Name: dielectric rheosans — simultaneous interrogation of impedance, rheology and small angle neutron scattering of complex fluids
Uploaded: 2017-04-10T12:30:00.000+00:00
Duration: 7 min 51 s
Description: Watch this Scientific Journal Video about Dielectric RheoSANS â€” Simultaneous Interrogation of Impedance, Rheology and Small Angle Neutron Scattering of Complex Fluids at JoVE.com

笔者想在这段时间内，以及国家研究委员会的支持，以确认NIST的中子研究中心CNS合作协议编号＃70NANB12H239赠款部分资金。某些商业设备，仪器，或材料在本文中被识别，以便充分地指定的实验步骤。这种标识不打算通过标准与技术研究所在暗示推荐或认可，也不是意在暗示材料或识别设备必然为宗旨的最好的。

1.安装在流变仪到SANS光束线注:参见图1的命名组件定义。 <ol><li>确保电力至所述流变仪是关闭的，换能器被锁定并安装马达空气轴承保护。关闭中子束，并关闭烤箱门。 </li><li>大底板安装在桌上，取出鼻子，安装窗口，并固定4个孔眼的安装支架流变仪的起重机适配器使得电缆不纠结，而不是扭曲。 </li><li>使用起重机，提起流变仪和从流变仪表操纵它搁置在朝外流变仪的液晶屏的表为中心，小心以引导电缆，以尽量减少缠结。 </li><li>使用SANS控制软件，送表到最小Z位置。 </li><li>取下流变仪鹤适配器和使用CR从平台提开ANE。 </li></ol> 2.介电电池组件注:参见图2的命名组件定义。 <ol><li>确保电力至所述流变仪是关闭的，换能器被锁定并安装马达空气轴承保护。在使用之前，用清洗洗涤剂溶液，然后用几个去离子水冲洗该介电杯和摆锤组件，并允许充分干燥。 </li><li>打开烤箱门，解锁换能器和卸下电机轴承锁。安装电介质的几何形状和电介质摆锤组件到流变仪的上部和下部工具安装件。使用2毫米六角扳手拧松电介质几何两个固定螺钉，并且使得它被安装在所述电介质的几何形状放置在介电盘组件。 </li><li>使用流变仪控制软件，零从样品几何下拉菜单的间隙，以及使用该轴向力下拉菜单应用10N的法向力。在压缩下，利用拧紧螺钉3-mm内六角扳手，直到电介质杯组件是完全固定到介电几何形状。 </li><li>将差距缩小到使用流变仪控制软件的测量间隙，并关闭烤箱门。确保炉子能充分与几何形状的顶部和底部的适当垂直间隙包围电介质细胞。如果需要高度调节，调节紧定螺钉，使得烤箱外壳与电介质细胞周围足够公差配合。当介质几何烤箱内符合并能进行全面的革命不沾炉壁实现足够的空间。 </li><li>卸下两个介电摆锤组件和电介质杯组件/介电几何成一体，并与所述下工具头上的流变仪对准工具更换。 </li></ol> 3.安装滑环注:参见图3步骤一步图案摘要。 <ol><li>安装电线挡板上的轴电介质的几何形状和电介质杯连接器连接到滑环连接器。 </li><li>保持滑环，以便它是同心与电介质杯组件/电介质的几何形状的轴，但是，从电介质几何凸缘上方。放置在滑环转接器（2次），使得它们的NOBS插入到钻入电介质几何孔及其基搁置在电介质几何凸缘。 </li><li>轻轻滑过滑环适配器上的滑环。滑环应围绕保持他们在的地方滑环适配器毫不费力地滑动。 </li></ol> 4.流变仪的对准注:参见图4光路的示意图。 <ol><li>紧密围绕流变仪校准工具烤箱。安装截短鼻子和样品孔（1mm宽×8毫米高），并使用流变仪控制软件，设置几何位移角0.49弧度的电动机控制下拉式菜单。 </li><li>使用SANS仪器控制软件，确保所有的中子导游被删除，打开烤箱门，使激光是可见的。通过使光束穿过烘箱并通过流变仪对准工具的中心处的狭缝横穿改变从SANS仪器控制软件表中的高度和角度进行流变仪的粗略对准。 </li><li>使用SANS仪器控制软件，调整台的高度和它的旋转来优化激光对准。注意当激光束穿过与几何位移设定在0.49拉德流变仪对准工具狭缝而不撞击其壁上和所述光束穿过在炉的中心线上的流变仪被对准。 </li></ol> 5.标定的SANS仪器的<ol><li>一旦所需的SANS仪器配置由仪器科学家对准，测量打开光束传输，空单元格散射和暗电流散射测量。 <ol><li>通过在所期望的检测器的位置3分钟执行波束透射测量执行打开光束透射测量。 </li><li>通过安装电介质的几何形状和在所期望的检测器位置测量散射测定进行空细胞散射测量。 </li><li>使用3毫米厚的片镉的该完全衰减的主光束散射信号执行暗电流散射测量。 </li></ol></li></ol> 6.连接的电气部件<ol><li>使用液晶显示屏至100mm设置的间隙。 </li><li>除去从底部工具法兰流变仪对准工具。重新安装在上部工具头和所述电介质杯组件/电介质的几何形状/滑环组件介电摆锤组件到下工具头为一体，并重新零间隙。 </li><li>确保碳刷组件是安全d可使用螺钉碳刷适配器，并固定碳刷适配器和碳刷组件使用螺钉流变仪。确保在碳电刷组件的碳刷与滑环的带槽金属环相配合。这确保了电接触的维护。 </li><li>连接在碳电刷组件和电介质摆锤组件的顶部和底部的汇流条的分别的阳针连接器的阴针连接器。确保连接到汇流条和终止在LCR测量仪的标记的屏蔽BNC电缆安装在其相应的BNC连接器。 </li><li>将标记"TO SANS"来连接到标有"AO0"的DAQ卡的BNC电缆将BNC电缆。将标记"FROM SANS"来连接到标有"AI0"的DAQ卡的BNC电缆将BNC电缆。将标记"触发"来连接到标有"AO1"的DAQ卡的BNC电缆将BNC电缆。连接BNC电缆连接到15针连接器上的流变仪的背面以标有"AI3"的BNC电缆。确保LCR测量仪和流变仪与控制计算机通信。 </li></ol> 7.准备仪器用于测量<ol><li>打开烤箱，设置间隙至100mm，和负载4毫升的炭黑分散体在碳酸亚丙酯进下平衡电介质杯组件，同时注意最小化样品的留在杯壁上。 </li><li>降低使用前面的液晶屏的几何形状到40毫米。设置使用电动机控制设置，以1弧度/秒的流变仪控制软件的速度。使用转换选项在流变仪上，降低电介质摆锤组件，直到间隙距离为0.5mm。 </li><li>在使用设备的软件，去电介质几何测量间隙，以及使用该马达控制设置为0弧度/秒设定流变仪控制软件的马达速度。在此阶段，所述样品是负载编辑。 注意:检查样品的液位一次，以确保样品的水平填充一路库埃特墙面无满溢。 </li><li>通过填充具有所需溶剂内部介电摆锤组件壁安装溶剂捕集器并将其放置在溶剂捕集器在电介质杯组件的边缘上。 </li></ol> 8.运行介电RheoSANS实验<ol><li>配置标有"TA_ARES_FlowSweep.vi"代码。一个GUI会出现与指定电介质RheoSANS实验的实验运行条件可修改的字段。设置按以下顺序这些字段。 <ol><li>指定的日志文件和日志文件的基本名称的路径。按菜单栏上的"运行"箭头按钮运行代码。 </li><li>选择流变参数 - 起始剪切速率（25弧度/秒），结束剪切速率（1弧度/秒），剪切速率的点的数量（6）和所述点是否应该洛加尔ithmically或线性间隔（单选按钮）。选择温度至25℃该实验。选择预剪切条件下（如果需要的话，使单选按钮为"ON"） - 在该实验中，使用600秒的25弧度/秒预剪切用300秒的等待时间在预剪切步骤之后。 </li><li>指定每个剪切速率和收集率的时间。启用握手单选按钮。上的测试参数选项卡中选择对数或线性扫描 - 如果单选按钮是绿色的，N个点的列表将被从对数分剪切速率至马克斯·希尔速率间隔开。 </li><li>如果需要的话通过"离散值"选项卡中指定的离散的剪切速率和时间。选择的频点的数量，频率最低，频率最高默认。设置时间相关的频率 - 指定所有剪切速率所需的时间取决于频率。设置为稳定状态时的时间 - 设置的时间，该代码将测量电介质参数的量在一个固定的频率uency作为时间为每个剪切速率的函数。 </li><li>指定的信号类型和幅度。指定以平均周期数和测量时间。 </li></ol></li><li>打开自动记录的SANS计算机上。设置SANS配置。选择配置，并指定运行时间是至少1分钟，长于包含在代码剪切速率列表内的总时间。 注意:当构造实现VIPER应改为"DIO STAT 16"，其指示其将等待从数据采集卡模拟信号来改变。 </li><li>配置流变仪控制软件。在实验中选项卡，在"程序"，按"打开程序文件"下拉菜单。导航到标有"介电RheoSANS脚本文件"的程序文件。确保流变仪已准备好执行实验。 </li><li>当SANS准备就绪，确保控制软件进行配置和流变仪续ROL软件脚本文件打开时，按"参数设置"。这会触发指定实验的执行，所有的数据应在整个预编程的样品运行记录。 </li></ol> 9.结束实验的<ol><li>关闭中子束和禁用自动登录。卸载样品并从流变仪去除电介质杯和摆锤组件。安装电动机空气轴承保护并锁定换能器。 </li><li>关闭计算机电源，LCR测试仪，和流变仪电源。断开气路。断开所有BNC电缆，并重新安装起重机提升到流变仪。 </li><li>卸载截断吻。重新装上流变仪的起重机适配器。提起桌上的流变仪和放置到流变仪表，确保电缆保持解开。 </li></ol><img alt="图1" src="/files/ftp_upload/55318/55318fig1.jpg" /> 图1:A） -联合电子）图片<html> SANS的光束线和流变仪必要的mponents对被标记和下面定义的光束线安装流变仪。 <a href="https://ecsource-jove-com.bdigitaluss.remotexs.co/files/ftp_upload/55318/55318fig1large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图2" src="/files/ftp_upload/55318/55318fig2.jpg" /> 图2: 组件图片的介质RheoSANS几何与标签定义以下术语。 <a href="https://ecsource-jove-com.bdigitaluss.remotexs.co/files/ftp_upload/55318/55318fig2large.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/55318/55318fig3.jpg" /> 图3:程序a.-d.）图片用于安装滑环到电介质RheoSANS几何，和e）完全组装介电RheoSANS几何的图片。ove.com/files/ftp_upload/55318/55318fig3large.jpg"目标=‘_空白’&gt;点击此处查看该图的放大版本。 <img alt="图4" src="/files/ftp_upload/55318/55318fig4.jpg" /> 图4: 通过烤箱几何结构和介电RheoSANS几何光路示意图。 <a href="https://ecsource-jove-com.bdigitaluss.remotexs.co/files/ftp_upload/55318/55318fig4large.jpg" target="_blank">请点击此处查看该图的放大版本。</a>

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	<li>Macosko, C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Rheology:+Principles,+Measurements+and+Applications.">Rheology: Principles, Measurements and Applications.</a> Powder Technology. 86 (3), (1996).</li><li>Barsoukov, E., Macdonald, J. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Impedance Spectroscopy Theory, Experiment, and Applications. , (2010).</li><li>Pelster, R., Simon, U. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nanodispersions+of+conducting+particles:+Preparation,+microstructure+and+dielectric+properties.">Nanodispersions of conducting particles: Preparation, microstructure and dielectric properties.</a> Colloid Polym. Sci. 277 (1), 2-14 (1999).</li><li>Hollingsworth, A. D., Saville, D. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Dielectric+spectroscopy+and+electrophoretic+mobility+measurements+interpreted+with+the+standard+electrokinetic+model.">Dielectric spectroscopy and electrophoretic mobility measurements interpreted with the standard electrokinetic model.</a> J. Colloid Interface Sci. 272 (1), 235-245 (2004).</li><li>Mewis, J., Spaull, A. J. B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Rheology+of+concentrated+dispersions.">Rheology of concentrated dispersions.</a> Adv. Colloid Interface Sci. 6 (3), 173-200 (1976).</li><li>Mijovi&#263;, J., Lee, H., Kenny, J., Mays, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Dynamics+in+Polymer-Silicate+Nanocomposites+As+Studied+by+Dielectric+Relaxation+Spectroscopy+and+Dynamic+Mechanical+Spectroscopy.">Dynamics in Polymer-Silicate Nanocomposites As Studied by Dielectric Relaxation Spectroscopy and Dynamic Mechanical Spectroscopy.</a> Macromolecules. 39 (6), 2172-2182 (2006).</li><li>Newbloom, G. M., Weigandt, K. M., Pozzo, D. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrical,+Mechanical,+and+Structural+Characterization+of+Self-Assembly+in+Poly(3-hexylthiophene)+Organogel+Networks.">Electrical, Mechanical, and Structural Characterization of Self-Assembly in Poly(3-hexylthiophene) Organogel Networks.</a> Macromolecules. 45 (8), 3452-3462 (2012).</li><li>Fowler, J. N., Kirkwood, J., Wagner, N. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Rheology+and+microstructure+of+shear+thickening+fluid+suspoemulsions.">Rheology and microstructure of shear thickening fluid suspoemulsions.</a> Appl. Rheol. 24 (4), 23049 (2014).</li><li>Wagner, N. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Rheo-optics.">Rheo-optics.</a> Curr. Opin. Colloid Interface Sci. 3 (4), 391-400 (1998).</li><li>Callaghan, P. 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=Rheo-NMR:+nuclear+magnetic+resonance+and+the+rheology+of+complex+fluids.">Rheo-NMR: nuclear magnetic resonance and the rheology of complex fluids.</a> Reports Prog. Phys. 62 (4), 599-670 (1999).</li><li>Gurnon, 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=Measuring+Material+Microstructure+Under+Flow+Using+1-2+Plane+Flow-Small+Angle+Neutron+Scattering.">Measuring Material Microstructure Under Flow Using 1-2 Plane Flow-Small Angle Neutron Scattering.</a> J. Vis. Exp. (84), e51068 (2014).</li><li>Calabrese, M. A., Rogers, S. A., Murphy, R. P., Wagner, N. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+rheology+and+microstructure+of+branched+micelles+under+shear.">The rheology and microstructure of branched micelles under shear.</a> J. Rheol. 59 (5), 1299-1328 (2015).</li><li>Helgeson, M. E., Vasquez, P. A., Kaler, E. W., Wagner, N. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Rheology+and+spatially+resolved+structure+of+cetyltrimethylammonium+bromide+wormlike+micelles+through+the+shear+banding+transition.">Rheology and spatially resolved structure of cetyltrimethylammonium bromide wormlike micelles through the shear banding transition.</a> J. Rheol. 53 (3), 727 (2009).</li><li>Calabrese, M. 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=An+optimized+protocol+for+the+analysis+of+time-resolved+elastic+scattering+experiments.">An optimized protocol for the analysis of time-resolved elastic scattering experiments.</a> Soft Matter. 12 (8), 2301-2308 (2016).</li><li>Eberle, A. P. R., Porcar, L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Flow-SANS+and+Rheo-SANS+applied+to+soft+matter.">Flow-SANS and Rheo-SANS applied to soft matter.</a> Curr. Opin. Colloid Interface Sci. 17 (1), 33-43 (2012).</li><li>Campos, J. W., 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=Investigation+of+carbon+materials+for+use+as+a+flowable+electrode+in+electrochemical+flow+capacitors.">Investigation of carbon materials for use as a flowable electrode in electrochemical flow capacitors.</a> Electrochim. Acta. 98, 123-130 (2013).</li><li>Duduta, 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=Semi-solid+lithium+rechargeable+flow+battery.">Semi-solid lithium rechargeable flow battery.</a> Adv. Energy Mater. 1 (4), 511-516 (2011).</li><li>Mewis, J., de Groot, L. M., Helsen, J. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Dielectric+Behaviour+of+Flowing+Thixotropic+Suspensions.">Dielectric Behaviour of Flowing Thixotropic Suspensions.</a> Colloids Surf. 22, (1987).</li><li>Richards, J. J., Wagner, N. J., Butler, P. D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+Strain-Controlled+RheoSANS+Instrument+for+the+Measurement+of+the+Microstructural,+Electrical+and+Mechanical+Properties+of+Soft+Materials.">A Strain-Controlled RheoSANS Instrument for the Measurement of the Microstructural, Electrical and Mechanical Properties of Soft Materials.</a> Rev. Sci. Instr. , (2016).</li><li>Youssry, 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=Non-aqueous+carbon+black+suspensions+for+lithium-based+redox+flow+batteries:+rheology+and+simultaneous+rheo-electrical+behavior.">Non-aqueous carbon black suspensions for lithium-based redox flow batteries: rheology and simultaneous rheo-electrical behavior.</a> Phys. Chem. Chem. Phys. PCCP. 15 (34), 14476-14486 (2013).</li><li>Cho, B. -. K., Jain, A., Gruner, S. M., Wiesner, U. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Mesophase+structure-mechanical+and+ionic+transport+correlations+in+extended+amphiphilic+dendrons.">Mesophase structure-mechanical and ionic transport correlations in extended amphiphilic dendrons.</a> Sci. 305 (5690), 1598-1601 (2004).</li><li>Kiel, J. W., MacKay, M. E., Kirby, B. J., Maranville, B. B., Majkrzak, C. F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Phase-sensitive+neutron+reflectometry+measurements+applied+in+the+study+of+photovoltaic+films.">Phase-sensitive neutron reflectometry measurements applied in the study of photovoltaic films.</a> J. Chem. Phys. 133 (7), 1-7 (2010).</li><li>L&#243;pez-Barr&#242;n, C. R., Chen, R., Wagner, N. J., Beltramo, P. J. <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+Pluronic+F127+Diacrylate+in+Ethylammonium+Nitrate:+Structure,+Rheology,+and+Ionic+Conductivity+before+and+after+Photo-Cross-Linking.">Self-Assembly of Pluronic F127 Diacrylate in Ethylammonium Nitrate: Structure, Rheology, and Ionic Conductivity before and after Photo-Cross-Linking.</a> Macromolecules. 49 (14), 5179-5189 (2016).</li></ol>

作者什么都没有透露。

介电RheoSANS实验同时措施作为其经历一个预定义变形的材料的流变学，电气和微观结构的响应。这里示出的例子是形成在电化学流动池使用的导电性添加剂的导电碳黑悬浮液中。介电RheoSANS仪器使得窄间隙库埃特细胞内剪切的径向平面的询问而不损害或者电或流变测量的保真度。此外，该几何形状允许对原始信号，扭矩，电阻，和相移的转换，到适当的固有的变量，如剪切应力，电导率和电容率。...

宏观性质的测量通常被用来获得基本的洞察胶体材料和自组装系统的性质，通常为了提高配方性能的发展理解的目的。具体地，流变学的领域中，其测量的流体的所施加的应力或变形的动态响应，同时提供了在平衡条件下，并且还远离平衡有价值的见解胶体行为，如处理消费者和工业流体的1次流变测试期间，凝胶，以及眼镜，也可用于测量流变学参数，例如粘度，由配方师的目标。虽然流变性是材料特性的强大的探针，它是胶体信息在微观水平的间接测量，例如，我们的基本胶态行为的理解可以通过结合采用c流变学测量大大增强omplementary技术。 一种这样的正交的技术是阻抗谱。阻抗谱是介电弛豫特性，其测量的材料所施加的振荡电场的响应的散装探针。 2从电松弛模式，即包括电荷传输和偏振材料内活性的阻抗谱的结果。 3，4这些测量提供特别是当与流变结合胶体行为的其他证据。 5因此，在探讨带电胶体分散体，蛋白质，离子表面活性剂，纳米复合材料，和其他系统的这些技术的组合是尤其相关。 6,7 在胶体行为调查的基本利益是材料的microstruc<html>真实存在。胶体流体的微结构被认为是编码所有的必需的信息来重构其两个流变和电气特性。从根本上说，我们寻求测量的纳米级微结构特征，导致测量的响应材料的快照。由于许多复杂流体在他们的历史进程依赖的复杂性，多在微观结构表征的努力都集中在使在材料的原位测量，因为它会变形。这提出了挑战实验者制定方法，以便能够使下例如稳态剪切，其中，所述粒子的速度取得了直接可视化本质上具有挑战性的纳米尺寸的颗粒的测量值。下流动的材料的微结构的直接测量已采取许多形式，从流变光学，流变显微镜和甚至流变-NMR。 8，9，屁股="外部参照"&gt; 10种小角散射方法，并且特别是小角中子散射（SANS）技术，已经证明自己有效在包括所有三个平面的堆积剪切场测量样品的时间平均微结构在稳定状态下剪切。 11，12，13然而，新的数据采集技术允许结构瞬变与时间分辨率细如10毫秒被捕获。 14 原位散射方法的不同的确结合流变数百最近的研究已经证明非常宝贵的。 15 一种新兴的工程挑战是使用胶态悬浮液在半固体液流电池电极的导电添加剂。 16在本申请中，导电胶体颗粒必须保持而脑膜电渗滤网络IAL通过电化学流动池泵送。这些材料的性能要求，要求他们保持不超过一个大范围剪切速率的流变性能的不利影响高导电性。 17因此，非常希望能够使胶体特性的测定以量化和表征这些材料远离他们的平衡状态的基本的流变学和电响应稳定和时间依赖性的剪切条件下。在这方面阻碍了进一步的理论发展的一个显著复杂的因素是炭黑浆料的触变性质。 18个这些历史流变依赖和电气特性做实验非常难以重现;由此，使得难以比较使用不同的方案来测量的数据集。此外，到目前为止还没有出现能够执行所有三个没有单一的几何形状，dielectric，流变学和微观结构表征，同时进行。同时测量是重要的，因为流动可以改变结构，使得处理的材料的其余部分的测量可能不提供下流动的特性，这是它们的使用更相关的准确指示。此外，因为许多炭黑浆料的测量的属性是依赖于几何形状，存在与比较从上不同的仪器相同的样品获得的数据的并发症。 19 为了满足计量这一挑战，我们开发的NIST中子研究中心和特拉华大学能够在原位阻抗谱新介质RheoSANS几何形状，在商业应变任意变形下材料的流变和SANS测量控制流变仪。这是通过开发一个能够测量的微观结构，ELECTRICA的库埃特几何启用升和两个同心圆柱体的间隙之间密闭的材料的流变响应。作为外筒旋转时，通过将样品的变形所施加的转矩的内筒上测量，并且阻抗测量跨越间隙径向制成。汽缸是从钛加工成是透明的中子和足以承受在流变仪中所经历的剪切应力。我们通过库埃特的径向位置进行测量SANS，并且已经证明它是能够测量从在经历变形样品高质量SANS图案。这样一来，所有的三个测量是对样品中感兴趣的同一区域，因为它经历了一个定义良好的变形轮廓制作。本文的目标是描述在电介质库埃特几何形状，其安装到所述RheoSANS仪器，和同时测量的成功执行。该流变仪可在NIST中心中子研究标准与技术研究所的国家。它被设计为在NG-7 SANS束线工作。我们已经提供了附图和已经被加工，并且为了使该测量组装自定义组件的详细描述。

<table><tbody><tr><td>ARES G2 Rheometer</td><td>TA Instruments</td><td>401000.501</td><td>Rheometer</td></tr><tr><td>ARES G2-DETA ACCY Kit</td><td>TA Instruments</td><td>402551.901</td><td>BNC Connectors</td></tr><tr><td>Geometry ARES 25 mm DETA</td><td>TA Instruments</td><td>402553.901</td><td>Dielectric Geometry</td></tr><tr><td>ARES G2 Forced Convection Oven</td><td>TA Instruments</td><td>401892.901</td><td>FCO</td></tr><tr><td>Agilent E4980A LCR Meter</td><td>TA Instruments</td><td>613.04946</td><td>LCR Meter</td></tr><tr><td>USB-6001</td><td>National Instruments</td><td>NI USB-6001</td><td>Data Acquisiton Card</td></tr><tr><td>Vulcan XC72R</td><td>Cabot</td><td>Vulcan XC72R</td><td></td></tr><tr><td>Propylene Carbonate</td><td>Aldrich</td><td>310328</td><td></td></tr><tr><td>LabVIEW&amp;nbsp; System Design Software</td><td>National Instruments</td><td>776671-35</td><td>Control Software&amp;nbsp;</td></tr></tbody></table>

dielectric rheosans &#8212; simultaneous interrogation of impedance, rheology and small angle neutron scattering of complex fluids

一种用于能够复杂流体的电气，机械和微结构性质的同时询问的一个新的电介质RheoSANS仪器的操作过程被呈现。该仪器由含有安装在市售的流变仪的改性强制对流烤箱内的库埃特几何形状。本仪器可用于在小角中子散射（SANS）在美国国家标准与技术研究院（NIST）中子研究中心（NCNR）光束线使用。库埃特几何被加工成透明的中子，并提供了电性能和钛汽缸之间密闭，同时样品经历任意变形的样品的微结构性质的测量。这些测量的同步是通过使用监视和控制的预定的实验方案的执行可定制程序使能。这里描述的是一个协议，以执行流扫描实验，其中剪切速率对数从最大值步进到保持在对于指定的时间周期中的每一步骤的最小值，而依赖于频率的介电测量制成。代表性的结果从由分散在碳酸丙烯酯炭黑聚集体组成的凝胶的样品所示。由于凝胶发生稳态剪切，炭黑网络是机械变形，这会导致与包含炭黑网络键断裂有关的传导率的初始降低。然而，在高剪切速率，电导率恢复被剪切增稠的发病有关。总的来说，这些结果证明了使用电介质RheoSANS几何这些悬浮液的流变电微结构性质的同时测量的效用。

由介电RheoSANS实验代表性的结果示于图5和6。这些数据被采取在碳酸丙烯酯中的悬浮液的导电炭黑。这些聚集体絮凝由于在形成的凝胶被导电相对低的固体加载量吸引相互作用。这种悬浮液的流变性和传导性反应是一个活跃的研究领域和目前的调查设法了解这些测量的微观起源。介电RheoSANS仪器是唯一适合，因为它同时探测的材料的电气和机械性能...

Watch this Scientific Journal Video about Dielectric RheoSANS â€” Simultaneous Interrogation of Impedance, Rheology and Small Angle Neutron Scattering of Complex Fluids at JoVE.com

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

在这里，我们提出了一个程序，用于同时阻抗，流变学和中子散射的从下剪切流软物质材料中测量。

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

A procedure for the operation of a new dielectric RheoSANS instrument capable of simultaneous interrogation of the electrical, mechanical and ...

dielectric-rheosans-simultaneous-interrogation-impedance-rheology

Universidad San Sebastian

Research

JoVE Journal

Engineering

10.3K 次观看.  National Institute of Standards and Technology. 在这里，我们提出了一个程序，用于同时阻抗，流变学和中子散射的从下剪切流软物质材料中测量。 

视频: Dielectric RheoSANS — Simultaneous Interrogation of Impedance, Rheology and Small Angle Neutron Scattering of Complex Fluids

Confocal Imaging of Confined Quiescent and Flowing Colloid-polymer Mixtures

The behavior of confined colloidal suspensions with attractive interparticle interactions is critical to the rational design of materials for directed assembly1-3, drug delivery4, improved hydrocarbon recovery5-7, and flowable electrodes for energy storage8. Suspensions containing fluorescent colloids and non-adsorbing polymers are appealing model systems, as the ratio of the polymer radius of gyration to the particle radius&#160;and concentration of polymer control the range and strength of the interparticle attraction, respectively. By tuning the polymer properties and the volume fraction of the colloids, colloid fluids, fluids of clusters, gels, crystals, and glasses can be obtained9.&#160;Confocal microscopy, a variant of fluorescence microscopy, allows an optically transparent and fluorescent sample to be imaged with high spatial and temporal resolution in three dimensions. In this technique, a small pinhole or slit blocks the emitted fluorescent light from regions of the sample that are outside the focal volume of the microscope optical system. As a result, only a thin section of the sample in the focal plane is imaged. This technique is particularly well suited to probe the structure and dynamics in dense colloidal suspensions at the single-particle scale: the particles are large enough to be resolved using visible light and diffuse slowly enough to be captured at typical scan speeds of commercial confocal systems10. Improvements in scan speeds and analysis algorithms have also enabled quantitative confocal imaging of flowing suspensions11-16,37.&#160;In this paper, we demonstrate confocal microscopy experiments to probe the confined phase behavior and flow properties of colloid-polymer mixtures. We first prepare colloid-polymer mixtures that are density- and refractive-index matched. Next, we report a standard protocol for imaging quiescent dense colloid-polymer mixtures under varying confinement in thin wedge-shaped cells. Finally, we demonstrate a protocol for imaging colloid-polymer mixtures during microchannel flow.

Confocal microscopy is used to image quiescent and flowing colloid-polymer mixtures, which are studied as model systems for attractive suspensions. Image analysis algorithms are used to calculate structural and dynamic metrics for the colloidal particles that measure changes due to geometric confinement.

密闭静态和流动胶体聚合物混合物的共聚焦成像

The behavior of confined colloidal suspensions with attractive interparticle interactions is critical to the rational design of materials for directed ...

科研

化学

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

A new small-angle neutron scattering (SANS) sample environment optimized for studying the microstructure of complex fluids under simple shear flow is presented. The SANS shear cell consists of a concentric cylinder Couette geometry that is sealed and rotating about a horizontal axis so that the vorticity direction of the flow field is aligned with the neutron beam enabling scattering from the 1-2 plane of shear (velocity-velocity gradient, respectively). This approach is an advance over previous shear cell sample environments as there is a strong coupling between the bulk rheology and microstructural features in the 1-2 plane of shear. Flow-instabilities, such as shear banding, can also be studied by spatially resolved measurements. This is accomplished in this sample environment by using a narrow aperture for the neutron beam and scanning along the velocity gradient direction. Time resolved experiments, such as flow start-ups and large amplitude oscillatory shear flow are also possible by synchronization of the shear motion and time-resolved detection of scattered neutrons. Representative results using the methods outlined here demonstrate the useful nature of spatial resolution for measuring the microstructure of a wormlike micelle solution that exhibits shear banding, a phenomenon that can only be investigated by resolving the structure along the velocity gradient direction. Finally, potential improvements to the current design are discussed along with suggestions for supplementary experiments as motivation for future experiments on a broad range of complex fluids in a variety of shear motions.

A shear cell is developed for small-angle neutron scattering measurements in the velocity-velocity gradient plane of shear and is used to characterize complex fluids. Spatially resolved measurements in the velocity gradient direction are possible for studying shear-banding materials. Applications include investigations of colloidal dispersions, polymer solutions, and self-assembled structures.

测量材料在微流使用1-2面流小角中子散射

A new small-angle neutron scattering (SANS) sample environment optimized for studying the microstructure of complex fluids under simple shear flow is ...

工程学

Quantitative and Qualitative Examination of Particle-particle Interactions Using Colloidal Probe Nanoscopy

Colloidal Probe Nanoscopy (CPN), the study of the nano-scale interactive forces between a specifically prepared colloidal probe and any chosen substrate using the Atomic Force Microscope (AFM), can provide key insights into physical interactions present within colloidal systems. Colloidal systems are widely existent in several applications including, pharmaceuticals, foods, paints, paper, soil and minerals, detergents, printing and much more.1-3 Furthermore, colloids can exist in many states such as emulsions, foams and suspensions. Using colloidal probe nanoscopy one can obtain key information on the adhesive properties, binding energies and even gain insight into the physical stability and coagulation kinetics of the colloids present within. Additionally, colloidal probe nanoscopy can be used with biological cells to aid in drug discovery and formulation development. In this paper we describe a method for conducting colloidal probe nanoscopy, discuss key factors that are important to consider during the measurement, and show that both quantitative and qualitative data that can be obtained from such measurements.

Colloidal probe nanoscopy can be used within a variety of fields to gain insight into the physical stability and coagulation kinetics of colloidal systems and aid in drug discovery and formulation sciences using biological systems. The method described within provides a quantitative and qualitative means to study such systems.

粒子粒子相互作用采用胶体探针纳米显微定量和定性检查

Colloidal Probe Nanoscopy (CPN), the study of the nano-scale interactive forces between a specifically prepared colloidal probe and any chosen substrate ...

An Analog Macroscopic Technique for Studying Molecular Hydrodynamic Processes in Dense Gases and Liquids

An analog, macroscopic method for studying molecular-scale hydrodynamic processes in dense gases and liquids is described. The technique applies a standard fluid dynamic diagnostic, particle image velocimetry (PIV), to measure: i) velocities of individual particles (grains), extant on short, grain-collision time-scales, ii) velocities of systems of particles, on both short collision-time- and long, continuum-flow-time-scales, iii) collective hydrodynamic modes known to exist in dense molecular fluids, and iv) short- and long-time-scale velocity autocorrelation functions, central to understanding particle-scale dynamics in strongly interacting, dense fluid systems. The basic system is composed of an imaging system, light source, vibrational sensors, vibrational system with a known media, and PIV and analysis software. Required experimental measurements and an outline of the theoretical tools needed when using the analog technique to study molecular-scale hydrodynamic processes are highlighted. The proposed technique provides a relatively straightforward alternative to photonic and neutron beam scattering methods traditionally used in molecular hydrodynamic studies.

An experimentally accessible analog method for studying molecular hydrodynamic processes in dense fluids is presented. The technique uses particle image velocimetry of vibrated, high-restitution grain piles and allows direct, macroscopic observation of dynamical processes known and predicted to exist in strongly interacting, high density gases and liquids.

一种研究稠密气体和液体分子流体力学过程的模拟宏观技术

An analog, macroscopic method for studying molecular-scale hydrodynamic processes in dense gases and liquids is described. The technique applies a ...

Combining Microfluidics and Microrheology to Determine Rheological Properties of Soft Matter during Repeated Phase Transitions

The microstructure of soft matter directly impacts macroscopic rheological properties and can be changed by factors including colloidal rearrangement during previous phase changes and applied shear. To determine the extent of these changes, we have developed a microfluidic device that enables repeated phase transitions induced by exchange of the surrounding fluid and microrheological characterization while limiting shear on the sample. This technique is &#181;2rheology, the combination of microfluidics and microrheology. The microfluidic device is a two-layer design with symmetric inlet streams entering a sample chamber that traps the gel sample in place during fluid exchange. Suction can be applied far away from the sample chamber to pull fluids into the sample chamber. Material rheological properties are characterized using multiple particle tracking microrheology (MPT). In MPT, fluorescent probe particles are embedded into the material and the Brownian motion of the probes is recorded using video microscopy. The movement of the particles is tracked and the mean-squared displacement (MSD) is calculated. The MSD is related to macroscopic rheological properties, using the Generalized Stokes-Einstein Relation. The phase of the material is identified by comparison to the critical relaxation exponent, determined using time-cure superposition. Measurements of a fibrous colloidal gel illustrate the utility of the technique. This gel has a delicate structure that can be irreversibly changed when shear is applied. &#181;2rheology data shows that the material repeatedly equilibrates to the same rheological properties after each phase transition, indicating that phase transitions do not play a role in microstructural changes. To determine the role of shear, samples can be sheared prior to injection into our microfluidic device. &#181;2rheology is a widely applicable technique for the characterization of soft matter enabling the determination of rheological properties of delicate microstructures in a single sample during phase transitions in response to repeated changes in the surrounding environmental conditions.

We demonstrate the fabrication and use of a microfluidic device that enables multiple particle tracking microrheology measurements to study the rheological effects of repeated phase transitions on soft matter.

微流体和 Microrheology 相结合测定软物质在重复相变过程中的流变特性

The microstructure of soft matter directly impacts macroscopic rheological properties and can be changed by factors including colloidal rearrangement ...

Studying Large Amplitude Oscillatory Shear Response of Soft Materials

We investigate the sequence of physical processes exhibited during large amplitude oscillatory shearing (LAOS) of polyethylene oxide (PEO) in dimethyl sulfoxide (DMSO) and xanthan gum in water &#8212; two concentrated polymer solutions used as viscosifiers in foods, enhanced oil recovery, and soil remediation. Understanding the nonlinear rheological behavior of soft materials is important in the design and controlled manufacturing of many consumer products. It is shown how the response to LAOS of these polymer solutions can be interpreted in terms of a clear transition from linear viscoelasticity to viscoplastic deformation and back again during a period. The LAOS results are analyzed via the fully quantitative Sequence of Physical Processes (SPP) technique, using free MATLAB-based software. A detailed protocol of performing a LAOS measurement with a commercial rheometer, analyzing nonlinear stress responses with the freeware, and interpreting physical processes under LAOS is presented. It is further shown that, within the SPP framework, a LAOS response contains information regarding the linear viscoelasticity, the transient flow curves, and the critical strain responsible for the onset of nonlinearity.

We present a detailed protocol outlining how to perform nonlinear oscillatory shear rheology on soft materials, and how to run the SPP-LAOS analysis to understand the responses as a sequence of physical processes.

软材料大振幅振荡剪切响应的研究

We investigate the sequence of physical processes exhibited during large amplitude oscillatory shearing (LAOS) of polyethylene oxide (PEO) in dimethyl ...

Assembly and Characterization of Polyelectrolyte Complex Micelles

Polyelectrolyte complex micelles (PCMs), core-shell nanoparticles formed by self-assembly of charged polymers in aqueous solution, provide a powerful platform for exploring the physics of polyelectrolyte interactions and also offer a promising solution to the pressing problem of delivering therapeutic oligonucleotides in vivo. Developing predictive structure-property relationships for PCMs has proven difficult, in part due to the presence of strong kinetic traps during nanoparticle self-assembly. This article discusses criteria for choosing polymers for PCM construction and provides protocols based on salt annealing that enable assembly of repeatable, low-polydispersity nanoparticles. We also discuss PCM characterization using light scattering, small-angle X-ray scattering, and electron microscopy.

We provide protocols and representative data for designing, assembling, and characterizing polyelectrolyte complex micelles, core-shell nanoparticles formed by polyelectrolytes and hydrophilic charged-uncharged block copolymers.

聚电解质复合微晶体的组装与特性

Polyelectrolyte complex micelles (PCMs), core-shell nanoparticles formed by self-assembly of charged polymers in aqueous solution, provide a powerful ...

Study of Protein Dynamics via Neutron Spin Echo Spectroscopy

Most human body proteins' activity and functionality are related to configurational changes of entire subdomains within the protein crystal structure. The crystal structures build the basis for any calculation that describes the structure or dynamics of a protein, most of the time with strong geometrical restrictions. However, these restrictions from the crystal structure are not present in the solution. The structure of the proteins in the solution may differ from the crystal due to rearrangements of loops or subdomains on the pico to nanosecond time scale (i.e., the internal protein dynamics time regime). The present work describes how slow motions on timescales of several tens of nanoseconds can be accessed using neutron scattering. In particular, the dynamical characterization of two major human proteins, an intrinsically disordered protein that lacks a well-defined secondary structure and a classical antibody protein, is addressed by neutron spin echo spectroscopy (NSE) combined with a wide range of laboratory characterization methods. Further insights into protein domain dynamics were achieved using mathematical modeling to describe the experimental neutron data and determine the crossover between combined diffusive and internal protein motions. The extraction of the internal dynamic contribution to the intermediate scattering function obtained from NSE, including the timescale of the various movements, allows further vision into the mechanical properties of single proteins and the softness of proteins in their nearly natural environment in the crowded protein solution.

Study of Protein Dynamics via Neutron Spin Echo Spectroscopy

The present protocol describes methods for investigating the structure and dynamics of two model proteins that have an important role in human health. The technique combines bench-top biophysical characterization with neutron spin echo spectroscopy to access the dynamics at time and length scales relevant for protein interdomain motions.

通过中子自旋回声光谱研究蛋白质动力学

Most human body proteins' activity and functionality are related to configurational changes of entire subdomains within the protein crystal structure. The ...

Studying Soft-matter and Biological Systems over a Wide Length-scale from Nanometer and Micrometer Sizes at the Small-angle Neutron Diffractometer KWS-2

The KWS-2 SANS diffractometer is dedicated to the investigation of soft matter and biophysical systems covering a wide length scale, from nm to &#181;m. The instrument is optimized for the exploration of the wide momentum transfer Q range between 1x10-4 and 0.5 &#197;-1 by combining classical pinhole, focusing (with lenses), and time-of-flight (with chopper) methods, while simultaneously providing high-neutron intensities with an adjustable resolution. Because of its ability to adjust the intensity and the resolution within wide limits during the experiment, combined with the possibility to equip specific sample environments and ancillary devices, the KWS-2 shows a high versatility in addressing the broad range of structural and morphological studies in the field. Equilibrium structures can be studied in static measurements, while dynamic and kinetic processes can be investigated over time scales between minutes to tens of milliseconds with time-resolved approaches. Typical systems that are investigated with the KWS-2 cover the range from complex, hierarchical systems that exhibit multiple structural levels (e.g., gels, networks, or macro-aggregates) to small and poorly-scattering systems (e.g., single polymers or proteins in solution). The recent upgrade of the detection system, which enables the detection of count rates in the MHz range, opens new opportunities to study even very small biological morphologies in buffer solution with weak scattering signals close to the buffer scattering level at high Q.
In this paper, we provide a protocol to investigate samples with characteristic size levels spanning a wide length scale and exhibiting ordering in the mesoscale structure using KWS-2. We present in detail how to use the multiple working modes that are offered by the instrument and the level of performance that is achieved.

Here, we present a protocol to investigate soft matter and biophysical systems over a wide mesoscopic length scale, from nm to &#181;m that involves the use of the KWS-2 SANS diffractometer at high intensities and an adjustable resolution.

在小角度中子衍射仪KWS-2研究软物质和生物系统在广泛的长度尺度从纳米，微米尺寸

The KWS-2 SANS diffractometer is dedicated to the investigation of soft matter and biophysical systems covering a wide length scale, from nm to &#181;m. ...

生物工程

Measuring the Time-Evolution of Nanoscale Materials with Stopped-Flow and Small-Angle Neutron Scattering

This paper presents the use of a stopped-flow small-angle neutron-scattering (SANS) sample environment to quickly mix liquid samples and study nanoscale kinetic processes on time scales of seconds to minutes. The stopped-flow sample environment uses commercially available syringe pumps to mix the desired volumes of liquid samples that are then injected through a dynamic mixer into a quartz glass cell in approximately 1 s. Time-resolved SANS data acquisition is synced with the sample mixing to follow the evolution of the nanostructure in solution after mixing. 
To make the most efficient use of neutron beam time, we use a series of flow selector valves to automatically load, rinse, and dry the cell between measurements, allowing for repeated data collection throughout multiple sample injections. Sample injections are repeated until sufficient neutron scattering statistics are collected. The mixing setup can be programmed to systematically vary conditions to measure the kinetics at different mixing ratios, sample concentrations, additive concentrations, and temperatures. The minimum sample volume required per injection is approximately 150 &#181;L depending on the path length of the quartz cell. 
Representative results using this stopped-flow sample environment are presented for rapid lipid exchange kinetics in the presence of an additive, cyclodextrin. The vesicles exchange outer-leaflet (exterior) lipids on the order of seconds and fully exchange both interior and exterior lipids within hours. Measuring lipid exchange kinetics requires in situ mixing to capture the faster (seconds) and slower (minutes) processes and extract the kinetic rate constants. The same sample environment can also be used to probe molecular exchange in other types of liquid samples such as lipid nanoparticles, proteins, surfactants, polymers, emulsions, or inorganic nanoparticles. Measuring the nanoscale structural transformations and kinetics of exchanging or reacting systems will provide new insights into processes that evolve at the nanoscale.

This protocol presents the use of a stopped-flow sample environment to quickly mix multiple liquid solutions in situ during a small-angle neutron scattering measurement and to study kinetic processes on nanometer length scales and second time scales.

利用停流和小角中子散射测量纳米材料的时间演化

This paper presents the use of a stopped-flow small-angle neutron-scattering (SANS) sample environment to quickly mix liquid samples and study nanoscale ...

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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