Name: using neutron spin echo resolved grazing incidence scattering to investigate organic solar cell materials
Uploaded: 2014-01-15T13:00:00
Description: Watch this Scientific Journal Video about Using Neutron Spin Echo Resolved Grazing Incidence Scattering to Investigate Organic Solar Cell Materials at JoVE.com

AJP由EPSRC软纳米技术平台赠款EP/E046215/1提供资金。中子实验由STFC通过分配实验时间来使用 OffSpec （RB 1110285） 来支持。

1. 样品准备
<ol><li>将2个4毫米厚的硅晶片放入氧气等离子体中，清洁硅基板10分钟。</li>
	<li>在基材上涂上第一层<ol>
<li>通过 0.45μm PTFE 过滤器 （PALL） 过滤聚聚物 （3，4-乙烯二硫苯）： 聚 （苯硫酸酯） （PEDOT：PSS）。</li>
		<li>每个样品使用约 0.5 毫升，在 5，000 rpm 旋转 60 秒时将 PEDOT：PSS 薄膜旋转到两个干净的基材上。</li>
		<li>在 70 °C 的烤箱中干燥每个基板 10 分钟。</li>
	</ol>
</li>
	<li>为第二?...

<ol>
	<li>Mezei, F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Neutron+spin+echo:+A+new+concept+in+polarized+thermal+neutron+techniques.">Neutron spin echo: A new concept in polarized thermal neutron techniques.</a> Zeitschriftf&#252;r Physik A Hadrons Nuclei. 255, 146-160 (1972).</li><li>Falus, P., Vorobiev, A., Krist, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Test+of+a+two-dimensional+neutron+spin+analyzer.">Test of a two-dimensional neutron spin analyzer.</a> Physica B Condens. Matter. Mater. Phys. , 385-386 (2006).</li><li>Ashkar, R., 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=Dynamical+theory+calculations+of+spin-echo+resolved+grazing-incidence+scattering+from+a+diffraction+grating.">Dynamical theory calculations of spin-echo resolved grazing-incidence scattering from a diffraction grating.</a> J. Appl. Crystallogr. 43 (3), 455-465 (2010).</li><li>Ashkar, R., 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=Dynamical+theory:+Application+to+spin-echo+resolved+grazing+incidence+scattering+from+periodic+structures.">Dynamical theory: Application to spin-echo resolved grazing incidence scattering from periodic structures.</a> J. Appl. Phys. 110 (10), (2011).</li><li>Pynn, R., Ashkar, R., Stonaha, P., Washington, <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A.L.,Some+recent+results+using+spin+echo+resolved+grazing+incidence+scattering.">A.L.,Some recent results using spin echo resolved grazing incidence scattering.</a> SERGIS). hysica B Condens. Matter. Mater. Phys. 406 (12), 2350-2353 (2011).</li><li>Ashkar, R., 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-Echo+Resolved+Grazing+Incidence+Scattering+(SERGIS)+at+Pulsed+and+CW+Neutron+Sources.">Spin-Echo Resolved Grazing Incidence Scattering (SERGIS) at Pulsed and CW Neutron Sources.</a> J. Phy. Conf. Ser. 251 (1), (2010).</li><li>Vorobiev, 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=Phase+and+microphase+separation+of+polymer+thin+films+dewetted+from+Silicon-A+spin-echo+resolved+grazing+incidence+neutron+scattering+study.">Phase and microphase separation of polymer thin films dewetted from Silicon-A spin-echo resolved grazing incidence neutron scattering study.</a> J. Phys. Chem. B. 115 (19), 5754-5765 (2011).</li><li>Major, 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=A+spin-echo+resolved+grazing+incidence+scattering+setup+for+the+neutron+interrogation+of+buried+nanostructures.">A spin-echo resolved grazing incidence scattering setup for the neutron interrogation of buried nanostructures.</a> Rev. Sci. Instrum. 80 (12), (2009).</li><li>Parnell, A. J., Dalgliesh, R. M., Jones, R. A. L., Dunbar, A. D. F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+neutron+spin+echo+resolved+grazing+incidence+scattering+study+of+crystallites+in+organic+photovoltaic+thin+films.">A neutron spin echo resolved grazing incidence scattering study of crystallites in organic photovoltaic thin films.</a> Appl. Phys. Lett. 102, (2013).</li><li>Dalgliesh, R. M., Langridge, S., Plomp, J., De Haan, V. O., Van Well, A. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Offspec,+the+ISIS+spin-echo+reflectometer.+hysica+B+Condens..">Offspec, the ISIS spin-echo reflectometer. hysica B Condens..</a> Matter. Mater. Phys. 406 (12), 2346-2349 (2011).</li><li>Krouglov, T., de Schepper, I. M., Bouwman, W. G., Rekveldt, M. T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Real-space+interpretation+of+spin-echo+small-angle+neutron+scattering.">Real-space interpretation of spin-echo small-angle neutron scattering.</a> J. Appl. Crystallogr. 36, 117-124 (2003).</li><li>Brady, M. A., Su, G. M., Chabinyc, M. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Recent+progress+in+the+morphology+of+bulk+heterojunctionphotovoltaics.">Recent progress in the morphology of bulk heterojunctionphotovoltaics.</a> Soft Matter. 7 (23), 11065-11077 (2011).</li><li>Huang, Y. -. C., 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=Study+of+the+effect+of+annealing+process+on+the+performance+of+P3HT/PCBM+photovoltaic+devices+using+scanning-probe+microscopy..">Study of the effect of annealing process on the performance of P3HT/PCBM photovoltaic devices using scanning-probe microscopy..</a> Solar Energy Mater. Solar Cells. 93 (6-7), 888-892 (2009).</li><li>Parnell, A. 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=Depletion+of+PCBM+at+the+Cathode+Interface+in+P3HT/PCBM+Thin+Films+as+Quantified+via+Neutron+Reflectivity+Measurements.">Depletion of PCBM at the Cathode Interface in P3HT/PCBM Thin Films as Quantified via Neutron Reflectivity Measurements.</a> Adv. Mater. 22 (22), 2444-2447 (2010).</li></ol>

图1中的显微镜数据清楚地表明，在使P3HT：PCBM薄膜退化之前是平坦光滑的，热退化后，表面存在许多大型不规则的PCBM晶体，横向尺寸在1-10微米之间。这归因于 PCBM 向薄膜顶部表面的迁移，以及随后的聚合以形成大型晶体。在图4中可以看到与从已分离样品中的PCBM晶体散射相关的强SERGIS信号。如果以类似微星稀释溶液的自旋回声小角度中子散射数据来考虑数据，则 SERGIS 实...

SERGIS 技术旨在利用薄膜样品的其他散射或显微技术，产生无法获取的独特结构信息。显微镜技术通常表面有限或需要重大改变/样品准备才能查看内部结构。传统的散射技术，如反射率，可以提供关于埋藏样品结构的详细信息，作为薄膜内部的深度函数，但不能轻易探测薄膜平面中的结构。最终，希望SERGIS能够探测到这种横向结构，即使埋在薄膜样品中。此处介绍的代表性结果表明，可以观察来自不规则样本特征的 SERGIS 信号，测量的信号可以与样本中所示特征相关的特征长度比例相关联，传统显微镜技术证实了这一点。
弹性自旋回声技术是由梅泽等人开发的。1在 20 世纪 70 年代。从那时起，SERGIS技术（这是Mezei等人思想的延伸）已经成功地证明使用各种样品，如高度定期衍射光栅2-6 和圆形脱湿聚合物液滴7。Pynn和同事已经开发出一种动态理论，以模拟从高度常规样本3-6，8中散射的强散射。这项工作突出了在进行这种测量时需要考虑的许多实际方面，并导致在一个小的多国社区内不断进行对话。
如果测量的样本由扁平基板上的薄膜组成，并包含散射特征，其密度为中等密度（30纳米至5微米），从而强烈散射中子，则最有可能获得SERGIS实验的良好结果，如作者9所示。与其他将样品作为深度函数探测的既定反射技术不同，SERGIS 技术具有探测样品表面平面结构的优势。此外，使用自旋回波可消除紧密结合中子束以获得高空间或能量分辨率的要求，因此可以实现显著的通量增益。这对于放牧发生几何形状特别相关，因为需要在一个方向上强力地协调光束，因此变化非常有限。因此，使用 OffSpec 仪器，应该可以在散装和表面结构中探测从 30 nm 到 5 μm 的长度尺度。

<table border="0" cellpadding="0" cellspacing="0" width="605">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Silicon 2 in silicon substrates</td>
			<td style="width:103px;">Prolog</td>
			<td style="width:119px;"></td>
			<td style="width:167px;">4 mm thick polished one side</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Oxygen plasma</td>
			<td style="width:103px;">Diener</td>
			<td style="width:119px;"></td>
			<td>Oxygen plasma cleaning system to clean substrates prior to coating</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Poly(3,4-ethylenedioxythiophene): poly(styrenesulfonate)</td>
			<td style="width:103px;">Ossila</td>
			<td style="width:119px;"></td>
			<td>PEDOT:PSS conductive polymer layer for organic photovoltaic samples</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">0.45 &#956;m PTFE filter</td>
			<td style="width:103px;">Sigma Aldrich</td>
			<td style="width:119px;"></td>
			<td>Filer to remove aggregates from PEDOT:PSS and P3HT solutions</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Chlorobenzene</td>
			<td style="width:103px;">Sigma Aldrich</td>
			<td style="width:119px;"></td>
			<td>Solvent for P3HT</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Poly(3-hexylthiophene-2,5-diyl)</td>
			<td style="width:103px;">Ossila</td>
			<td style="width:119px;"></td>
			<td>P3HT - polymer used in polymer photovoltaics</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Spin Coater</td>
			<td style="width:103px;">Laurell</td>
			<td style="width:119px;"></td>
			<td>Deposition system for making flat thin polymer films</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Vacuum Oven</td>
			<td style="width:103px;">Binder</td>
			<td style="width:119px;"></td>
			<td>Oven fro annealing samples after preparation</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Nikon Eclipse E600 optical microscope</td>
			<td style="width:103px;">Nikon</td>
			<td style="width:119px;"></td>
			<td>Microscope</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Veeco Dimension 3100 AFM</td>
			<td style="width:103px;">Veeco</td>
			<td style="width:119px;"></td>
			<td>AFM</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Tapping mode tips (~275 kHz)</td>
			<td style="width:103px;">Olympus</td>
			<td style="width:119px;"></td>
			<td>AFM tips</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Quartz Disc</td>
			<td style="width:103px;"></td>
			<td style="width:119px;"></td>
			<td>Refrence samples for SERGIS measurement</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Spin Echo off-specular reflectometer</td>
			<td colspan="2">OffSpec at the ISIS Pulsed Neutron and Muon Source (Oxfordshire, UK)</td>
			<td>Produces pulsed neutrons 2-14 &#197;</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Neutron Detector</td>
			<td style="width:103px;">Offspec</td>
			<td style="width:119px;"></td>
			<td>vertically oriented linear scintillator detector</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">RF spin flippers</td>
			<td style="width:103px;">Offspec</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Magnetic Field Guides</td>
			<td style="width:103px;">Offspec</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Data Manipulation Software</td>
			<td style="width:103px;">Mantid</td>
			<td style="width:119px;"></td>
			<td><a href="http://www.mantidproject.org/Main_Page">http://www.mantidproject.org/Main_Page</a></td>
		</tr>
	</tbody>
</table>

using neutron spin echo resolved grazing incidence scattering to investigate organic solar cell materials

自旋回声解决放牧发生率散射 （SERGIS） 技术已用于探测与形状不规则的晶体相关的长度尺度。中子通过两个定义明确的磁场区域：一个在样品之前和之后。两个磁场区域具有相反的极性，并且经过调整，因此，在不受到干扰的情况下，中子在两个区域中飞行时，将经历相同数量的朝对方向的预兆。在这种情况下，第二臂的中子预感据说是第一个"回波"的，并且保留了束的原始极化。如果中子与样品相互作用并弹性散射，则穿过第二个手臂的路径与第一个手臂不同，并且原始极化不会恢复。中子束的去极化是一个高度敏感的探测器，角度非常小（<50μrad），但仍允许使用高强度、发散的光束。与参考样本相比，从样品反射的光束偏振程度的降低可能与样品内的结构直接相关。
与中子反射测量中观察到的散射相比，SERGIS信号通常较弱，如果被调查样本中的平面结构稀释、无序、体积小、多散射或中子散射对比度低，则不太可能观测到。因此，如果测量的样本由扁平基板上的薄膜组成，并包含包含中等尺寸特征（30 nm 至 5 μm）的高密度（30 nm 至 5 μm），从而强烈散射中子或将特征排列在晶格上，则极有可能获得良好的结果。SERGIS 技术的一个优点是它可以探测样品平面中的结构。

这里展示的 [6，6] - 苯-C61-丁酸甲基酯 （PCBM） 和聚 （3-六甲基二苯-2，5-二甲基） （P3HT） 样本具有显著意义，因为它们在有机光伏细胞12，13中广泛应用为散装异质结材料。通常，在有机光伏装置的制造过程中，P3HT：PCBM 混合溶液由混合溶液旋转铸造，在聚聚（3，4-乙二氧二苯）:p溶胶（苯硫酸酯）（PEDOT：PSS）涂层透明阳极（通常为氧化钛）上形成薄膜。然后，产生的薄膜涂在金属层中?...

Watch this Scientific Journal Video about Using Neutron Spin Echo Resolved Grazing Incidence Scattering to Investigate Organic Solar Cell Materials at JoVE.com

Using Neutron Spin Echo Resolved Grazing Incidence Scattering to Investigate Organic Solar Cell Materials

利用自旋回声解决放牧发生率散射（SERGIS）作为中子散射技术，探测不规则样品的长度尺度方面取得了进展。使用SERGIS技术对[6，6]-苯-C61-丁酸甲基酯的晶体进行了探测，结果经光学和原子力显微镜确认。

使用中子自旋回声解决放牧发生率散射调查有机太阳能电池材料

The spin echo resolved grazing incidence scattering (SERGIS) technique has been used to probe the length-scales associated with irregularly shaped ...

Research

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Angle-resolved Photoemission Spectroscopy At Ultra-low Temperatures

在极低的温度下角分辨光电子能谱

The physical properties of a material are defined by its  electronic structure. Electrons in solids are characterized by energy (&omega;)  and momentum ...

科研

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Concurrent Quantitative Conductivity and Mechanical Properties Measurements of Organic Photovoltaic Materials using AFM

并行定量的导电性和力学性能测试的有机光伏材料利用原子力显微镜

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Measuring Material Microstructure Under Flow Using 1-2 Plane Flow-Small Angle Neutron Scattering

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原位中子衍射用特制的锂离子电池

Li-ion batteries are widely used in portable electronic devices and are considered as promising candidates for higher-energy applications such as electric ...

Using Synchrotron Radiation Microtomography to Investigate Multi-scale Three-dimensional Microelectronic Packages

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Recombination Dynamics in Thin-film Photovoltaic Materials via Time-resolved Microwave Conductivity

通过时间分辨微波电导率重组动力学薄膜光伏材料

A method for investigating recombination dynamics of photo-induced charge carriers in thin film semiconductors, specifically in photovoltaic materials ...

Electrospinning of Photocatalytic Electrodes for Dye-sensitized Solar Cells

染料敏化太阳能电池的光催化电极的电纺丝

This work demonstrates a protocol to fabricate a fiber-based photoanode for dye-sensitized solar cells, consisting of a light-scattering layer made of ...

Dielectric RheoSANS &#8212; Simultaneous Interrogation of Impedance, Rheology and Small Angle Neutron Scattering of Complex Fluids

Dielectric RheoSANS ÃƒÆ’Ã‚Â¢ÃƒÂ¢Ã¢â‚¬Å¡Ã‚Â¬ÃƒÂ¢Ã¢â€šÂ¬Ã‚Â Simultaneous Interrogation of Impedance, Rheology and Small Angle Neutron Scattering of Complex Fluids

介电RheoSANS  - 阻抗，流变性和复杂流体的小角中子散射的同时拷问

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Simultaneous Multi-surface Anodizations and Stair-like Reverse Biases Detachment of Anodic Aluminum Oxides in Sulfuric and Oxalic Acid Electrolyte

阳极氧化铝在硫酸和草酸电解质中的同时多表面 Anodizations 和阶梯式反向偏置剥离

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The goal of this protocol is to present how to perform spin- and angle-resolved photoemission spectroscopy combined with polarization-variable 7-eV laser ...