Name: preparation and characterization of c60/graphene hybrid nanostructures
Uploaded: 2018-05-15T13:00:00
Description: Watch this Scientific Journal Video about Preparation and Characterization of C60/Graphene Hybrid Nanostructures at JoVE.com

这项工作由美国陆军研究办公室在赠款 W911NF-15-1-0414 下支持。

1. 自制努森细胞的研制
<ol><li>
准备努森单元的组件
	<ol>
<li>购买 cf 法兰基电源馈 (2.75 "CF, 4 针不锈钢)。钻两个螺纹孔通过馈, 在十字点之间的一个直径 1.30 "线和它的周长。</li>
		<li>准备一个玻璃管 (0.315 "外径 (OD), 2.50" 长度)。</li>
		<li>采购薄铜板 (99.9%) 与 0.005 "厚度。用剪刀将一张纸切成 7.5 "L x 5.0" W 的尺寸, 然后将其卷曲到带有 1.45 "手动直径" 的空心圆柱形通盾(</str...

<ol>
	<li>Gutzler, R., Heckl, W. M., Lackinger, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Combination+of+a+Knudsen+effusion+cell+with+a+quartz+crystal+microbalance:+In+situ+measurement+of+molecular+evaporation+rates+with+a+fully+functional+deposition+source.">Combination of a Knudsen effusion cell with a quartz crystal microbalance: In situ measurement of molecular evaporation rates with a fully functional deposition source.</a> Review of Scientific Instruments. 81, 015108 (2010).</li><li>de Barros, A. L. F., 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=A+simple+experimental+arrangement+for+measuring+the+vapour+pressures+and+sublimation+enthalpies+by+the+Knudsen+effusion+method:+Application+to+DNA+and+RNA+bases.">A simple experimental arrangement for measuring the vapour pressures and sublimation enthalpies by the Knudsen effusion method: Application to DNA and RNA bases.</a> Nuclear Instruments &amp; Methods in Physics Research Section a-Accelerators Spectrometers Detectors and Associated Equipment. 560, (2006).</li><li>Shukla, A. 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=Versatile+UHV+compatible+Knudsen+type+effusion+cell.">Versatile UHV compatible Knudsen type effusion cell.</a> Review of Scientific Instruments. 75, 4467 (2004).</li><li>Cho, 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=Structural+and+Electronic+Decoupling+of+C60+from+Epitaxial+Graphene+on+SiC.">Structural and Electronic Decoupling of C60 from Epitaxial Graphene on SiC.</a> Nano Letters. 12, 3018 (2012).</li><li>Jung, M., 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=Atomically+resolved+orientational+ordering+of+C60+molecules+on+epitaxial+graphene+on+Cu(111).">Atomically resolved orientational ordering of C60 molecules on epitaxial graphene on Cu(111).</a> Nanoscale. 6 (111), 11835 (2014).</li><li>Li, G., 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=Self-assembly+of+C60+monolayer+on+epitaxially+grown,+nanostructured+graphene+on+Ru(0001)+surface.">Self-assembly of C60 monolayer on epitaxially grown, nanostructured graphene on Ru(0001) surface.</a> Applied Physics Letters. 100 (0001), 013304 (2012).</li><li>Lu, 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=Using+the+Graphene+Moire+Pattern+for+the+Trapping+of+C60+and+Homoepitaxy+of+Graphene.">Using the Graphene Moire Pattern for the Trapping of C60 and Homoepitaxy of Graphene.</a> Acs Nano. 6, 944 (2012).</li><li>Zhou, H. 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=Direct+imaging+of+intrinsic+molecular+orbitals+using+two-dimensional,+epitaxially-grown,+nanostructured+graphene+for+study+of+single+molecule+and+interactions.">Direct imaging of intrinsic molecular orbitals using two-dimensional, epitaxially-grown, nanostructured graphene for study of single molecule and interactions.</a> Applied Physics Letters. 99, 153101 (2011).</li><li>Belaish, I., 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=Spin+Cast+Thin-Films+of+Fullerenes+and+Fluorinated+Fullerenes+-+Preparation+and+Characterization+by+X-Ray+Reflectivity+and+Surface+Diffuse-X-Ray+Scattering.">Spin Cast Thin-Films of Fullerenes and Fluorinated Fullerenes - Preparation and Characterization by X-Ray Reflectivity and Surface Diffuse-X-Ray Scattering.</a> Journal of Applied Physics. 71, 5248 (1992).</li><li>Bezmel'nitsyn, V. N., Eletskii, A. V., Okun', M. V. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Fullerenes+in+solutions.">Fullerenes in solutions.</a> Uspekhi Fizicheskikh Nauk. 168, 1195 (1998).</li><li>Ma, D. N., Sandoval, S., Muralidharan, K., Raghavan, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Effect+of+surface+preparation+of+copper+on+spin-coating+driven+self-assembly+of+fullerene+molecules.">Effect of surface preparation of copper on spin-coating driven self-assembly of fullerene molecules.</a> Microelectronic Engineering. 170, 8 (2017).</li><li>Chen, C. H., Zheng, H. S., Mills, A., Heflin, J. R., Tao, C. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Temperature+Evolution+of+Quasi-one-dimensional+C60+Nanostructures+on+Rippled+Graphene.">Temperature Evolution of Quasi-one-dimensional C60 Nanostructures on Rippled Graphene.</a> Scientific Reports. 5, 14336 (2015).</li></ol>

本协议所描述的技术设计用于有机材料和其他高蒸气压材料的热沉积。这些技术可与超高真空系统集成, 具有样品制备区域, 能够支持分子蒸发和热退火。本实验的目的是在石墨烯基体上沉积 c60分子, 并研究 c60的自组装和热效应。
该方法的好处是, 它提供了一个超级干净的样品时, 与其他薄膜制备方法, 如自旋涂层。与化学气相沉积 (CVD) 等复杂技术相比, 这种?...

本协议解释如何在石墨烯上沉积和操作 c60分子, 这样可以实现1D 和 quasi-1D C60链结构。这项实验的技术是为了解决需要引导考察到理想的配置, 而不必依赖手动操作, 这是缓慢的, 并可能需要很大的努力。这里描述的过程依赖于使用一个高真空系统与样品准备区域能支持分子沉积和热退火样品。STM 是用来表征样品, 但其他分子分辨率技术可以应用。
努森细胞内分子的热蒸发是制备薄膜的一种高效、清洁的方法。在本协议中, 努森单元用于将 C60分子蒸发到石墨烯基板上。此努森电池蒸发器主要由石英管、加热灯丝、热电偶线和贯穿件可1、2、3组成.石英管用于容纳分子, 钨灯丝通过应用电流加热石英管中的分子, 热电偶导线用于测量温度。实验中, 通过对努森细胞中温度源的调节, 控制了沉积速率。热电偶导线附着在石英管的外壁上, 因此通常测量外部壁的温度, 这与分子源所在细胞内的温度稍有不同。为了获得石英管的精确温度, 我们用两个热电偶装置进行了标定, 以测量管内外的温度, 并记录了温度差。这样, 我们就可以更精确地控制在分子蒸发实验中使用连接到石英管外的热电偶线的温度。由于少量的升华分子将在一个较低的压力下的气态相, 当分子被蒸发, 通常有一个相关的压力变化。因此, 我们仔细地监视负载锁中压力的变化。
该蒸发器可用于存放各种分子源, 如 c60、c70、硼酞菁染料氯化物、Ga、Al 和Hg4、5、6、7、8。与其他薄膜制备技术相比, 自旋铸造9,10,11, 高真空中的热蒸发更清洁和多功能, 因为没有溶剂需要证言。此外, 沉积前的脱气过程提高了源的纯度, 消除了可能的杂质。

<table>
	<tbody>
		<tr>
			<td>CF Flanged power feedthrough</td>
			<td>Kurt J. Lesker</td>
			<td>EFT0042033</td>
			<td></td>
		</tr>
		<tr>
			<td>Copper sheets</td>
			<td>Alfa Aesar</td>
			<td>7440-50-8</td>
			<td></td>
		</tr>
		<tr>
			<td>Thermocouple chromel/alumel wires</td>
			<td>Omega Engineering</td>
			<td>ST032034/ST080042</td>
			<td></td>
		</tr>
		<tr>
			<td>Tungsten wires</td>
			<td>Alfa Aesar</td>
			<td>7440-33-7</td>
			<td></td>
		</tr>
		<tr>
			<td>Stainless steel rods</td>
			<td>McMaster-Carr</td>
			<td>95412A868</td>
			<td></td>
		</tr>
		<tr>
			<td>Copper wires</td>
			<td>McMaster-Carr</td>
			<td>8873K28</td>
			<td></td>
		</tr>
		<tr>
			<td>Hollow copper rods</td>
			<td>McMaster-Carr</td>
			<td>7190K52</td>
			<td></td>
		</tr>
		<tr>
			<td>C60</td>
			<td>MER Corporation</td>
			<td>MR6LP</td>
			<td></td>
		</tr>
	</tbody>
</table>

preparation and characterization of c60/graphene hybrid nanostructures

高真空环境下的物理热沉积是制备石墨烯上新型分子纳米结构的一种清洁、可控的方法。我们提出了在波纹石墨烯上沉积和被动操作 C60分子的方法, 它推动了实现涉及 1D C60/石墨烯混合结构的应用。本博览会所采用的技术是针对高真空系统的, 其制备区域能够支持分子沉积以及样品的热退火。我们专注于 C60在低压沉积使用一个自制的努森细胞连接到扫描隧穿显微镜 (STM) 系统。通过控制努森细胞的温度和沉积时间来调节沉积分子的数量。一维 (1D) C60链结构, 其宽度为三个分子, 可通过对实验条件的调整来制备。C60分子的表面流动性随退火温度的增加而增大, 使它们能够在波纹石墨烯的周期性电位内移动。使用此机制, 可以控制 1D C60链结构的过渡到六角封闭包装 quasi-1D 条纹结构。

蒸发后, 新沉积的 C60的石墨烯退火为 2 h 的150摄氏度。图 2a中的大型 STM 映像显示了此初始退火过程后发现的特性 quasi-1D C60链结构。在图 2b中进行更仔细的检查, 可显示此1D 结构的详细信息, 其中每个明亮的球面凸起表示一个单一的 C60分子。通常, 1D 链作为分子和三分子 c 60 链出现, 其平均值为 c 60-C 60 距...

Watch this Scientific Journal Video about Preparation and Characterization of C60/Graphene Hybrid Nanostructures at JoVE.com

Preparation and Characterization of C60/Graphene Hybrid Nanostructures

C 型60/石墨烯混合纳米结构的制备与表征

在这里, 我们提出了一个协议, 以制造的 C60/石墨烯混合纳米结构的物理热蒸发。特别是, 适当地操纵沉积和退火条件, 可以控制在波纹石墨烯上创建1D 和准 1D C60结构。

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Preparation and Characterization of C60/Graphene Hybrid Nanostructures

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