我们承认特拉华大学硕士机械师铝长矛，用于加工剪切单元和塞德里克·加格农先生的设计和绘图。这手稿是根据从NIST，美国商务部合作协议70NANB7H6178准备。这项工作动用了美国国家科学基金会根据协议号DMR-0944772支持部分设施。该语句，结果，结论和建议仅代表作者（S），并不一定反映NIST或美国商业部的观点。

图2示出了附连到基板，其被安装到样品上的环境阶段的试验板，并在中子束的SANS实验对准的组装剪切细胞。步进马达，齿轮箱和皮带传动，狭缝马达阶段，剪切细胞和中子束的方向被标在图2中。本协议提供的方向组装的剪切单元（第1节），剪切单元安装到样品环境阶段（第2节），校准几何形状设计，SANS实验（第3节），装样品（第4节），运行实验和数据收集（第5）和结束实验（第6条）。供参考， 图3是组装的电池和图4的示意性示出了从前面板布置到后板的分解剪切细胞部分，左到右，和用于组装所需的工具（以1/16和3/16内六角板手s，并且在开口扳手3/8）。从左至右图4是前板，轴承，弹簧加载的套管，O型圈，石英窗口，中间板与O形环，样品进入口和注射器连接器，止动螺钉，心轴，而对于部分背板（石英窗，O型圈，弹簧式衬套，轴承），背板，四个内六角螺钉和快速连接冷却软管连接快速接头。 1。组装剪切单元格（插图到右中图2） <ol><li>制备中间板进行组装。 <ol><li>清洁中间板包括样品和设定螺杆的途径和由分数标记标识板的顶部。 </li><li>使用三组，螺丝密封装样的途径。包装每个固定螺丝的螺纹密封胶带，并使用六角扳手1/16插入每个螺丝到每个孔在“底部”（2）和一个固定螺丝插入“方”的孔。 </li><lI&gt;将圆形白色O型圈（中号2-14，氟橡胶标AS568尺寸035）在对中板两侧的沟槽。 </li></ol></li><li>备的正面和背面板组装（ 图5）。 <ol><li>压配合在轴承插入每个正面和背面板构成。 </li><li>插入弹簧加载的套管（这是一个密封）与弹簧侧朝向样本开放到前板和后板。 </li><li>放置（在ID 2-1/4）丁腈橡胶平方双重密封件的O形圈的小（在ID 1-5/8）和大到凹槽中的每个正面和背面板构成。 </li><li>放置在石英窗上的正方形O形环在每块板的顶部。 </li></ol></li><li>装配前部和中间板一起。 <ol><li>放置在前板在一个平面上;对齐得分在中间和前板的顶部，并放置在中间板的前板。如果有必要，涂抹少量适当的油脂，以圆形O形圈在T他中间板组装过程中举行的地方。 </li></ol></li><li>组装模芯和背板一起。 <ol><li>将模芯的短端插入背板。使用均匀涂于力和芯棒将“点击”到位。请注意该芯棒现持有的石英窗和方形O型圈的地方在后面板上。 </li></ol></li><li>组装前板，中板，芯棒和背板在一起。 <ol><li>设置一个凸起的平台与中间板朝上放在前面和中间板组件。这就提出了平台，是让芯棒轴空间的组件下方延伸，而无需访问表。 </li><li>前面板上组件的顶部与背面板组件的得分将比分对齐。 </li><li>插入芯棒轴的长的部分到前板组件。确保在中板的圆形O型圈装配过程中保持正确的坐姿。小区瓦特生病滑动起来，并再次，“咔嚓”当正确安装。 </li><li>使用四个内六角螺钉和内六角扳手3/16螺丝组装在一起。拧紧螺钉以交叉图案，使得该细胞保持同心度。 </li></ol></li><li>包裹螺纹密封带绕两个接入端口和拧入中间板的顶部。加强与在开口扳手3/8。 </li><li>将镉掩模（ 图6）插入加工成前板的前部的接纳槽。应用胶带或粘性，如果需要举行面具到位。 </li><li>使用快速连接器上的前板和后板的顶部端口之间交叉连接的冷却剂的软管。 </li></ol> 2。安装剪切单元格进入光束线<ol><li>覆盖SANS检测窗口与安全防护罩。 </li><li>问负责仪器设备的科学家对准样品环境阶段的中子束。 </l我&gt; <li>使用四个¼英寸x 20六角头螺栓艾伦和内六角扳手3/16挂载面包板的样品环境的阶段。 </li><li>附加剪切单元组件与位于底板小区安装支架（已附着在试验板（ 图7））。 <ol><li>识别单元的安装支架和轴联接器安装于基板（ 图8）。确保止动螺钉的杆耦合器被松开。 </li><li>对准杆耦合器和心轴的轴，使得在耦合器中的止动螺钉将螺丝拧入心轴的轴的平坦部分。 </li><li>水平方向的剪切单元滑入电池安装架，以使组装的样子，在图8中所示， 此步骤，应小心进行，因为它不能弯曲的心轴的轴或杆耦合器是重要的。 </li><li>附加剪切电池组件到电池安装架具有两个凹头帽螺丝用3/16内六角扳手。拧紧始终确保剪切单元是针对电池安装支架齐平。 </li><li>加强对在用内六角扳手1/16到剪切单元芯棒轴连接到驱动器组件上的轴连接器两个设定螺钉。 </li></ol></li><li>对准中子束的剪切单元格的几何形状。 <ol><li>使用激光来调整SANS样本环境阶段，使得该心轴的轴的高度是相同的中子束。对齐的在剪切单元到中子束线路径的中心的间隙的中心。 </li></ol></li><li>将适当的镉缝成安装在面包板（ 图8）缝电机组装阶段。如果需要固定狭缝与粘性。 注意：该狭缝应当与前板齐平，并放置约剪切单元的间隙内。选择的缝隙相应于所希望的实验。对于分辩率的差距在实验0.1毫米0.2毫米的弯曲狭缝可用。而对测量不要求空间分辨率0.8毫米的长方形狭缝是可取的。 </li><li>使用曲柄来调整传动皮带的张力，以便有大约¼在偏转在带移动电机的位置。当松紧适度，用在阿伦7/64扳手拧紧固定螺丝位于方向盘下方锁定电机位置。 注意：可选的齿轮减速可被添加​​到所述马达组件。根据所需的特定实验所需的剪切速率，此选项可能是必要的。 </li><li>使用快速接头连接两个冷却液浴软管剪切单元格。 </li><li>调整任何观测相机或特定于观察实验等辅助设备。 </li><li>取下安全罩保护SANS的探测器窗口。 </li></ol> 3。 SANS的设置和校准<ol><li>附上＆0.5＃160，光圈入射中子束对吻的结束。 </li><li>设置所需的SANS检测器位置（Q-范围），中子的波长，波长和传播下列标准SANS的协议和对实验条件进行了优化。 注：计算为样品到检测器的距离是基于样品环境阶段位于“胡伯表”。 </li><li>与剪切单元的间隙对准的狭缝的位置。 <ol><li>使用狭缝马达阶段（ 图8），以使该狭缝的位置与剪切单元的间隙。使用激光来模拟中子束和反射镜，以检测激光一旦其穿过剪切单元组件的所述间隙内的石英窗。 </li><li>微调用SANS传输测量的狭缝的位置。系统地改变从剪切单元间隙的内壁狭缝电机位置来使用0.1毫米马达狭缝翻译步骤的剪切单元间隙的外壁上。使用SANS观察传输（通常为2秒），并记录该狭缝马达位置对每个发送测量（ 图9）。 注：如果空间分辨率的需要，确定所需的SANS的实验电机的位置。如果空间分辨率是没有必要的识别对准的剪切单元间隙的中间狭缝的单电机位置。对准在剪切细胞间隙的缝隙是完成一个很好的尝试是至关重要的。也有可能（和建议）使用水来对齐用SANS传输测量的狭缝的位置。使用水降低了传输，并提供与剪切电池外壳（ 图9）的对比。 注：按照样品装载协议（第4节）装入水进入细胞内。使用水一般需要剪切细胞被从底板取出，分解，干燥，重新组合和重新安装到基板上装载SA前投影机的简易实验。只要在底板上不从样品环境阶段除去这应该不是一个问题，但它始终是重要的，以验证该狭缝对准的配合间隙。 </li></ol></li><li>校准样品的几何形状<ol><li>根据SANS的标准化程序进行阻断光束暗计数和一个空单元格的测量。请注意，空单元格测量应在每个空间位置由3.3节进行的狭缝校准确定执行。 </li></ol></li></ol> 4。样品装载协议<ol><li>把安全防护罩SANS的探测器窗口上。 </li><li>安装两个注射器接头（尼龙）和带螺纹的注射器装置（蓝色和黄色）的钢管在样品池的顶部。确保旋塞处于关闭位置。 </li><li>样品预加载到10ml注射器螺纹（最小样品体积为6毫升）中。确保样品是免费的气泡。 <ol><li>通过离心分离或轻度或加热样品以降低样品的粘度，同时装载注射器消除气泡。如果样品被加热时，它是强烈建议的剪切单元的温度也增加了在将样品加载到帮助。 </li></ol></li><li>将空注射器没有在柱塞的连接器上的剪切单元的中间接收过量的样品（ 图8）。 </li><li>放置在另一个连接器上的样品注射器（ 图8）。 </li><li>打开两个旋塞。 </li><li>注入样品慢慢直到样品开始进入到空的注射器。 </li><li>从剪切单元的间隙去除任何气泡。 <ol><li>转动电机控制关闭，以释放电机，并允许带手动移动。 </li><li>剪切样品用手工来帮助移动的气泡，剪切单元的顶部，由此额外的样品注入通常会推动气泡进入出口和流出的剪切单元间隙。 </li></ol></li><li>关闭旋塞锁定在样品中的细胞。 </li><li>改变水浴中，以所要求的试验温度下的温度，和前提进行样本剪切历程为合适。 </li><li>检查是否有气泡（和实验过程中经常这样做）。如果气泡观察;打开旋塞，用旋转气泡移动到剪切带的顶部，并注入更多的样品，推动了泡沫细胞的剪切带。 </li><li>从梁区域中删除安全盾和任何多余的工具和用品。 </li></ol> 5。运行剪切实验和收集数据SANS <ol><li>对于简单的稳态剪切实验： <ol><li>与电机控制软件（参见电机控制软件操作相关的文档）相关联的稳态剪切控制文​​件中设置的剪切速率。 </li><li>确定剪切方向在实验过程中的样品。 </li><li>根据SANS的标准化程序设置所需的SANS实验。 </li><li>开始剪切电池电动机。 </li><li>启动SANS实验。检查探测器计数，观察SANS的2D模式，以确保SANS结果剪切过程中被正确记录。观察到的在对有代表性的结果的部分中讨论的表面活性剂溶液的典型模式的一个例子示于图10。 </li><li>为每个所需的剪切速率重复该过程（第5.1节）。 </li></ol></li><li>时间分辨振荡剪切实验： <ol><li>验证了振荡剪切实验的触发位置。对于振荡剪切，这是在最大应变和最小（零）的应变速率的点。 </li><li>设置振荡频率和振幅与电机控制软件相关的时间分辨控制文件中（参见电机控器相关文档l通过软件操作）。请注意，应变振幅是根据所施加的应变集中于零的幅度定义，并且是流变学上定义的应变幅度。 </li><li>开始的振荡剪切试验的剪切电池电动机。 </li><li>启动SANS实验。检查检测器计数，观察2D模式，以确保SANS是否正确被在振荡剪切记录。 </li><li>时间戳记的中子探测器的日志文件复制从NISTO到夏洛特和预处理使用由NCNR提供的软件的数据。 </li><li>降低预处理数据集与还原软件包IGOR。 </li><li>对于每个，所需的振荡频率和应变振幅条件重复上述步骤（第5.2节）。 </li></ol></li></ol> 6。实验结束<ol><li>关闭中子束和电机控制。 </li><li>将安全防护罩SANS的检测窗口。 </li><li>让样品和装置标D在闭合光束5分钟。从底板卸下剪切单元格之前执行的标准辐射检查。 </li><li>打开旋塞的样品端口和撤回或使用样品注射器推出样品。收回样品，关闭旋塞，并取下注射器。 </li><li>关闭温浴。从脱开的剪切细胞快速连接端口流体浴冷却软管。 </li><li>松开用1/16的内六角扳手芯轴和驱动轴之间的联轴器的内六角螺钉。使用3/16内六角扳手拧开，剪切单元连接到电池安装支架上的两个内六角螺钉。滑动剪切细胞到细胞的安装支架。 </li><li>通过反转装配协议（该协议第1条）拆卸剪切单元格。 </li><li>用肥皂水清洗剪切单元格。彻底清洗和干燥。 </li></ol>

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J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Relating+shear+banding,+structure,+and+phase+behavior+in+wormlike+micellar+solutions.">Relating shear banding, structure, and phase behavior in wormlike micellar solutions.</a> Soft Matter. 5, 3858-3869 (2009).</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, 727-756 (2009).</li><li>Liberatore, M. 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=Microstructure+and+shear+rheology+of+entangled+wormlike+micelles+in+solution.">Microstructure and shear rheology of entangled wormlike micelles in solution.</a> J. Rheol. 53, 441-458 (2009).</li><li>Maranzano, B. 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=Flow-small+angle+neutron+scattering+measurements+of+colloidal+dispersion+microstructure+evolution+through+the+shear+thickening+transition.">Flow-small angle neutron scattering measurements of colloidal dispersion microstructure evolution through the shear thickening transition.</a> J. Chem. Phys. 117, 10291-10302 (2002).</li><li>Wagner, N. J., Ackerson, B. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Analysis+of+nonequilibrium+structures+of+shearing+colloidal+suspensions.">Analysis of nonequilibrium structures of shearing colloidal suspensions.</a> J. Chem. Phys. 97, 1473-1483 (1992).</li><li>Zhou, L., Vasquez, P. A., Cook, L. P., McKinley, G. H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Modeling+the+inhomogeneous+response+and+formation+of+shear+bands+in+steady+and+transient+flows+of+entangled+liquids.">Modeling the inhomogeneous response and formation of shear bands in steady and transient flows of entangled liquids.</a> J. Rheol. 52, 591-623 (2008).</li><li>Spenley, N. A., Cates, M. E., McLeish, T. C. B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nonlinear+rheology+of+wormlike+micelles+Phys.">Nonlinear rheology of wormlike micelles Phys.</a> Rev. Lett. 71, 939-942 (1993).</li><li>Lopez-Barron, C., Gurnon, A. K., Porcar, L., 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=Structural+Evolution+of+a+Model,+Shear-Bading+Wormlike+Micellar+Soution+during+Shear+Start+Up+and+Cessation.">Structural Evolution of a Model, Shear-Bading Wormlike Micellar Soution during Shear Start Up and Cessation.</a> Phys. Rev. Lett.. , (2013).</li></ol>

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能够测量通过小角中子散射剪切复杂流体的剪切速度，速度梯度面的显微组织的新仪器开发和验证。剪切单元设计使用的补充辐射源其他工具，如X射线和光散射，以及能够在剪切（速度-涡量和速度梯度涡度）的两个面表征微观流变SANS工具8 ，10。这个仪器的功能为稳态剪 ​​切和时间依赖性流动，如振动或启动剪切流，后者使用一种频闪方法和时间分辨中子散射技术11，12，21。?...

发展中的必然现象一个科学的认识，需要准确和精确的测量。计量也是成功的工程新工艺和材料和设计的基础。 流变学是物质的变形和流动的科学。流变学是中央在我们处理各种材料的能力，同时可用于由产品配方，针对特定的材料特性。前者的典型实例包括模制的聚合物或复合材料形成，而后者包括日常消费品如油漆，洗发水和食品的开发。熔融聚合物的粘度是否被控制，使得它可以有效地注射模制或洗发剂的粘弹性的改变，从而它具有为消费者正确的一致性，流变学特性是通过改变材料1的配方来控制。材料和产品的流变性也取决于T他结构在流体状态和该结构的范围从微观到纳米级。此外，这种结构的加工参数，如流量的流量和时间，挑战的流变流中进行测量的结构而变化。它是满足的，部分由本文中所描述的新型仪器仪表这一挑战。 能够探测下剪切流动的软质材料的微观结构新颖的技术可以造福软质材料的产品设计和工艺条件优化。对于软质材料在各种行业和基础科学的应用程序的许多有趣的和长期存在的挑战涉及不寻常的流动行为，如胶体悬浮液剪切增稠2，剪切和蠕虫状胶束的3涡带，以及固有的非均质性流胶凝胶4-6。是的流变不断挑战阐明microstru在流变学反应，有时甚至在剪切粘弹性材料的速度场的非线性ctural起源。这一挑战，需要同时采集的显微组织为两个空间位置中的流场和时间依赖行为，这已经被证明是一个艰巨的任务，对实验者的函数。 小角中子散射（SANS），特别适合用于测量复杂流体的结构，因为它可以探测的材料是不透光的。还选择性氘可以被用来提供可以出现在X射线散射7类似的组件之间的对比。此外，中子具有过X射线的优势，因为有生物或其他软质样品的无辐射的伤害。在这里所示的实验中，由一个反应器或一个散裂源产生冷中子被准直和一个样本时亮起。散射强度毅关于该材料的长度上的视场结构信息从原子尺度到几百纳米（和超小角度中子散射到几十微米），但在一个傅立叶变换的形式实空间结构的变换。因此，数据的解释可以是具有挑战性的，并涉及逆变换或比较微观模型或模拟。更多关于SANS仪器仪表，实验，对比匹配可对发布在中心的中子科学，www.cns.che.udel.edu的网站上找到的教程。 在这里，我们描述了一个剪切单元旨在扩展SANS的方法来检查材料在流动。一般的方法和仪器，以及最近应用的主要文献回顾最近的概述可以在参考图8和其中所引用的参考文献中找到。一个既方便又近乎理想的环境下与剪切流探测流体结构SANS是一个狭长的间隙库埃特的几何形状，也被称为同心圆筒9。这种几何形状适用于一个简单的（ 即层）的剪切流动的样品，同时保持足够通畅的体积为入射中子束。流的应用打破了微结构的对称性，正如在简单剪切流动的材料的显微结构的这样一个完整的表征要求在剪切的所有三个平面显微测量。两个平面的剪切可以使用标准库爱特几何结构（ 图1a）进行调查：中子束被配置为沿速度梯度方向行进并探测速度涡度（1-3）的剪切平面（“径向”配置） ，或者，该光束通过一个狭长切口并平行于流动方向的准直，从而探测的速度梯度涡度（2-3）面（“切向”配置）。本仪器可Çommercially和最近已记录用于检查下剪切10复杂流体。上述综述了其使用的相关设备和跨范围广泛的材料和应用8结构-性质的决心。时间分辨的实验中，如用于振荡剪切流动也有报道11，12。 常流的最有趣和最重要的飞机是速度，速度梯度（1-2）平面（ 图1b），但它也是最难以调查，因为它需要特殊的仪器。自定义剪切单元格的设计，使速度，速度梯度（1-2）平面由SANS使得中子束传播平行于剪切13-16的涡轴的直接调查。在流动的1-2平面测量是获得一个定量的了解的剪切粘度至关重要的，因为他们elucid吃相结构的取向与流动方向15，17，18。这对于材料如聚合物，自组装的表面活性剂，胶体，以及其他复杂流体重要。另外，也可以调查材料的显微组织为在剪切流的梯度方向跨越间隙位置的函数。与另外的空间分辨率，该方法提供了一种装置，用于学习表现出沿剪切的梯度方向微观结构的变化的材料。一个例子为其中调查改变微观结构和组成沿流的梯度方向是剪切条带。剪切带是由微观结构和流动方向，结果在非均匀流场13之间的耦合现象。在这篇文章中，我们描述了仪器，它的组件和流程，SANS的测量技术于NIST的中心氖实施UTRON研究（NCNR）在美国国家标准与技术研究院（NIST）在马里兰州盖瑟斯堡。此示例环境是特拉华大学，NIST和研究所劳厄 - 朗之万（ILL）之间的合作的结果，并已在两个馆际互借和NIST得到顺利实施。出于本文的目的，这里的协议SANS的特定部分所关注的，该技术被描述为在NIST实施。然而，修改这些工具的具体细节应该是简单的，整体的技术可以在任何SANS的仪器来实现稳流（5.1节）。此外，配备了时间分辨SANS的功能工具也可能进行振荡剪切流SANS实验（5.2节）。剪切电池组件的技术图纸是作为图12-23。

<table border="0" cellpadding="0" cellspacing="0" width="785">
	<tbody>
		<tr>
			<td>Deuterated Water (99.9%)</td>
			<td>Cambridge Isotopes</td>
			<td>7789-20-0</td>
			<td>83.3 wt % in formulation 
			D2O</td>
		</tr>
		<tr>
			<td>CTAB- Cetyl Trimethyl Ammonium Bromide&#160;</td>
			<td>Sigma-Aldrich</td>
			<td>57-09-0&#160;</td>
			<td>16.7 wt % in formulation 
			CH3(CH2)15N(Br)(CH3)3</td>
		</tr>
		<tr>
			<td>1/16&#34; Allen wrench</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>3/16&#34; Allen wrench</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>3/8&#34; open end wrench</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>tape</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>thread seal tape</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td style="font-size: 13px; line-height: 1.6em;">syringes (2)</td>
			<td style="font-size: 13px; line-height: 1.6em;"></td>
			<td style="font-size: 13px; line-height: 1.6em;"></td>
		</tr>
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measuring material microstructure under flow using 1-2 plane flow-small angle neutron scattering

为研究在简单剪切流复杂流体的微观结构优化的一个新的小角度中子散射（SANS）样品环境呈现。 SANS的剪切单元由被密封并绕一水平轴以使流场的涡度方向与中子束能够从1-2平面的剪切（速度，速度梯度散射对准的同心圆筒库埃特几何形状，分别）。这种做法是一个进步比以前的剪切细胞样品环境，因为有大量的流变性和微观结构特征之间的强耦合剪切的1-2平面。流动的不稳定性，如剪切带，也可以通过空间分辨测量来研究。这是通过使用一个窄孔，用于中子束和扫描沿速度梯度方向来实现在此示例环境。时间分辨实验，如流的初创企业和大振幅振荡她芳流也是可能的剪切运动和时间分辨检测散射中子的同步。使用此处所述的方法的代表性结果证明空间分辨率的测量的蠕虫状胶束溶液表现出剪切带，这种现象只能通过解析沿速度梯度方向上的结构进行研究的微观结构的有用性质。最后，目前的设计潜力的改进与建议补充实验，动机，未来在范围广泛的复杂流体中的各种剪切运动的实验探讨。

一个成功的流SANS实验的代表性结果示于图9，10，和11。这些例子是从制造上的蠕虫状胶束水溶液（WLM）（ 表1）已知在剪切的某些条件表现出剪切带调查。科学发现的一个完整的讨论可以参考15-17被发现。 图10表示使用剪切单元格下剪切流得到散射图案的效果。研究的样本是一种粘弹性蠕虫状胶束（WLM）解决方案包括...

Watch this Scientific Journal Video about Measuring Material Microstructure Under Flow Using 1-2 Plane Flow-Small Angle Neutron Scattering at JoVE.com

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

的剪切单元中的剪切速度，速度梯度平面开发用于小角中子散射测量，并用于表征复杂的流体。在速度梯度方向的空间分辨测量是可能用于研究剪切带的材料。应用包括胶态分散体的调查后，聚合物溶液，和自组装结构。

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 ...

measuring-material-microstructure-under-flow-using-1-2-plane-flow

Research

JoVE Journal

Engineering

14.2K 次观看.  University of Delaware. 的剪切单元中的剪切速度，速度梯度平面开发用于小角中子散射测量，并用于表征复杂的流体。在速度梯度方向的空间分辨测量是可能用于研究剪切带的材料。应用包括胶态分散体的调查后，聚合物溶液，和自组装结构。 

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

Measuring Spatially- and Directionally-varying Light Scattering from Biological Material

Light interacts with an organism's integument on a variety of spatial scales. For example in an iridescent bird: nano-scale structures produce color; the milli-scale structure of barbs and barbules largely determines the directional pattern of reflected light; and through the macro-scale spatial structure of overlapping, curved feathers, these directional effects create the visual texture. Milli-scale and macro-scale effects determine where on the organism's body, and from what viewpoints and under what illumination, the iridescent colors are seen. Thus, the highly directional flash of brilliant color from the iridescent throat of a hummingbird is inadequately explained by its nano-scale structure alone and questions remain. From a given observation point, which milli-scale elements of the feather are oriented to reflect strongly? Do some species produce broader "windows" for observation of iridescence than others? These and similar questions may be asked about any organisms that have evolved a particular surface appearance for signaling, camouflage, or other reasons.
In order to study the directional patterns of light scattering from feathers, and their relationship to the bird's milli-scale morphology, we developed a protocol for measuring light scattered from biological materials using many high-resolution photographs taken with varying illumination and viewing directions. Since we measure scattered light as a function of direction, we can observe the characteristic features in the directional distribution of light scattered from that particular feather, and because barbs and barbules are resolved in our images, we can clearly attribute the directional features to these different milli-scale structures. Keeping the specimen intact preserves the gross-scale scattering behavior seen in nature. The method described here presents a generalized protocol for analyzing spatially- and directionally-varying light scattering from complex biological materials at multiple structural scales.

We present a non-destructive method for sampling spatial variation in the direction of light scattered from structurally complex materials. By keeping the material intact, we preserve gross-scale scattering behavior, while concurrently capturing fine-scale directional contributions with high-resolution imaging. Results are visualized in software at biologically-relevant positions and scales.

从生物材料空间定向变化的光散射测量

Light interacts with an organism's integument on a variety of spatial scales. For example in an iridescent bird: nano-scale structures produce color; the ...

科研

工程学

Atom Probe Tomography Studies on the Cu(In,Ga)Se2 Grain Boundaries

Compared with the existent techniques, atom probe tomography is a unique technique able to chemically characterize the internal interfaces at the nanoscale and in three dimensions. Indeed, APT possesses high sensitivity (in the order of ppm) and high spatial resolution (sub nm).
Considerable efforts were done here to prepare an APT tip which contains the desired grain boundary with a known structure. Indeed, site-specific sample preparation using combined focused-ion-beam, electron backscatter diffraction, and transmission electron microscopy is presented in this work. This method allows selected grain boundaries with a known structure and location in Cu(In,Ga)Se2 thin-films to be studied by atom probe tomography.
Finally, we discuss the advantages and drawbacks of using the atom probe tomography technique to study the grain boundaries in Cu(In,Ga)Se2 thin-film solar cells.

Atom Probe Tomography Studies on the CuIn,GaSe2 Grain Boundaries

In this work, we describe the use of the atom-probe tomography technique for studying the grain boundaries of the absorber layer in a CIGS solar cell. A novel approach to prepare the atom probe tips containing the desired grain boundary with a known structure is also presented here.

原子探针层析成像研究在Cu（铟，镓）硒<sub&gt; 2</sub&gt;晶界

Compared with the existent techniques, atom probe tomography is a unique technique able to chemically characterize the internal interfaces at the ...

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

The spin echo resolved grazing incidence scattering (SERGIS) technique has been used to probe the length-scales associated with irregularly shaped crystallites. Neutrons are passed through two well defined regions of magnetic field; one before and one after the sample. The two magnetic field regions have opposite polarity and are tuned such that neutrons travelling through both regions, without being perturbed, will undergo the same number of precessions in opposing directions. In this case the neutron precession in the second arm is said to &#34;echo&#34; the first, and the original polarization of the beam is preserved. If the neutron interacts with a sample and scatters elastically the path through the second arm is not the same as the first and the original polarization is not recovered. Depolarization of the neutron beam is a highly sensitive probe at very small angles (&#60;50&#160;&#956;rad) but still allows a high intensity, divergent beam to be used. The decrease in polarization of the beam reflected from the sample as compared to that from the reference sample can be directly related to structure within the sample.
In comparison to scattering observed in neutron reflection measurements the SERGIS signals are often weak and are unlikely to be observed if the in-plane structures within the sample under investigation are dilute, disordered, small in size and polydisperse or the neutron scattering contrast is low. Therefore, good results will most likely be obtained using the SERGIS technique if the sample being measured consist of thin films on a flat substrate and contain scattering features that contains a high density of moderately sized features (30 nm to 5 &#181;m) which scatter neutrons strongly or the features are arranged on a lattice. An advantage of the SERGIS technique is that it can probe structures in the plane of the sample.

Progress has been made in utilizing spin echo resolved grazing incidence scattering (SERGIS) as a neutron scattering technique to probe the length-scales in irregular samples. Crystallites of [6,6]-phenyl-C61-butyric acid methyl ester have been probed using the SERGIS technique and the results confirmed by optical and atomic force microscopy.

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 ...

In Situ Neutron Powder Diffraction Using Custom-made Lithium-ion Batteries

Li-ion batteries are widely used in portable electronic devices and are considered as promising candidates for higher-energy applications such as electric vehicles.1,2 However, many challenges, such as energy density and battery lifetimes, need to be overcome before this particular battery technology can be widely implemented in such applications.3 This research is challenging, and we outline a method to address these challenges using in situ NPD to probe the crystal structure of electrodes undergoing electrochemical cycling (charge/discharge) in a battery. NPD data help determine the underlying structural mechanism responsible for a range of electrode properties, and this information can direct the development of better electrodes and batteries.
We briefly review six types of battery designs custom-made for NPD experiments and detail the method to construct the &#8216;roll-over&#8217; cell that we have successfully used on the high-intensity NPD instrument, WOMBAT, at the Australian Nuclear Science and Technology Organisation (ANSTO). The design considerations and materials used for cell construction are discussed in conjunction with aspects of the actual in situ NPD experiment and initial directions are presented on how to analyze such complex in situ data.

In Situ Neutron Powder Diffraction Using Custom-made Lithium-ion Batteries

We describe the design and construction of an electrochemical cell for the examination of electrode materials using in situ neutron powder diffraction (NPD). We briefly comment on alternate in situ NPD cell designs and discuss methods for the analysis of the corresponding in situ NPD data produced using this cell.

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 ...

Characterization of Full Set Material Constants and Their Temperature Dependence for Piezoelectric Materials Using Resonant Ultrasound Spectroscopy

During the operation of high power electromechanical devices, a temperature rise is unavoidable due to mechanical and electrical losses, causing the degradation of device performance. In order to evaluate such degradations using computer simulations, full matrix material properties at elevated temperatures are needed as inputs. It is extremely difficult to measure such data for ferroelectric materials due to their strong anisotropic nature and property variation among samples of different geometries. Because the degree of depolarization is boundary condition dependent, data obtained by the IEEE (Institute of Electrical and Electronics Engineers) impedance resonance technique, which requires several samples with drastically different geometries, usually lack self-consistency. The resonant ultrasound spectroscopy (RUS) technique allows the full set material constants to be measured using only one sample, which can eliminate errors caused by sample to sample variation. A detailed RUS procedure is demonstrated here using a lead zirconate titanate (PZT-4) piezoceramic sample. In the example, the complete set of material constants was measured from room temperature to 120 &#176;C. Measured free dielectric constants <img alt="Equation 1" src="/files/ftp_upload/53461/image001.jpg" /> and&#160;<img alt="Equation 2" src="/files/ftp_upload/53461/image002.jpg" /> were compared with calculated ones based on the measured full set data, and piezoelectric constants d15 and d33 were also calculated using different formulas. Excellent agreement was found in the entire range of temperatures, which confirmed the self-consistency of the data set obtained by the RUS.

This protocol describes the procedure of measuring the temperature dependence of the full set material constants of piezoelectric materials using resonant ultrasound spectroscopy (RUS).

全套材料常数表征及其温度依赖性的压电材料使用共振超声波谱

During the operation of high power electromechanical devices, a temperature rise is unavoidable due to mechanical and electrical losses, causing the ...

Experimental Methods for Investigation of Shape Memory Based Elastocaloric Cooling Processes and Model Validation

Shape Memory Alloys (SMA) using elastocaloric cooling processes have the potential to be an environmentally friendly alternative to the conventional vapor compression based cooling process. Nickel-Titanium (Ni-Ti) based alloy systems, especially, show large elastocaloric effects. Furthermore, exhibit large latent heats which is a necessary material property for the development of an efficient solid-state based cooling process. A scientific test rig has been designed to investigate these processes and the elastocaloric effects in SMAs. The realized test rig enables independent control of an SMA&#39;s mechanical loading and unloading cycles, as well as conductive heat transfer between SMA cooling elements and a heat source/sink. The test rig is equipped with a comprehensive monitoring system capable of synchronized measurements of mechanical and thermal parameters. In addition to determining the process-dependent mechanical work, the system also enables measurement of thermal caloric aspects of the elastocaloric cooling effect through use of a high-performance infrared camera. This combination is of particular interest, because it allows illustrations of localization and rate effects &#8212; both important for efficient heat transfer from the medium to be cooled.
The work presented describes an experimental method to identify elastocaloric material properties in different materials and sample geometries. Furthermore, the test rig is used to investigate different cooling process variations. The introduced analysis methods enable a differentiated consideration of material, process and related boundary condition influences on the process efficiency. The comparison of the experimental data with the simulation results (of a thermomechanically coupled finite element model) allows for better understanding of the underlying physics of the elastocaloric effect. In addition, the experimental results, as well as the findings based on the simulation results, are used to improve the material properties.

Experimental methods for investigation of solid state cooling processes and characterization of elastocaloric material properties of Shape Memory Alloys (SMA) are presented. A custom-built test rig has been designed for controlling and comprehensive monitoring of elastocaloric cooling processes. Furthermore, it provides a validation platform for thermomechanically coupled modeling approaches.

基于形状记忆调查Elastocaloric冷却过程和模型验证实验方法

Shape Memory Alloys (SMA) using elastocaloric cooling processes have the potential to be an environmentally friendly alternative to the conventional vapor ...

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

A procedure for the operation of a new dielectric RheoSANS instrument capable of simultaneous interrogation of the electrical, mechanical and microstructural properties of complex fluids is presented. The instrument consists of a Couette geometry contained within a modified forced convection oven mounted on a commercial rheometer. This instrument is available for use on the small angle neutron scattering (SANS) beamlines at the National Institute of Standards and Technology (NIST) Center for Neutron Research (NCNR). The Couette geometry is machined to be transparent to neutrons and provides for measurement of the electrical properties and microstructural properties of a sample confined between titanium cylinders while the sample undergoes arbitrary deformation. Synchronization of these measurements is enabled through the use of a customizable program that monitors and controls the execution of predetermined experimental protocols. Described here is a protocol to perform a flow sweep experiment where the shear rate is logarithmically stepped from a maximum value to a minimum value holding at each step for a specified period of time while frequency dependent dielectric measurements are made. Representative results are shown from a sample consisting of a gel composed of carbon black aggregates dispersed in propylene carbonate. As the gel undergoes steady shear, the carbon black network is mechanically deformed, which causes an initial decrease in conductivity associated with the breaking of bonds comprising the carbon black network. However, at higher shear rates, the conductivity recovers associated with the onset of shear thickening. Overall, these results demonstrate the utility of the simultaneous measurement of the rheo-electro-microstructural properties of these suspensions using the dielectric RheoSANS geometry.

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

Here, we present a procedure for the measurement of simultaneous impedance, rheology and neutron scattering from soft matter materials under shear flow.

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 ...

Scanning Light Scattering Profiler (SLPS) Based Methodology to Quantitatively Evaluate Forward and Backward Light Scattering from Intraocular Lenses

The scanning light scattering profiler (SLSP) methodology has been developed for the full-angle quantitative evaluation of forward and backward light scattering from intraocular lenses (IOLs) using goniophotometer principles. This protocol describes the SLSP platform and how it employs a 360&#176; rotational photodetector sensor that is scanned around an IOL sample while recording the intensity and location of scattered light as it passes through the IOL medium. The SLSP platform can be used to predict, non-clinically, the propensity for current and novel IOL designs and materials to induce light scatter. Non-clinical evaluation of light scattering properties of IOLs can significantly reduce the number of patient complaints related to unwanted glare, glistening, optical defects, poor image quality, and other phenomena associated with the unintended light scattering. Future studies should be conducted to correlate SLSP data with clinical results to help identify which measured light scatter is most problematic for patients that have undergone cataract surgery subsequent to IOL implantation.

Scanning Light Scattering Profiler SLPS Based Methodology to Quantitatively Evaluate Forward and Backward Light Scattering from Intraocular Lenses

This protocol describes the scanning light scattering profiler (SLSP) that enables the full-angle quantitative evaluation of forward and backward scattering of light from intraocular lenses (IOLs) using goniophotometer principles.

基于扫描光散射分析器（SLPS）的方法来量化评估来自眼内镜的前向和后向光散射

The scanning light scattering profiler (SLSP) methodology has been developed for the full-angle quantitative evaluation of forward and backward light ...

High-speed Continuous-wave Stimulated Brillouin Scattering Spectrometer for Material Analysis

Recent years have witnessed a significant increase in the use of spontaneous Brillouin spectrometers for non-contact analysis of soft matter, such as aqueous solutions and biomaterials, with fast acquisition times. Here, we discuss the assembly and operation of a Brillouin spectrometer that uses stimulated Brillouin scattering (SBS) to measure stimulated Brillouin gain (SBG) spectra of water and lipid emulsion-based tissue-like samples in transmission mode with &lt;10 MHz spectral-resolution and &lt;35 MHz Brillouin-shift measurement precision at &lt;100 ms. The spectrometer consists of two nearly counter-propagating continuous-wave (CW) narrow-linewidth lasers at 780 nm whose frequency detuning is scanned through the material Brillouin shift. By using an ultra-narrowband hot rubidium-85 vapor notch filter and a phase-sensitive detector, the signal-to-noise-ratio of the SBG signal is significantly enhanced compared to that obtained with existing CW-SBS spectrometers. This improvement enables measurement of SBG spectra with up to 100-fold faster acquisition times, thereby facilitating high spectral-resolution and high-precision Brillouin analysis of soft materials at high speed.

We describe the construction of a rapid continuous-wave-stimulated-Brillouin-scattering (CW-SBS) spectrometer. The spectrometer employs single-frequency diode-lasers and an atomic vapor notch-filter to acquire transmission spectra of turbid/non-turbid samples with high spectral-resolution at speeds up to 100-fold faster than those of existing CW-SBS spectrometers. This improvement enables high-speed Brillouin material analysis.

用于材料分析的高速连续波受激布里渊散射光谱仪

Recent years have witnessed a significant increase in the use of spontaneous Brillouin spectrometers for non-contact analysis of soft matter, such as ...

Measurement of Dynamic Force Acted on Water Strider Leg Jumping Upward by the PVDF Film Sensor

This study aimed to make an explanation for the phenomenon in nature that water strider usually jumps or glides on the water surface easily but quickly, with its peak locomotion speed reaching 150 cm/s. First of all, we observed the microstructure and hierarchy of water strider legs using the scanning electron microscope. On the basis of the observed morphology of the legs, a theoretical model of the detachment from water surface was established, which explained water striders' capability to slide on water surface effortlessly in terms of energy reduction. Secondly, a dynamic force measurement system was devised using the PVDF film sensor with excellent sensitivity, which could detect the whole interaction process. Subsequently, a single leg in contact with water was pulled upward at different speeds, and the adhesion force was measured at the same time. The results of the departing experiment suggested a deep understanding of the fast jumping of water striders.

The protocol here is dedicated to investigating the free and quick maneuvering of water strider on water surface. The protocol includes observing the microstructure of legs and measuring the adhesion force when departing from water surface at different speeds.

PVDF 薄膜传感器对水黾腿跳起动力的测量

This study aimed to make an explanation for the phenomenon in nature that water strider usually jumps or glides on the water surface easily but quickly, ...