置按8.6使激光点集中在硅的洁净区。 </li><li>设置谱仪零级，并使用内置的光谱仪（ 图10 E成分），观察摄像头查看光谱仪的第一阶段，输入狭缝的图像（狭缝1）。 </li><li>开槽1，检查，使用上述观察相机，该refle从样品反恐执行局的激光狭缝进入。 </li><li>通过调整耦合透镜（L3）确保中心激光点输入狭缝水平和垂直方向上的摄像头。 </li><li>反复减少狭缝宽度1，重复8.10，以确保正确的激光集中在狭缝1和照相机。在此过程中调整聚焦耦合透镜的以最小化从狭缝1的激光的散射确保反射的激光光在狭缝1的平面大致聚焦。 </li><li>开缝1，使得反射的激光光不显著由狭缝1裁剪。 </li><li>设置光谱仪软件，根据制造商的协议，收集拉曼520 -1硅拉曼散射的峰值。 </li><li>将电源设置为10毫瓦。 </li><li>以反复拉曼光谱一个秒曝光开始聚焦。 </li><li>调整样本的Z-焦点，直到定义良好的520厘米-1硅峰观察。 </li><li>通过调节输入半波片最大化这个信号（HWP2）（这将取决于传出共振的偏振并在分光计的光栅），输入透镜和样品中的Z-焦点。 </li></ol> 9.单个拉曼光谱的测量<ol><li>设定所需温度（4 K），并允许系统平衡（〜40分钟）。 </li><li>在PM2到〜2 MW机组入射激光的功率。 </li><li>上设置分光计软件波长在步骤8.4确定。 </li><li>坐落于光谱仪的软件中心转移至0厘米-1，并获得一个短（500毫秒），拉曼光谱测量激光线。 </li><li>使用价值在9.4确定了光谱仪软件设置新的，更精确的波长。 </li><li>在软件中设定中心偏移和频谱窗口来观察预测拉曼模式，从而使光谱窗口不包括激光线尾。 </li><li>移动样品位置感兴趣的区域（用于捆绑管的样品位置的选择是非常重要的，详情见第14条）。 </li> &lt;LI&gt;获取拉曼光谱采用CCD重点1秒曝光根据制造商的协议。 </li><li>调整使用阶段控制器以最大化在功率计（PM1）的反射功率样本的Z聚焦位置。 </li><li>使用合适的曝光时间来获得足够的信号（&gt; 1,000计数绝对）获得的拉曼光谱。 </li></ol> 10.拉曼截面激光功率依赖性的测量方法<ol><li>设置激光波长为在工作温度下的特定样品的共鸣估计的峰值。 </li><li>设置一个低功率（〜0.1毫瓦），并获得拉曼光谱按本协议第9.3-9.10。 </li><li>增加功率（由〜0.1毫瓦），确保作为HWP1转动样品激光光斑不移位。如果HWP1的旋转激光光斑位移然后重新调整为每8.3，以确保不会发生这种情况，并重新开始实验。 </li><li>重复10.3多达约5兆瓦合适的范围内的权力。重复此PROCES是对每一个工作温度。 </li><li>积的观察拉曼特征与激光功率拟合强度并确定线性区域。在该温度下执行所有后续的共振拉曼实验与线性区域的功率上限的80％。 </li></ol>拉曼截面激光能源的依赖11.测量<ol><li>将所需的激发波长（ 如 700纳米）和调整系统按照第8.1-8.6，入射功率设定为从第10条确定。 </li><li>通过调节样品的Z聚焦最大化反射功率并以检查的主要拉曼特征的强度连续采集1秒的曝光。 </li><li>设置曝光时间和积累对CCD信号的最大化，而不饱和探测器。 </li><li>减谱注意到在文件名中使用的光栅，曝光时间，累积，中心拉曼位移，激发能量和入射功率。 </li><li>接着设置EXC通过重复步骤8.1-8.6确保入射激光功率itation波长是恒定的，然后最大化反射功率按照步骤11.2。对于初次使用的结果激发波长的激光相隔约10纳米。对于约2纳米的外观质量效果的激光波长分离是可取的。 </li><li>在每次六个新的激发波长回到一个先前的激发波长（ 如 700纳米），重复11.1-11.5。从重复光谱绘制一个密钥的拉曼特征的拟合强度作为实验时间的函数，并确保没有长期漂移。 </li></ol> 12.拉曼光谱的偏振相关的测量<ol><li>放置的偏振分析仪（POL2）到物镜和分光计之间的路径， 如图10（紫色虚线）。此外放置一个半波片和偏振器（HWP3和POL3）插入之前的物镜的光路;这将被用于旋转入射偏振。确保所有的偏振器和HWPS正确对齐，所以入射辐射垂直于光轴并通过光学器件的中心行进。 </li><li>调整POL3通过垂直偏振光。使用强拉曼信号， 如一块裸硅，调整（POL 2）通过垂直偏振光和调整HWP2最大化拉曼信号强度。注意HWP2的旋转和光进入光谱仪的偏振方向。确保在实验的其余部分，在实验的光入射的偏振是通过调整HWP2以补偿在偏振分析器传递方向的任何变化不变。 </li><li>检查检偏器的排列;旋转偏振器180°，以确保信号仍然是相同的。 </li><li>执行步骤12.3的HWP（旋转它在90°左右其完整的革命）。 </LI&gt; <li>注意在每一步中的信号是否有任何变化。 </li><li>通过调节Z-焦点最大化反射功率和使用适当的输入功率和曝光时间/积累获得拉曼光谱。 </li><li>调整采集偏振片与适当的间距（10°）和以上述方式调整HWP在12.2讨论，以保持在光谱仪恒定的光入射的偏振。 </li><li>重复步骤12.7直至全方位偏振片的已经测量。 </li><li>入射的光的偏振改变到目标到水平。 </li><li>检查此并没有引起激光点到样品上移动。重复步骤12.7和12.8的测量。也可使用其他入射偏振但至少有两个，垂直极化是必需的。如果使用POL3和上的光的偏振的目标之间的光学元件的非水平或垂直偏振光的效果需要考虑的体贴离子。 </li><li>检查该预期1D对象的合奏来确定哪些拉曼特征与封装的纳米线（见代表结果）相关联的偏振波依赖性。 </li></ol> 13.拉曼光谱的温度依赖性的测量<ol><li>将按照制造商的协议低温恒温器控制器上新的样品温度。 </li><li>通过观察低温恒温器的温度和样品的移动确保了低温恒温器是在热平衡并有继续之前没有样品的移动。 </li><li>通过观察在低温恒温器样品使用和不使用激光照射校正样品位置的任何热漂移。 </li><li>确保激光功率在下面从第10步线性制度。 </li><li>测量拉曼截面的激光能源的依赖在部分10是用于样品的光学共振共同随温度到移位虽然ö随温度FTEN的谐振变化的能量相对缓慢。 </li></ol>样品部位的选择14 <ol><li>安装样品之后，发现在样品的明显位置， 例如 ，一个角，并注意低温恒温器的翻译阶段的位置，通过在如由蓝色虚线在图10中所示的组分中加入。 </li><li>移动到另一个位置明显， 例如沿边缘之一，并注意其位置。 注:学习充满碳纳米管合奏时，样品的位置是非常重要的。它很可能是该样本将是不均匀的。样品上的有利地位具有以下特点。 </li><li>发现通过微米尺度的细节在显微镜允许你确实返回到其位置观察时在视觉上明​​显的位置。 </li><li>从样品测量的拉曼信号，并稍微调整XY位置，检查区域的同质性在几微米小号卡尔。如果信号变化显著选择不同的位置。 </li><li>捕捉点的图像，并注意从样品角的相对坐标，以便能够恢复到样品。 </li></ol> 15.数据后处理<ol><li>导入到的光谱数据处理软件。 </li><li>规范化每个光谱相对于激光功率和照射时间来获得每兆瓦每秒计数。 </li><li>正确的光谱效率。 注:某些光谱仪软件自动执行此操作，但是，如果没有，则按照下面的步骤。步骤15.3.1-15.3.2可为任何特定的光谱仪进行一次再后来根据需要使用。 <ol><li>放置一个校准白色光源在样品的位置，并测量其光谱与光谱仪的所有标准设置。 </li><li>划分为白色光源，以获得可以通过光谱仪的校准曲线的白色光光谱。存储吞吐量文件供以后使用。 </li><li>由可以通过在相同条件下的频谱除以所测量的拉曼光谱。 </li></ol></li><li>使用适当的数据处理软件绘制的拉曼光谱。 </li><li>检查光谱谱中能量的激光跳跃的证据。这将产生更广泛的峰或峰在频谱加倍了。 </li><li>通过检查一个已知的拉曼特征， 例如硅的LO（纵光学）声子，或检查的突然变化在所有的拉曼的移位相同的量提供在相关光谱查询的拉曼位移校正。 </li><li>适合使用标准线的形状和非线性弯曲拟合程序以获得用于所有功能的振幅，中心偏移和宽度的拉曼特征。 </li><li>绘制拟合参数对激光能量和温度的要求。 </li></ol>

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The authors have nothing to disclose.

而一个大量的研究已在纳米线所做的最小直径的基本的限制纳米线可能，极端的纳米线，也几乎没有被研究。它已经表明，这些纳米线的特性不会形成具有稍微更大直径的纳米线的连续; 例如，它们可以显示出它们的亲本材料的完全新的晶体形式。考虑到大量的可能亲本材料，并且每个父母可以产生许多多于一个极端纳米线可能纳米线的范围物理学是巨大的。 极端纳米线的研究还处于初期阶段，这一事实是不是因为生产它们的方法是没有很好地建立。载于本文的熔渗过程是可靠的，并已被许多团体和其他方法，如升华馅都可以，如果熔渗不适于任何特定的填充。在部分字段由缺乏非破坏性地表征极端的纳米线的相对简单和广泛适用的方法的阻碍。如果碳纳米管的场是任何指导，拉曼光谱具有作为选择的解决该问题的方法的好机会。在极端的纳米线获得有用的拉曼光谱，关键是要认识到，在共同与拉曼散射的所有其它1D系统的谐振增强是用于观察任何散射的必要条件。一旦特定样品类型的全共振行为已经使用载于该协议，可以使用拉曼大多数应用的固定共振激发能量来表征，这将加快测量样品和降低成本的方法测定拉曼系统的需要。 正如在本文介绍的结果显示在极端纳米线获得高品质的共振拉曼结果的关键问题是需要能够可重复地重新调整可调谐激光器的光束数天以高精度。这需要特定的修改的实验系统，并注意在实验的最重要的细节;正确聚焦光学系统，激光束到所述显微镜物镜和精确地校正该样品的任何横向移动的能力的精确对准。技术开发，实现这种形式本文的基础。他人已经开发的技术和系统用于改进的谐振拉曼实验，包括先驱如分枝卡多纳谁施加的技术范围广的体积和量子阱系统的再现性。我们的技术也是建立在拉曼碳纳米管的先驱，包括M. Dresselhaus 21的工作。然而这里提出的协议，特别适合于在极端的纳米线共振拉曼实验。 在S的一个关键部分该协议的uccess在图10所示的实验系统的开发。该图演示了在协议中详述的拉曼实验中使用的光学装置的平面图。激光通过在样品一50X物镜（标记OB），在低温恒温器密封按照协议聚焦。此低温恒温器被安装在XYZ载物台以允许样品的3维运动重新定位和聚焦的目的。激光通过A和B（作为一个泵浦源和Ti:分别蓝宝石）产生，所提供的材料的文件中被提到的激光的具体细节。当使用商用激光线路滤波器（C成分）激光通过虹膜1和2和准直用透镜1和2（L1和L2）的中心定向。光穿过一个半波片和偏振器（HWP1和POL1）在PM2来控制偏振和激光功率入射的平面，如在协议详述。激光通过通过可调谐滤波器，C和利用反射镜M1和M2，转向到正确光路，使得其垂直于目标（OB）的背面，并集中在摄像机C1和C2。 ND滤光片是用于背反射光束从物镜到功率计，PM1位置，以允许进行聚焦过程（步骤9.9）。从样品背散射光被收集，并通过透镜3（L3）和狭缝1传递到光谱仪。调整透镜的狭缝宽度和位置是很重要的，以最大化拉曼信号，如在协议部分8详述如果激光波长是出了激光线的过滤器操作范围内时，体积布拉格设置需要被用作每8.2节.1-8.2.3。重要的是，该光学组向上是根据黑色虚线按照图10改变，并且反射镜M3被从路径中移除。最后，如​​果进行偏振依赖性的实验中，这是重要的控制偏振并保持进入分光计偏振，这是在协议和部件的部分12说明被添加到设置由紫色虚线在图10中突出显示。蓝色如图10虚线所示是部件加入，以允许样品的实时成像由协议的部分14所指示的。 如同所有的实验方法共振拉曼散射有其局限性。具体地，可用的可调谐激光源和检测器意味着它更容易在光谱范围内350-1,000纳米虽然分机进一步执行到红外线和紫外线是可能的。具有可调源进行拉曼散射所需要的实验系统并不便宜有一个合理的估计在出版时间为£200-300k。此外，所需要的系统的复杂性意味着它们需要一定的了解光学光谱成功运行。然而拉曼散射提供的信息的组合，是很难从其它技术获得。值得注意的是它有可能获得拉曼散射，并且因此振动能，从可以尚未通过任何其它技术来实现各单壁碳纳米管。 现在，纳米线的谐振开始被确定这开辟了一个范围拉曼散射的可能扩展。在我们看来，扩展到电化学门极端纳米线20的温度下降到4 KB 36，允许在纳米线测量在很宽的范围内的电荷密度将是关键理解这些材料。最后用拉曼散射对理解极端纳米线的结构和熔化转变可能有助于优化可进一步产生的样品的质量。

拉曼光谱和共振拉曼光谱是广泛和科技开发成熟的技术。虽然第一拉曼本人于1928年1中报告的关键广泛使用拉曼光谱是激光，在共振拉曼的情况下可调谐激光器，以提供高强度，窄带宽激发源的发展。本文阐述了为什么共振拉曼散射是直径〜1-5原子的调查基础物理和一般和极端的纳米线的一维表征系统的样本， 如纳米线一个特别重要的方法。它还讨论特别这种纳米线的拉曼光谱和一个协议，允许这些被克服，从而实现在这些系统中的拉曼散射效率的激光能源的依赖高重复性的测量困难。 有一个广泛的EXTEnded，结晶维量子系统，也被称为纳米线，可供学习和应用。这些包括蒸气-液体-固体生长的半导体纳米线2，光刻限定纳米线3，阳极氧化铝和跟踪蚀刻膜模板纳米线4等。在这些系统中的利益的一个关键原因是，他们结合了沿着结构自由移动的能力，电子和其他大型激发量子限制效应。在某些方面的纳米线是从它们的母体材料， 例如降低电磁屏蔽相当不同，由于自由电荷5，并在某些情况下，减少了电子散射导致弹道输运6。然而，在许多方面，纳米线仍然批量等， 如局部粘合和晶体结构，以及几乎总是的电子波函数在原子尺度的基本质量仅弱改性散装比较，以便该包络近似7是有效的。然而，由于该密闭方向的尺寸减小到几个原子，可发生形成以前从未见过同素异形体8-10与全新的粘接纳米线。这些纳米线在两种意义上的极端;它们是在截面11-13的可能降低的极限，他们有极端属性10,13,14。 进行共振拉曼光谱之前，有必要以产生极端的纳米线的样品。列于本文中用于产生这些纳米线的方法是材料成的单壁碳纳米管的熔渗。熔渗是用于获得连续填充的单壁碳纳米管（SWNT），另一个是升华，这是受欢迎的引入某些分子（ 即富勒烯）以及一些二进制盐双高产填充协议之一，最近碘化铯13。而后者的方法产生接近定量充填，它被限制在该材料被引入必须容易升华这大大限制了可被引入到单壁碳纳米管的馅料的数量和类型。熔渗灌装协议可与照顾，可用于生产近定量灌装15和具有比升华协议的限制较少。这些是，该材料必须具有表面张力低于100-200 MN M -1和低于约1300 K A熔融温度，以避免损坏主机的SWNT。16 透射电子显微镜（TEM）是表征碳纳米管的填充物的质量，并确定所产生的极端的纳米线的晶体结构或结构的最佳方法。解决SWNT嵌入水晶碎片的结构从高分辨图像涉及图像模拟的试验和错误的比较，从审判水晶碎片MODELS和实验获得的图像的对比度。本文介绍了确认极端纳米线图案的单壁碳纳米管样品中的高分辨图像模拟的微观结构的序幕，他们的光谱表征的协议。 共振拉曼光谱17是一个理想的工具既理解极端纳米线的基本物理和，一旦共振能量已经确定，用于表征纳米线的样品的类型和质量。从根本上讲，共振拉曼允许直接测定光学和振动激发能量17。与共振的光子能量的关系的附加 ​​建模是可能的量化电子-声子的相互作用17。一旦共振能量已经被确定为特定极端纳米线，纳米线的拉曼光谱可用于跟踪应变18和结构相改变19由于温度，静水压力，或电线的弯曲。虽然它仍有待证实，很可能是，在一些磁极端纳米线自旋激励将导致拉曼散射允许它们进行探测。拉曼散射的延伸到在一个光谱电化学电池保持样品可以用于探测极端纳米线和主机纳米管20之间的电荷转移。作为一种表征工具拉曼光谱提供非接触式，非破坏性检测纳米线类型和质量21的方法。它可以用作用于表征生产和/或纯化和之后的样品的工具，即使在纳米线已被包括在器件如晶体管或复合物，它们在必要的光子能量至少部分透明的。 有没有一种技术，可以为共振拉曼散射（RRS）的直接替代;然而有一个范围的重叠部分ASPE其它技术的能力克拉此方法。在确定极端纳米线的UV-VIS-NIR吸收测量22提供一个更简单的技术的光学跃迁能量的条款。然而，在具有不同结构的吸收光谱的合奏不能在不同的光学特性分离成与特定结构相关组样品。共振拉曼散射才能做到这一点，由于光学和振动光谱的关系。的两种技术，其中的UV-VIS-NIR吸收测量亮点目标共振拉曼的能量的组合可以显着加快的整个过程。光致发光光谱激发（PLE）23确实提供了不同的光学转换单个样品中相关联的能力;然而，它仅适用于某些，特别是非金属纳米线，并且它是仅略小于复杂得多RRS来执行，并在一般需要来自ENVIRO保护单分散样品市民明白是完全成功的。不像PLE，共振拉曼光谱同样适用捆绑和单分散的样品，因此需要很少的样品制备。虽然尚未很少使用，个别纳米线24，随后通过透射电子显微镜（TEM），纳米线的结构可识别所有的线的光学激发能量的在研究的光谱范围，并确定一个特定的纳米线结构的分析瑞利散射光谱。然而，该技术不能提供所述振动能量信息可能与RRS;这是非常具有挑战性的表演，是永远不会适合作为一般的表征工具。在振动能量信息方面目前唯一可行的选择是红外光谱不过25，这是有可能的，因为选择规则，探测一组不同的振动能量，因而是互补而不是竞争。此外IRŞpectroscopy将遭受与合奏样品作为UV-VIS-NIR吸收测量相同的问题。 正如已经讨论的拉曼光谱已经被应用到范围广泛的科学内的问题。在分子系统是用来补充红外光谱用于确定振动光谱，也可以作为用于分析材料的组成的指纹技术。它已被广泛利用在结晶系统， 例如 ，在固体系列图书的光散射包括九卷。在3D和2D系统的情况下，共振激发被用于增强整体散射强度多为拉曼过程中导致的标准选择规则击穿和量化的相互作用的能力内增强特定的光学跃迁的贡献较少使用在与特定的电子态的拉曼光谱中观察到的激发。最近，拉曼光谱一直中心tØ碳纳米管，尤其是单壁碳纳米管的研究。碳纳米管研究21突出的事实，即对于一维系统共振激发是不可选的，因为它是用于3D和3D系统拉曼的大多数应用中，但是绝对必要的。这是因为，非谐振拉曼散射太弱被观察，这是仅当激发谐振与状态的光密度的强烈面包车霍夫奇点，即是在特别1D系统的一个特征，即任何拉曼光谱可以观察到。因此，在极端的纳米线的情况下，利用拉曼光谱需要一个完整的共振拉曼测量，找到所有的纳米线的共振的样品中之前，拉曼光谱可用于研究这些材料。

<table>
	<tbody>
		<tr>
			<td>Carbon Nanotubes</td>
			<td>Nanointegris</td>
			<td>NI96</td>
			<td></td>
		</tr>
		<tr>
			<td>Carbon Nanotubes</td>
			<td>Private</td>
			<td></td>
			<td>Synthesis described in Eurasian Chem.-Technol. J. 2005, 5, 7-18.</td>
		</tr>
		<tr>
			<td>Mercury Telluride</td>
			<td>VMR</td>
			<td></td>
			<td>99.999% metals basis</td>
		</tr>
		<tr>
			<td>Silica Quartz Tubing</td>
			<td>H. Baumbach &#38; Co.&#160;</td>
			<td></td>
			<td>Various diameters and lengths used - typically 1 cm OD, 0.8 cm ID and 8cm long.&#160;</td>
		</tr>
		<tr>
			<td>Tube furnace</td>
			<td>Carbolite</td>
			<td>&#160;MTF-12/38/250</td>
			<td></td>
		</tr>
		<tr>
			<td>JEOL ARM 200F&#160;</td>
			<td>JEOL&#160;</td>
			<td></td>
			<td>200 kV High Resolution TEM Operated at 80 kV and equipped with&#160;</td>
		</tr>
		<tr>
			<td></td>
			<td></td>
			<td></td>
			<td>CEOS hardware spherical aberation (Cs) imaging corrector. Cs corrected&#160;</td>
		</tr>
		<tr>
			<td></td>
			<td></td>
			<td></td>
			<td>to 0.001 mm.</td>
		</tr>
		<tr>
			<td>SC1000 ORIUS camera</td>
			<td>Gatan</td>
			<td></td>
			<td>Size of CCD 4008 x 2672</td>
		</tr>
		<tr>
			<td>Digital Micrograph Suite 2.31</td>
			<td>Gatan</td>
			<td></td>
			<td>64 bit version</td>
		</tr>
		<tr>
			<td>XMax X-ray Microanalysis&#160;</td>
			<td>Oxford Instruments</td>
			<td></td>
			<td>This detector uses the silicon drift detection (SDD) principle. 1 nm diameter electron probe.</td>
		</tr>
		<tr>
			<td></td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Crystalmaker Ver 8.7</td>
			<td>Crystalmaker</td>
			<td></td>
			<td>Used for assembling crystal fragments for image simulations</td>
		</tr>
		<tr>
			<td>Nanotube Modeler</td>
			<td colspan="2">JCrystalSoft &#169;2015-2015</td>
			<td>Used for generating Nanotube models</td>
		</tr>
		<tr>
			<td>SimulaTEM</td>
			<td>Private</td>
			<td></td>
			<td>Ultramicroscopy, 2010, 110, 95-104.</td>
		</tr>
		<tr>
			<td></td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Verdi V8 Pump</td>
			<td>Coherent</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Mira 900 Ti:Sapphire</td>
			<td>Coherent</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Volume Bragg Grating</td>
			<td>Optigrate</td>
			<td></td>
			<td>Specfication between 680-720nm</td>
		</tr>
		<tr>
			<td>Photonetc TLS 850 LLTF&#160;</td>
			<td>Photonetc</td>
			<td></td>
			<td>Tunable between 700-1000nm</td>
		</tr>
		<tr>
			<td>LMPLAN IR50x MircoscopeObjective</td>
			<td>Olympus</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Cryostat</td>
			<td>Oxford Instruments</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Triple Raman Spectrometers</td>
			<td>Princeton Instruments</td>
			<td></td>
			<td>triple 600nm using gratings 900, 900, 1800 lines/mm</td>
		</tr>
		<tr>
			<td>CCD</td>
			<td>Princeton Instruments</td>
			<td></td>
			<td>deep depleted, UV enchanced liquid N2 Cooled Silicon CCD</td>
		</tr>
	</tbody>
</table>

resonance raman spectroscopy of extreme nanowires and other 1d systems

This paper briefly describes how nanowires with diameters corresponding to 1 to 5 atoms can be produced by melting a range of inorganic solids in the presence of carbon nanotubes. These nanowires are extreme in the sense that they are the limit of miniaturization of nanowires and their behavior is not always a simple extrapolation of the behavior of larger nanowires as their diameter decreases. The paper then describes the methods required to obtain Raman spectra from extreme nanowires and the fact that due to the van Hove singularities that 1D systems exhibit in their optical density of states, that determining the correct choice of photon excitation energy is critical. It describes the techniques required to determine the photon energy dependence of the resonances observed in Raman spectroscopy of 1D systems and in particular how to obtain measurements of Raman cross-sections with better than 8% noise and measure the variation in the resonance as a function of sample temperature. The paper describes the importance of ensuring that the Raman scattering is linearly proportional to the intensity of the laser excitation intensity. It also describes how to use the polarization dependence of the Raman scattering to separate Raman scattering of the encapsulated 1D systems from those of other extraneous components in any sample.

一系列的HRTEM图像和模拟上HGTE的样品的代表性结果@单壁碳纳米管在整个图1A显示图1中的图像- F，描绘低维，密闭HGTE极端纳米线，直径为〜1nm时，其微观结构对应在REF 14所讨论的形式。束和离散管的代表性图像示于图1D呈现。根据该协议，则产生一个试验模型和整个各种倾斜角度和光束方向，在此代表性结果模拟在图1A，B，C，这些图像模拟可以是互相关，以现实的实验结果（ 图1D表示， F），可以看作是一个很好的匹配与仿真。 在本文中描述的实验的主要目的是测量从极端纳米线像图2中所示的拉曼光谱。使用来自相同的生长批次中存在的图1中的纳米线采取HGTE极端纳米线的样品，测量在图2中呈现的光谱。将样品用拉曼的制备方法载于第6和协议7。在图2中呈现的谱显示有大量的峰，其中大部分可以归因于极端纳米线振动激发和多声子拉曼涉及这些振动激发的泛音和组合。基本振动模式中，A（45 -1），B（52 -1），C（94 -1）和D（115 -1），以及一些它们的组合和泛音标记在光谱可见高达至少6 阶 。该HGTE拉曼光谱的详细归属和解释载于参考14。它应当指出的是强多声子拉曼是II-IV族材料，例如HGTE的共同特征，而不一定是所有极的纳米线的样品的特征。除了纳米线设有拉曼光谱还含有一种碳纳米管的拉曼特征;主要是由于在168 -1 1.67 eV的14，其共振能量观察径向呼吸模式是从的填充拉曼特征（ 图4）的谐振能量明显不同。主机管拉曼特征可以从用于填充的纯碳纳米管的拉曼光谱来明确地识别。具有更广泛的激发能的未填充管的共振拉曼调查显示在辅助材料与本数据中确定的5 RBMS的初始归属沿。 图2给出的数据证明了强大的激励激光能源的依赖，我在1D系统的共同。这种能量依赖性的任何拉曼特征观察是由于极端的纳米线，而不是其他形式的母体材料组成，或者其热分解产物，它保留在样品中的清洗后的主要指标之一。另一个关键指标是所观察到的特征与那些的散装HGTE 30，它们通过纵向光学（LO）声子模式137 -1支配大不相同。有在文献中显著的证据表明，直径向下至3nm HGTE的纳米粒子的拉曼光谱是由本体的LO声子衍生的振动模式为主，同样是用尺寸下至2nm HGTE量子阱真。该特定拉曼特征与纳米线，而不是母体材料的纳米颗粒或块状物相关联的最后的关键指标是类似图3所示的特性的偏振相关性。如本文更详细的参考14吨讨论他拉曼从随机取向的一维系统的合奏散射优先极化方向相同为3的对比度激磁激光:1，从而显示了8字形的存在于图3所示的最佳结果的特征图。它来测试该优选发射方向与激发极化旋转时， 如图3中 ，作为偏振拉曼由于其他机制并不少见是重要的。这是很可能观察到的对比度低于3:1的纳米线的厚层，如在图3还示出了，这可以归因于该层内的光的散射。 拉曼峰的填充管样品中不存在于未填充的管，而不是由于残留填充在另一种可能的解释是，填充或残余物质导致SWCNT拉曼光谱的修改。对于插件其中有金属的单壁碳纳米管的tance样品中HGTE填充的样品，我们观察到相反偏振波依赖性的情况下蒸发到他们表现出"壁球"振动模式。31,32不过（ 图3），以对于壁球模式观察。31另外该基本模式的高次谐波的HGTE光谱观测，并没有为壁球模式光谱的事实使我们排除了HGTE拉曼功能的壁球模式的解释。 使用该协议所载文章全共振拉曼实验采取对B拉曼特征的强度的激发光子能量的关系呈现如图4所示 。同时提出从进行的实验同样的结果得到了充分开发的协议之前， 。与协议就有可能获得关于索纳重复，单点的独立测量值的变化如图5的约8％的NCE轮廓。需要为了得到良好质量的光谱要控制的系统的对准的主要部分是激光束到显微镜物镜的取向，然后将光束聚焦到例子。光束对准的重要性在图6a中，E是示出。在该图中的拉曼光谱示（ 图6a，蓝色迹线）与正确对准到两个波束转向摄像机（c和e）和亚最佳光谱（ 图6a，绿色迹线）与梁故意不对准的光束。通过每个帧B的垂直和水平中心的点A线， 例如在图6示出有小的水平漂移的激光对准当图6b和6d进行比较，如图所示。绿色和蓝色痕迹6比较一个，这是清楚的是一个小的未对准可导致拉曼信号击中CCD的显著变化（&gt; 50％的损失）。 使用反射的束强度，以确保目标被正确聚焦在样品上的重要性，和相关性，在图7中示出。该图表示拉曼强度与反射光信号为目标和样品之间的距离的函数。是峰的拉曼，Z位置（物镜和样本之间的距离）的精度的10％之内需要更好地大于20微米，其比功率和拉曼的峰值位置作为之间的距离相当大的在图7中。 在协议中讨论的，重要的是对拉曼光谱的激光激发强度的影响考虑在内，而且实验是在其中测量共振配置文件时的拉曼散射是成正比的激发强度的制度。 HGTE极端纳米线，因为每协议的第9测定的拉曼散射强度的激发强度的依赖代表性的测量，示于图8。如在图8提出的拉曼强度最初与激发强度线性增加最多的强度为1.5×10 4个之前开始显示与用于信号饱和的倾向非线性行为。不同样品的精确激发强度的行为会有所不同，因此，必须进行测量和考虑。从图8中的拉曼强度显然内激发强度比〜0.2毫瓦/毫米2越大非线性区域。还示出的是一个线性拟合在低激发强度的数据表明，在足够足够低的激发我ntensities拉曼强度正比于激发强度（达〜0.1毫瓦/毫米2）。它重申这个数据是该特定样本位置独特在特定温度下（4 K）和当一个不同的样品/温度研究的实验必须重复按照协议的步骤是重要的。作为一个一般的经验规则，它是理想的线性状态使用的最大功率的80％左右。 一旦高质量共振能量依赖性轮廓已经测量这些随后可以分析得到的范围内的信息。底层拉曼过程理论是众所周知的，并随时间变化的微扰理论17，通常使用一个费 ​​曼图方法21,33计算，可以用来预测谐振型材和甚至绝对强度。在该光学转换是离散的和在能量以及分离出的限制的理论预测，拉马Ñ​​强度为单声子散射如下在光学过渡乘以由一个中心的洛伦兹线形中心以上对于斯托克斯散射或低于反斯托克斯拉曼散射1声子能量1声子能量。如果声子的能量小相比谐振线宽，作为为HGTE纳米线的情况下，这将导致具有罗伦兹共振平方线形。然而，在一维系统中，很可能在光谱的特征将用由状态的连续的货车霍夫奇点相关联。此外，还有可能是样品进一步拓宽了过渡内不均匀。如果其中一个或两个都是真的，那么国家对光跃迁密度将改变，并可以支配的线形。这种情况变得更加复杂，因为拉曼散射是一个连贯的过程，涉及不同的散射序列和不同的中间状态，因此干涉效应旨意改变谐振轮廓34。出于同样的原因相干寿命的中间态之间的任何变化，也可以影响线形35。从缺陷和双共振的影响，特别是在较高阶拉曼散射弹性散射的介入的可能性，这种情况21,35进一步复杂化。它往往因此不可能先验预测预期的拉曼谐振轮廓。然而共振拉曼散射已经被用于提取约不同的材料系统，其中包括的特征在光谱的能量，国家负责这些功能的性质和电子-声子的相互作用17的定量强度的性质的大量信息。为了更好地量化的共振内的光学特性的能量和精力充沛的宽度轮廓它常常是有帮助他们使用标准光学lineshapes之一以适应。在我们试图洛伦兹的HGTE纳米线的情况下，洛伦兹平方和高斯lineshapes发现高斯lineshapes成为最佳拟合（ 图4）。需要明确的是，这是一个现象配合和使用高斯线形的不能在其中产生谐振的光学特性的展宽的性质来解释。从这些拟合我们可以确定负责谐振是1.76 eV的光学特性的能量。 HGTE极端纳米线的共振行为的更详细的分析将另行公布。 拉曼光谱的温度依赖性的测定使附加物理被探测。尤其是振动能量和振动峰的宽度允许非谐效应，导致晶格扩张和基本限制在声子的一生的转变进行调查。 Resonan测量CE配置文件作为温度的函数将允许确定光能量的温度依赖性。示可能的温度相关效应一些代表性结果示于图9中。从图9可以看出（a和b），该温度增加频谱宽度扩大和模式的中心移软化，这与理论在线预测。最引人注目的是窗口C，表示在B模式的强度急剧下降客作为温度的函数。这种效果，这将在更详细地在一个单独的出版物讨论的，主要是由于在负责随着温度的共振的光学状态的相干寿命的降低和明显的证据表明拉曼散射可以远提供信息超出可能与吸收测量。 如图5。 <img alt="图1" src="/files/ftp_upload/53434/53434fig1.jpg" /> 图1:用对比的模拟结果极端纳米线的HRTEM结构模型，HRTEM模拟协议和嵌入〜1.4 nm的直径的单壁碳纳米管〜1nm厚HGTE纳米线的试验图像。一个典型的局部剖面模型（ 一 ）<html> 3纳米长HGTE的片段嵌入在（10,10）SWNT。电子束的方向（B）为代表的一系列HGTE @（10,10）SWNT复合材料（C，LH模拟）和倾斜（D，RH模拟）的取向不同的预测。高分辨透射电子显微镜图像（ 即右上）可以对表（C）相匹配，并与实验图像匹配（D左上角和右上角）。从细单壁碳纳米管束（e）中得到高分辨图像，用于观察嵌入式〜1纳米的纳米线HGTE（I，II和III），并在画面模拟相关（ 即镶石I&#39;，II&#39;和III&#39;）。一些片段被倾斜（F，左）角T，通过模拟（F，中间）仿照对应于剖切模型f中的权利。F ="htt​​ps://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/53434/53434fig1large.jpg"目标="_空白"&gt;点击此处查看该图的放大版本。 <img alt="图2" src="/files/ftp_upload/53434/53434fig2.jpg" /> 图2:极端碲化汞的拉曼光谱碳纳米管嵌入在 HGTE极端纳米线的代表拉曼光谱在4 K的多个激发光子能量获得的单壁碳纳米管。各种痕迹对应激发1.78，1.77，1.75和1.71 eV的为蓝色，绿色红色和紫色分别线能量。 <a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/53434/53434fig2large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图3" src="/files/ftp_upload/53434/53434fig3.jpg" /> 图3:乙峰拟合强度作为分析陈子昂的函数<html>乐。在1.77 eV的B的峰值的拟合强度的极坐标图和4 K作为分析角度的函数在垂直（蓝色）和横向（绿色）事件的两极分化。 <a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/53434/53434fig3large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图4" src="/files/ftp_upload/53434/53434fig4.jpg" /> 图4:共振效应HGTE的B模式观察@单壁碳纳米管的B共振轮廓（52 -1）模式为激光波长的两个（ 一 ），其中详述的协议被附着到壳体和情况（b的功能。 ）采取的协议被开发之前。高斯线宽周围1.77±1兆电子伏和1.74±3兆电子伏分别居中为a和b。错误是由嵌合常规的95％置信界限来确定。文件/ ftp_upload / 53434 / 53434fig4large.jpg"目标="_空白"&gt;点击此处查看该图的放大版本。 <img alt="图5" src="/files/ftp_upload/53434/53434fig5.jpg" /> 图5:在整个实验RRS 702纳米的入射光波长拉曼光谱的独立重复一系列的拉曼光谱，整个实验相同的条件下拍摄。光谱显示了共振拉曼实验中在4K一个702纳米的激光线测得的A和B模式。 <a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/53434/53434fig5large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图6" src="/files/ftp_upload/53434/53434fig6.jpg" /> 图6:HGTE的拉曼光谱@当系统优化，故意失谐采取单壁碳纳米管的拉曼光谱获取了ŧ室温当系统完全一致（蓝色线），并故意错位（绿色线）。帧（B，D）上显示照相机（C2）的激光图像以及（c，e）表示对照相机（C1）的激光光斑。该井对齐谱对应于从b和c图像，而故意不对齐的光谱是通过D和E所示。 <a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/53434/53434fig6large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图7" src="/files/ftp_upload/53434/53434fig7.jpg" /> 图7:反射功率和Si峰的相应的拉曼峰强度与样品焦点位置的函数的归一化的情节上反射功率计（PM2）和拉曼INT的归一化强度测量功率（红色）密度（蓝色）为样本和目标之间的距离的函数。 <a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/53434/53434fig7large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图8" src="/files/ftp_upload/53434/53434fig8.jpg" /> 图8:在4 K和702纳米的对B的拉曼模式的强度的绘图用洛伦兹嵌合作为激发强度的函数定量 B模式作为入射功率的函数，其中一个适合被施加到确定的拟合强度。线性状态。 <a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/53434/53434fig8large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图9" src="/files/ftp_upload/53434/53434fig9.jpg" /> 图9:HGTE的B模式温度的关系@在固定的单壁碳纳米管（1.77电子伏特）的激发能量。在恒定激发能量（1.77电子伏特）作为温度的函数获得的拉曼光谱。窗户交流分别表示B模式的频谱宽度，中心偏移和装配强度。显示误差线是从拟合程序的95％置信区间。 <a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/53434/53434fig9large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图10" src="/files/ftp_upload/53434/53434fig10.jpg" /> 图10:对于共振拉曼光谱实验采用的光学装置的原理图显示在协议讨论的所有实验采用的光学设置<a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/53434/53434fig10large.jpg" target="_blank">，请点击此处查看该图的放大版本。</a>

Watch this Scientific Journal Video about Resonance Raman Spectroscopy of Extreme Nanowires and Other 1D Systems at JoVE.com

Resonance Raman Spectroscopy of Extreme Nanowires and Other 1D Systems

The paper describes a method for producing extreme nanowires by melt infiltration into carbon nanotubes and how 1D systems may be characterized and investigated using Resonance Raman Spectroscopy to determine vibrational and optical excitation energies.

至尊纳米线和其他维系统的共振拉曼光谱

This paper briefly describes how nanowires with diameters corresponding to 1 to 5 atoms can be produced by melting a range of inorganic solids in the ...

resonance-raman-spectroscopy-of-extreme-nanowires-and-other-1d-systems

Nanyang Technological University

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JoVE Journal

Engineering

15.0K 次观看.  University of Southampton. The paper describes a method for producing extreme nanowires by melt infiltration into carbon nanotubes and how 1D systems may be characterized and investigated using Resonance Raman Spectroscopy to determine vibrational and optical excitation energies.

视频: Resonance Raman Spectroscopy of Extreme Nanowires and Other 1D Systems

Synthesis and Microdiffraction at Extreme Pressures and Temperatures

High pressure compounds and polymorphs are investigated for a broad range of purposes such as determine structures and processes of deep planetary interiors, design materials with novel properties, understand the mechanical behavior of materials exposed to very high stresses as in explosions or impacts. Synthesis and structural analysis of materials at extreme conditions of pressure and temperature entails remarkable technical challenges. In the laser heated diamond anvil cell (LH-DAC), very high pressure is generated between the tips of two opposing diamond anvils forced against each other; focused infrared laser beams, shined through the diamonds, allow to reach very high temperatures on samples absorbing the laser radiation. When the LH-DAC is installed in a synchrotron beamline that provides extremely brilliant x-ray radiation, the structure of materials under extreme conditions can be probed in situ. LH-DAC samples, although very small, can show highly variable grain size, phase and chemical composition. In order to obtain the high resolution structural analysis and the most comprehensive characterization of a sample, we collect diffraction data in 2D grids and combine powder, single crystal and multigrain diffraction techniques. Representative results obtained in the synthesis of a new iron oxide, Fe4O5 1 will be shown.

The laser heated diamond anvil cell combined with synchrotron micro-diffraction techniques allows researchers to explore the nature and properties of new phases of matter at extreme pressure and temperature (PT) conditions. Heterogeneous samples can be characterized in situ under high pressure by 2D mapping and combined powder, single-crystal and multigrain diffraction approaches.

在极端的压力和温度的合成和Microdiffraction

High pressure compounds and polymorphs are investigated for a broad range of purposes such as determine structures and processes of deep planetary ...

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工程学

Ultrahigh Density Array of Vertically Aligned Small-molecular Organic Nanowires on Arbitrary Substrates

In recent years &pi;-conjugated organic semiconductors have emerged as the active material in a number of diverse applications including large-area, low-cost displays, photovoltaics, printable and flexible electronics and organic spin valves. Organics allow (a) low-cost, low-temperature processing and (b) molecular-level design of electronic, optical and spin transport characteristics. Such features are not readily available for mainstream inorganic semiconductors, which have enabled organics to carve a niche in the silicon-dominated electronics market. The first generation of organic-based devices has focused on thin film geometries, grown by physical vapor deposition or solution processing. However, it has been realized that organic nanostructures can be used to enhance performance of above-mentioned applications and significant effort has been invested in exploring methods for organic nanostructure fabrication.	
A particularly interesting class of organic nanostructures is the one in which vertically oriented organic nanowires, nanorods or nanotubes are organized in a well-regimented, high-density array. Such structures are highly versatile and are ideal morphological architectures for various applications such as chemical sensors, split-dipole nanoantennas, photovoltaic devices with radially heterostructured "core-shell" nanowires, and memory devices with a cross-point geometry. Such architecture is generally realized by a template-directed approach. In the past this method has been used to grow metal and inorganic semiconductor nanowire arrays. More recently &pi;-conjugated polymer nanowires have been grown within nanoporous templates. However, these approaches have had limited success in growing nanowires of technologically important &pi;-conjugated small molecular weight organics, such as tris-8-hydroxyquinoline aluminum (Alq3), rubrene and methanofullerenes, which are commonly used in diverse areas including organic displays, photovoltaics, thin film transistors and spintronics.	
Recently we have been able to address the above-mentioned issue by employing a novel "centrifugation-assisted" approach. This method therefore broadens the spectrum of organic materials that can be patterned in a vertically ordered nanowire array. Due to the technological importance of Alq3, rubrene and methanofullerenes, our method can be used to explore how the nanostructuring of these materials affects the performance of aforementioned organic devices. The purpose of this article is to describe the technical details of the above-mentioned protocol, demonstrate how this process can be extended to grow small-molecular organic nanowires on arbitrary substrates and finally, to discuss the critical steps, limitations, possible modifications, trouble-shooting and future applications.

We report a simple method for fabricating an ultrahigh density array of vertically ordered small-molecular organic nanowires. This method allows for synthesis of complex heterostructured hybrid nanowire geometries, which can be inexpensively grown on arbitrary substrates. These structures have potential applications in organic electronics, optoelectronics, chemical sensing, photovoltaics and spintronics.

超高密度垂直对齐的任意基质的小分子有机纳米线阵列

In  recent years &pi;-conjugated  organic semiconductors have emerged as the active material in a number of  diverse applications including large-area, ...

Monolayer Contact Doping of Silicon Surfaces and Nanowires Using Organophosphorus Compounds

Monolayer Contact Doping (MLCD) is a simple method for doping of surfaces and nanostructures1. MLCD results in the formation of highly controlled, ultra shallow and sharp doping profiles at the nanometer scale. In MLCD process the dopant source is a monolayer containing dopant atoms.
In this article a detailed procedure for surface doping of silicon substrate as well as silicon nanowires is demonstrated. Phosphorus dopant source was formed using tetraethyl methylenediphosphonate monolayer on a silicon substrate. This monolayer containing substrate was brought to contact with a pristine intrinsic silicon target substrate and annealed while in contact. Sheet resistance of the target substrate was measured using 4 point probe. Intrinsic silicon nanowires were synthesized by chemical vapor deposition (CVD) process using a vapor-liquid-solid (VLS) mechanism; gold nanoparticles were used as catalyst for nanowire growth. The nanowires were suspended in ethanol by mild sonication. This suspension was used to dropcast the nanowires on silicon substrate with a silicon nitride dielectric top layer. These nanowires were doped with phosphorus in similar manner as used for the intrinsic silicon wafer. Standard photolithography process was used to fabricate metal electrodes for the formation of nanowire based field effect transistor (NW-FET). The electrical properties of a representative nanowire device were measured by a semiconductor device analyzer and a probe station.

A detailed procedure for surface doping of Silicon interfaces is provided. The ultra-shallow surface doping is demonstrated by using phosphorus containing monolayers and rapid annealing process. The method can be used for doping of macroscopic area surfaces as well as nanostructures.

Monolayer Contact Doping (MLCD) is a simple method for doping of surfaces and nanostructures1. MLCD results in the formation of highly controlled, ultra ...

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 ...

Preparation and Use of Photocatalytically Active Segmented Ag|ZnO and Coaxial TiO2-Ag Nanowires Made by Templated Electrodeposition

Photocatalytically active nanostructures require a large specific surface area with the presence of many catalytically active sites for the oxidation and reduction half reactions, and fast electron (hole) diffusion and charge separation. Nanowires present suitable architectures to meet these requirements. Axially segmented Ag|ZnO and radially segmented (coaxial) TiO2-Ag nanowires with a diameter of 200 nm and a length of 6-20 &#181;m were made by templated electrodeposition within the pores of polycarbonate track-etched (PCTE) or anodized aluminum oxide (AAO) membranes, respectively. In the photocatalytic experiments, the ZnO and TiO2 phases acted as photoanodes, and Ag as cathode. No external circuit is needed to connect both electrodes, which is a key advantage over conventional photo-electrochemical cells. For making segmented Ag|ZnO nanowires, the Ag salt electrolyte was replaced after formation of the Ag segment to form a ZnO segment attached to the Ag segment. For making coaxial TiO2-Ag nanowires, a TiO2 gel was first formed by the electrochemically induced sol-gel method. Drying and thermal annealing of the as-formed TiO2 gel resulted in the formation of crystalline TiO2 nanotubes. A subsequent Ag electrodeposition step inside the TiO2 nanotubes resulted in formation of coaxial TiO2-Ag nanowires. Due to the combination of an n-type semiconductor (ZnO or TiO2) and a metal (Ag) within the same nanowire, a Schottky barrier was created at the interface between the phases. To demonstrate the photocatalytic activity of these nanowires, the Ag|ZnO nanowires were used in a photocatalytic experiment in which H2 gas was detected upon UV illumination of the nanowires dispersed in a methanol/water mixture. After 17 min&#160;of illumination, approximately 0.2 vol% H2 gas was detected from a suspension of ~0.1 g of Ag|ZnO nanowires in a 50 ml 80 vol% aqueous methanol solution.

Preparation and Use of Photocatalytically Active Segmented Ag|ZnO and Coaxial TiO2-Ag Nanowires Made by Templated Electrodeposition

Procedures are outlined to prepare segmented and coaxial nanowires via templated electrodeposition in nanopores. As examples, segmented nanowires consisting of Ag and ZnO segments, and coaxial nanowires consisting of a TiO2 shell and a Ag core were made. The nanowires were used in photocatalytic hydrogen formation experiments.

制备和使用光催化活性分段银|氧化锌和二氧化钛同轴<sub&gt; 2</sub&gt;银纳米线制成由模板电

Photocatalytically active nanostructures require a large specific surface area with the presence of many catalytically active sites for the oxidation and ...

High-Sensitivity Nuclear Magnetic Resonance at Giga-Pascal Pressures: A New Tool for Probing Electronic and Chemical Properties of Condensed Matter under Extreme Conditions

Nuclear Magnetic Resonance (NMR) is one of the most important techniques for the study of condensed matter systems, their chemical structure, and their electronic properties. The application of high pressure enables one to synthesize new materials, but the response of known materials to high pressure is a very useful tool for studying their electronic structure and developing theories. For example, high-pressure synthesis might be at the origin of life; and understanding the behavior of small molecules under extreme pressure will tell us more about fundamental processes in our universe. It is no wonder that there has always been great interest in having NMR available at high pressures. Unfortunately, the desired pressures are often well into the Giga-Pascal (GPa) range and require special anvil cell devices where only very small, secluded volumes are available. This has restricted the use of NMR almost entirely in the past, and only recently, a new approach to high-sensitivity GPa NMR, which has a resonating micro-coil inside the sample chamber, was put forward. This approach enables us to achieve high sensitivity with experiments that bring the power of NMR to Giga-Pascal pressure condensed matter research. First applications, the detection of a topological electronic transition in ordinary aluminum metal and the closing of the pseudo-gap in high-temperature superconductivity, show the power of such an approach. Meanwhile, the range of achievable pressures was increased tremendously with a new generation of anvil cells (up to 10.1 GPa), that fit standard-bore NMR magnets. This approach might become a new, important tool for the investigation of many condensed matter systems, in chemistry, geochemistry, and in physics, since we can now watch structural changes with the eyes of a very versatile probe.

Nuclear magnetic resonance is one of the most important spectroscopic tools. Here, the development of a new approach under high pressure, currently up to 10.1 GPa, is presented. This opens a new window into condensed matter physics and chemistry, where high-pressure research is of great importance.

高灵敏度核磁共振的千兆帕斯卡压力:一种新的工具，用于极端条件下探测电子和化工凝聚态的性质

Nuclear Magnetic Resonance (NMR) is one of the most important techniques for the study of condensed matter systems, their chemical structure, and their ...

Surface Enhanced Raman Spectroscopy Detection of Biomolecules Using EBL Fabricated Nanostructured Substrates

Fabrication and characterization of conjugate nano-biological systems interfacing metallic nanostructures on solid supports with immobilized biomolecules is reported. The entire sequence of relevant experimental steps is described, involving the fabrication of nanostructured substrates using electron beam lithography, immobilization of biomolecules on the substrates, and their characterization utilizing surface-enhanced Raman spectroscopy (SERS). Three different designs of nano-biological systems are employed, including protein A, glucose binding protein, and a dopamine binding DNA aptamer. In the latter two cases, the binding of respective ligands, D-glucose and dopamine, is also included. The three kinds of biomolecules are immobilized on nanostructured substrates by different methods, and the results of SERS imaging are reported. The capabilities of SERS to detect vibrational modes from surface-immobilized proteins, as well as to capture the protein-ligand and aptamer-ligand binding are demonstrated. The results also illustrate the influence of the surface nanostructure geometry, biomolecules immobilization strategy, Raman activity of the molecules and presence or absence of the ligand binding on the SERS spectra acquired.

We describe the fabrication and characterization of nano-biological systems interfacing nanostructured substrates with immobilized proteins and aptamers. The relevant experimental steps involving lithographic fabrication of nanostructured substrates, bio-functionalization, and surface-enhanced Raman spectroscopy (SERS) characterization, are reported. SERS detection of surface-immobilized proteins, and probing of protein-ligand and aptamer-ligand binding is demonstrated.

表面增强拉曼光谱检测生物分子利用EBL装配纳米衬底

Fabrication and characterization of conjugate nano-biological systems interfacing metallic nanostructures on solid supports with immobilized biomolecules ...

Characterization of Nanocrystal Size Distribution using Raman Spectroscopy with a Multi-particle Phonon Confinement Model

Analysis of the size distribution of nanocrystals is a critical requirement for the processing and optimization of their size-dependent properties. The common techniques used for the size analysis are transmission electron microscopy (TEM), X-ray diffraction (XRD) and photoluminescence spectroscopy (PL). These techniques, however, are not suitable for analyzing the nanocrystal size distribution in a fast, non-destructive and a reliable manner at the same time. Our aim in this work is to demonstrate that size distribution of semiconductor nanocrystals that are subject to size-dependent phonon confinement effects, can be quantitatively estimated in a non-destructive, fast and reliable manner using Raman spectroscopy. Moreover, mixed size distributions can be separately probed, and their respective volumetric ratios can be estimated using this technique. In order to analyze the size distribution, we have formulized an analytical expression of one-particle PCM and projected it onto a generic distribution function that will represent the size distribution of analyzed nanocrystal. As a model experiment, we have analyzed the size distribution of free-standing silicon nanocrystals (Si-NCs) with multi-modal size distributions. The estimated size distributions are in excellent agreement with TEM and PL results, revealing the reliability of our model.

We demonstrate how to determine the size distribution of semiconductor nanocrystals in a quantitative manner using Raman spectroscopy employing an analytically defined multi-particle phonon confinement model. Results obtained are in excellent agreement with the other size analysis techniques like transmission electron microscopy and photoluminescence spectroscopy.

使用拉曼光谱与多颗粒的声子坐月子型号纳米大小分布的特征

Analysis of the size distribution of nanocrystals is a critical requirement for the processing and optimization of their size-dependent properties. The ...

A Fabrication Method for Highly Stretchable Conductors with Silver Nanowires

Stretchable electronics are identified as a key technology for electronic applications in the next generation. One of the challenges in fabrication of stretchable electronic devices is the preparation of stretchable conductors with great mechanical stability. In this study, we developed a simple fabrication method to chemically solder the contact points between silver nanowire (AgNW) networks. AgNW nanomesh was first deposited on a glass slide via spray coating method. A reactive ink composed of silver nanoparticle (AgNPs) precursors was applied over the spray coated AgNW thin films. After heating for 40 min, AgNPs were preferentially generated over the nanowire junctions to solder the AgNW nanomesh, and reinforced the conducting network. The chemically modified AgNW thin film was then transferred to polyurethane (PU) substrates by casting method. The soldered AgNW thin films on PU exhibited no obvious change in electrical conductivity under stretching or rolling process with elongation strains up to 120%.

A simple synthesis method is used to chemically solder silver nanowire thin film to fabricate highly stretchable and conductive metal conductors.

对于高伸缩的导线与银纳米线制作方法

Stretchable electronics are identified as a key technology for electronic applications in the next generation. One of the challenges in fabrication of ...

High Resolution Phonon-assisted Quasi-resonance Fluorescence Spectroscopy

High resolution optical spectroscopy methods are demanding in terms of either technology, equipment, complexity, time or a combination of these. Here we demonstrate an optical spectroscopy method that is capable of resolving spectral features beyond that of the spin fine structure and homogeneous linewidth of single quantum dots (QDs) using a standard, easy-to-use spectrometer setup. This method incorporates both laser and photoluminescence spectroscopy, combining the advantage of laser line-width limited resolution with multi-channel photoluminescence detection. Such a scheme allows for considerable improvement of resolution over that of a common single-stage spectrometer. The method uses phonons to assist in the measurement of the photoluminescence of a single quantum dot after resonant excitation of its ground state transition. The phonon&#39;s energy difference allows one to separate and filter out the laser light exciting the quantum dot. An advantageous feature of this method is its straight forward integration into standard spectroscopy setups, which are accessible to most researchers.

The manuscript describes a method of phonon-assisted quasi-resonant fluorescence spectroscopy that incorporates both laser-limited resolution and photoluminescence (PL) spectroscopy. This method utilizes optical phonons to provide linewidth-limited resolution spectra of atom-like semiconductor structures in the energy domain. The method is also easily realized with a single spectrometer optical spectroscopy setup.

高分辨率声子辅助准共振荧光光谱仪

High resolution optical spectroscopy methods are demanding in terms of either technology, equipment, complexity, time or a combination of these. Here we ...