Name: dynamic pore-scale reservoir-condition imaging of reaction in carbonates using synchrotron fast tomography
Uploaded: 2017-02-21T12:30:00.000+00:00
Duration: 10 min 18 s
Description: Watch this Scientific Journal Video about Dynamic Pore-scale Reservoir-condition Imaging of Reaction in Carbonates Using Synchrotron Fast Tomography at JoVE.com

We gratefully acknowledge funding from the Qatar Carbonates and Carbon Storage Research Centre (QCCSRC), provided jointly by Qatar Petroleum, Shell, and Qatar Science &amp; Technology Park. We also gratefully acknowledge the funding and support provided by Diamond Lightsource and Manchester University at the I13 Imaging Branch.

1.成像策略设计<ol><li>计算在最高粉束能量和磁通束线的X射线谱，以便利用实验调谐曲线和测量滤波器的传输进行预测的成像性能。钻石Lightsource I13-2&#39;粉红梁"的X射线谱的一个例子示于图2。 </li><li>作为低能量的X射线引起的样品的加热和不添加到成像对比，滤出的X射线频谱的较低部分，使得只有最高能量的X射线在成像样品使用。选择的那个通过计算在现有的光波长31,32理论滤波器透射吸收在适合于光源的光的所希望的低波长的材料线滤波器。这里，可以使用铝和金在该光源的光束线。 <ol><li>使用由combina的带通滤波器的X射线滤波器的高通和一个X射线反射镜接近临界角的低通滤波操作和灰。在这种情况下，使用一组为0.2mm热解碳0.2毫米铝过滤器和用于反射镜的铂涂覆的带材1.15毫弧度的入射角下。反射镜反射低于30千电子伏特和附加在线过滤器被安装为2mm的Al和0.1微米的Au其中在13和22千电子伏有吸收峰，分别筛选更多的低能量X射线的唯一的光。 图3描绘了束线成像装置。 </li></ol></li><li>选择在现有的光的频率和流量的光束线丰富scintillates闪烁体。在这种情况下，闪烁屏幕是由250微米厚的镉tungstenate（CdWO 4），其上叠加了750微米厚的铅tungstenate（钨酸铅4）。然后选择一个客观的镜头和相机的视适当的领域，抢购时间分辨率为experimental要求。在这种情况下，夫妇与0.04与PCO EDGE 5.5 CMOS摄像的孔并用一1.25X物镜捕获的视4毫米场与0.001秒的帧速率。 </li><li>选择图像采集的&#39;flyscan"技术为舞台旋转这种方法减少了样品的震动。传统采集要求阶段停留在每一角增量，取投影，然后移动到下一个角度。在这些动态tomographies图像获取用&#39;flyscan&#39;，它接受作为舞台移动断层扫描，并假定一个角增量，使得每个相继投影之间的差小完成。该&#39;flyscan&#39;方法消除了起动和停止运动的小振动的效果和更快地提供更高质量的图像。 </li></ol> 2.设备和电池的组装<ol><li> 装载在用于岩心驱替制备芯进入细胞。 </st荣&gt; <ol><li>首先，包芯在铝箔的一个层和插入一个套筒（ 例如 ，氟橡胶）（ 图4）。 </li><li>切断套筒尺寸，使得它比纤芯和内部端部装配件的组合长度短2毫米。端部装配件是1/16"国家管螺纹（NPT），对已加工成5mm的外径联合接头，而套筒是4毫米内径。 </li><li>伸过来5 mm页端接头套筒来创建一个密封。确保没有端部配件和芯之间的任何空间，以确保围压不超过压缩套管和夹断流动。 </li><li>包裹在铝两个附加层中的配件和套筒既能防止气态的 CO 2扩散进入限制流体并保持套筒就位在接头和防止液压通路从连接围和孔隙流体。 </li><li>把核心HOL滑动管子和密封件放回原处明镜回到一起并通过更换螺栓密封端盖和端部配件。 </li></ol></li><li>安装在舞台上的芯保持器和连接流和电气线路。 </li><li>测试阶段转动，并确保所有的流量和电气线路可自由旋转为-90°〜90°。 </li><li> 取之前开始实验的整个芯的干扫描。 <ol><li>扫描在大约4毫米的宽度和长度的重叠部分中的核心。校准扫描曝光时间为15000左右的平均计数值，以确保高的信号噪声比，而不过度饱和闪烁器。每次取干扫描至少有2400的预测保持相衬和边缘清晰度。 </li><li>取闪烁器，使得任何损害和外部噪声可以重建过程中占的平面和暗图像。由芯保持器移出的视场取单位并考虑只是闪烁体的图像与在横梁上。采取利用与梁关的相同方法深色衣物。 </li></ol></li></ol> 3.系统加压<ol><li> 通过反应器容器的顶部倾倒流体在加载在1％（重量）氯化钾（KCl）中氯化物的5％（重量）氯化钠（NaCl）食盐水进入拆卸反应器中。 <ol><li>加入粉状碳酸盐岩以实现所需盐水酸度。在这种情况下不加入碳酸酯。 </li><li>通过拧紧螺栓和加热胶带重新打包，并插入温度探头进入前重新组装反应器。 </li><li>负载CO 2的进入喷射泵由（ 图1中V 1）打开阀1。 </li><li>关闭阀1和加压喷射泵100巴。 </li><li>开阀2 CO 2淹没反应堆。加热该反应器50℃，用在组合一个PID控制的加热卷绕温度探头和反对对具有夹带搅拌器由外部电动机驱动tinuously搅拌。平衡用CO 2的盐水在10MPa和50℃2和6小时之间，以确保该盐水是完全用CO 2饱和的和碳酸酯完全溶解。 </li></ol></li><li> 前连接核心保持器，彻底吹扫空气和可能沉淀的系统在先前实验的行。要做到这一点，连接线的上方和芯保持器下面绕过芯保持器（U1和U2）。 <ol><li>负载去离子（DI）水成通过设置在接收泵笔芯通过阀11接收泵。 </li><li>开阀7,4和3，并使用在恒压模式的接收泵向后通过该系统，并从反应器下面阀3的驱动DI水。使用大约十系统卷，以确保线条都清晰的空气，并冲洗干净。 </li></ol></li><li> 清空接收泵次，然后通过阀11和负载DI水进入围泵通过阀10装入25％（重量）的KI盐水到接收泵。 <ol><li>关闭阀10并打开阀8和6，使用限制泵在2MPa限制的核心。 </li><li>关闭阀门11和加压接收泵10栏。 </li><li>打开阀9，7,4，和3，并使用所产生的压力降来驱动KI通过芯掺杂盐水洗涤。 </li><li>逐步加强围和孔隙压力，直到一个合理的流量建立。通过核心驱动盐水的约两个完整系统卷，并通过在反应器下面阀3排出的流体。在这种方式，所有空气被从系统中排出和芯充斥着高对比度盐水洗涤，使未掺杂的反应盐水的到来易于观察。 </li><li>关闭阀3和逐步增加围和孔隙压力，直到芯12兆帕局限和孔隙压力为10MPa。开关PID控制器上以使芯50 C。 </li><li>停止接收泵，关闭阀3，并打开阀5在反应器的底部到反应器系统连接到的核心。 </li></ol></li></ol> 4.流体流动和图像采集<ol><li>中心芯部的中间在视场并为核心充斥跟踪岩心驱替进展连续服用的2-D投影。通过打开粉光束，并使用相机拍摄的图像不旋转阶段采取的2-D投影。反应液注射前开始的2-D的预测给出了前盐水图像清晰，稍后将相对于后续的盐水填充的图像。 </li><li> 设置接收泵以从而通过磁芯在所需流动条件拉动流体从反应器中的期望的流速再填充而离开喷射泵从前端调节压力。 <ol><li>监控的2-D凸起用于衰减该信号功盐水的到来的变化。当反应盐水到达时，芯体的传输将增加，并且随着更多的光照射到闪烁器和掺杂盐水是由高度X-射线透明反应流体位移的二维凸起将大大变亮。如果存在反应性和非反应性盐水之间没有衰减差异然后，取决于束线谱，重新从步骤2.1具有较高盐浓度的KI的实验或使用不同的高度吸收的盐可以是必需的。 </li><li>停止的2-D扫描和3-D取tomographies依次一样快的成像装置允许。使用每次扫描大约1000预测。扫描只使用180°的旋转（相对于传统的360度）的核心。同时使用旋转更少度降低了信噪比，这是更快的，并有助于避免拉伸和缠结的流动和电气线路。以3-D扫描，直到eith器的时间限制达到或芯看起来充分溶解有内部结构倒塌的迫在眉睫的危险（从而导致这两个围压和未来整个芯干扫描数据的损失）。 </li></ol></li><li> 上次扫描拍摄后，有效地将系统减压，以避免任何核心的进一步反应。 <ol><li>首先停止接收泵。然后关闭阀5的反应器连接到系统的其余部分。 </li><li>步骤的系统压力下使用约束和接收泵周围兆帕的压力保持在限制液体。 </li><li>一旦内达到大气压力为1MPa，打开围和接收泵用阀10和11以及在恒流模式运行排出任何剩余流体。 </li><li>关闭PID控制器和在芯保持器以释放任何残留的系统压力的顶部打开工会4路（U2）。 </li><li>慢慢松开围线而醒目过量的二围水用吸水纸。关闭阀6和7和断开工会1和电力线。 </li><li>松开阶段夹，从舞台上拆下核心持有人。 </li></ol></li><li>小心地从芯保持核心组件，然后断开内部端接头套管。不要从袖子去掉内核，因为这样做可能会破坏脆弱的反应的核心。放置在一个完整的去离子水的烧杯中的套筒覆盖的核心，以稀释的任何潜在的反应盐水洗涤，并停止所有反应。 </li><li>干燥在60℃的烘箱整个芯为至少12小时。然后用传统的样品安装重新安装在舞台上的核心，并在相同的分辨率和预测作为初始干扫描扫描一遍。 </li></ol> 5.图像处理<ol><li>通过假设任何影响更正使用多色束关联的任何束硬化的重建图像是放射状符号公制高斯函数33。 </li><li>筛选使用边缘保留滤波器，如非本地化装置以增加信号噪声34，35中的图像（见<a href="https://www-jove-com.bdigitaluss.remotexs.co/files/ftp_upload/53763/5.2_Filtering.png" target="_blank">参考文件</a> ）。 </li><li> 段使用的一个分水岭干扫描图像分割 算法 36 和界定种子岩石和无效的 （见 <a href="https://www-jove-com.bdigitaluss.remotexs.co/files/ftp_upload/53763/5.3_Segmentation.png" target="_blank">补充文件</a> ）。 <ol><li>采取具有反应盐水芯的第一图像和每个后续图像注册到第一图像，并使用与第一图像作为参考兰克泽斯37重采样方法重新取样它。作为正在进行的反应趋于模糊的边缘，对图像分水岭分割不足够精确分割。 </li><li>从第一图像中减去每个反应芯图像得到的差图象。段差图像转换成变化和没有变化。寄存器分割干扫描到第一反应扫描，然后减去从分割干扫描分段变化以实现分段反应图像38。 </li></ol></li></ol> 6.造型<ol><li>使用二值图像作为输入到一个无论是直接的纳维-斯托克斯流求解器39，40，或网络抽取模型41（ 图8）来表征通透性的改变，并提供物理见解溶解的动态。 </li></ol>

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The authors have nothing to disclose.

在储层条件异构孔结构反应的动态影像中最关键的步骤是:1）的粉红色光束内的细胞的精确的温度控制; 2）快速移动阶段成功的核心持有人的稳定性; 3）有效的数据处理和存储技术; 4）时间分辨图像的有效分割。 温度控制是用粉红色光束油藏条件下成像的关键。如果温度上升到高于在反应器温度，CO 2将在孔隙空间exsolve和既改变盐水的pH值，并在可能改变溶出44的性质孔隙空间创建超临界的 CO 2的神经节。使用过滤器来吸收低能量的X射线是用于除去此额外的温度应力允许热电偶和加热缠绕，有效地控制温度在外部的关键。然而，过滤器降低光束的总能量可以通过，因此必须谨慎使用，以便不显著增加总采集时间。此外，滤波器类型和厚度必须进行调整以符合特定能量的波长和吞吐量的束线的。 芯保持器经受断层采集期间旋转和振动应力，可能会导致该碳纤维套筒阶段转动期间摇动和模糊的突起。为了尽量减少这种潜力，芯保持器被设计成一个短6厘米套筒在同步加速器使用。这个套筒不会与台式扫描仪使用有利，因为钢端部装配件将抑制源 - 样品距离和几何放大的最小化。然而，在一个平行光源这些都不顾虑。 在一系列的拍摄各断层扫描可具有尺寸超过20 GB的意思是一个系列100的扫描将在大小2 TB。当在连续服用多种扫描非常归仁ckly两个仪器的带宽和存储选项提供了大量的数据管理挑战。实验成像设备的设计必须考虑到这些约束条件，以充分实现快速断层的动态显像潜力。数据传输瓶颈，必须在开始实验和技术基础设施适应这样如相机问题，读出速度快，传输带宽和存储写入速度不抑制采集速度的潜力之前予以确定。 溶解的时间分辨图像的有效分割提供了一个挑战。当一个断层扫描是在不断变化的系统中的固 - 液边界的边缘可以变得模糊。这使得模糊传统的分割技术，如分水岭，这是假设的界限将是最高的衰减梯度的区域，更成功的作品。为了规避这一点，unreac的差分图像泰德并反应图像被计算，提供变化的唯一的区域的图像。此方法允许连续地改变孔结构的成功分割。 同步加速器加上一个水库规模装置快速层析是一个功能强大的实验方法，该方法可以适用于探索一个范围的应用，包括多相流过程中，对流 - 扩散，并在化学上异构介质传输。然而，目前的装置限制为秒，单相的实验，和小样本大小量级的时间分辨率。未来设计升级可以包括用于三相功能的其他的泵，增加光通量，以便能够穿透较大介质，更好的重建技术，允许更少突起每次扫描进行拍摄，并多元办法图像采集以及可以进一步改善信息分割深度，宽度，和准确性。

碳捕获和储存（CCS）的一个主要关注的是长期贮存的安全1，2。二氧化碳，CO 2注入到地下将在宿主盐水溶解，并形成碳酸3，4，5。该酸性盐水必须与反应并溶解围岩，尤其是当主岩是石灰石6的电位。溶解可以有利，并允许继续地层渗透率7和更大的存储持久8。然而，地质密封完整性可通过该溶解受到损害，并允许CO 2迁移到表面9。存储永久性的准确预测建模因此依赖于盐水岩系统充分理解溶解和分布和流体的运动在地下10，11，12的速度。 然而，性质和溶解在碳酸盐的速率依赖于盐水13，14，15，16和主岩17的两个属性。溶解率也强烈地依赖于盐水的温度和压力6，使实验技术的发展在重要代表性油藏条件下测量复杂的时间依赖的过程。 之前的实验观察到，现场规模的反应率通常要比实验间歇反应器测量18，19低几个数量级。风化，矿物heterogene性，并且在非均相流场不完全混合是这种现象的可能的解释。然而，这是不可能的评估最显著因素而不反应期间不断变化的孔隙空间的直接观察。因此，需要动态孔隙规模的实验，以提供两者见解运输和反应之间的相互影响，并验证的预测模型。 在碳存储应用研究孔隙尺度过程建立的实验方法是X射线微断层（μCT）20，21。 μ-CT有几个好处:它达到下的高空间分辨率到约1微米，其是非侵入性的，并提供了三维图像。石灰石溶解已经研究在芯（〜厘米）比例22和发现岩盐水洗涤反应增加物理异质性。要提前多不同的T的理解ransport和反应条件改变复杂固体和孔结构，有必要测量在孔隙空间几何，拓扑反应引起的变化，并在贮存器的温度和压力在地下岩石系统流，并以更高的分辨率，以详细调查孔隙规模的过程。本文介绍了在复杂的孔隙结构的岩石学活性溶解过程，专注于测量油藏条件下二氧化碳 -acidified盐水和石灰岩之间的时间和空间依赖性反应速率的方法。 已经有多项研究已在复杂碳酸盐23，24，25，26，27看了看反应，但由于实验或成像约束他们已经不是仅限于前，后的反应图像或没有完成在代表性的地下条件。 Menke等 28已经在孔隙尺度历时几个小时，在有代表性的一个含水层在约1公里的深度的温度和压力下进行反应的原位成像动态二氧化碳 -acidified盐水和Ketton石灰石之间。然而，Ketton是大颗粒比较均匀的岩石在很短的时间容易图像（〜17分钟），并与一些预测（〜400）。大多数碳酸盐岩都需要许多预测准确地解决它可以使用传统的μ-CT一个非常耗时的过程孔隙结构复杂 - 无论是与在同步辐射光源的单色光束或台式X射线扫描仪。因此，需要断层的一个快速的方法来查看动态异构碳酸盐反应引起的变化。 的时间量花费图像样本由第通量控制E X射线源。扫描的一种方法很快是使用同步加速器源20的多色光束。这种所谓的&#39;粉红梁"，提供了幅度较多的光级比台式来源，因此，可采取在数万的秒，而不是小时的时间尺度上的图像。一个由偶极磁体的周期结构的波荡产生粉红梁。电子束被迫接受振荡，因为它穿过磁体并因此辐射能量。产生的能量是浓缩缩小波长频带和是非常激烈的。反射镜和过滤器然后用于缩小光的光谱，以适应实验需要。镜吸收高能量光谱而过滤器吸收低能量。因此，可以对光谱缩小到仅使用这些工具的辐射的期望的频带。 但是，使用该强X射线通量是并非没有挑战。该粉红梁频谱的低能量X射线被示例作为热吸收。这可以用的原位装置中的温度控制干扰而引起的 CO 2从溶液中20至exsolve。 的 CO 2 -饱和食盐水是热和压力，因此，在热平衡的变化小可以显著改变的原位流体5的pH值非常敏感。因此，对于X射线光谱仔细设计和控制元件必须纳入之前成像的光束线设备。 快速断层也以高速率产生数据的大量。从照相机和随后的存储读出的数据的限制提供大幅的技术挑战。有些人通过采取几个连续的扫描和读取它们对外部数据服务器之前，相机内存存储他们克服这一点。然而，这需要该实验是relatively短相机内存只能容纳数据的有限体积。分箱相机上的数据也减少，因为它减少了需要被传输的数据量的传送时间，但它具有降低图像的质量的潜力。或者，数据可以在每次扫描后开始下一，这将增加扫描之间的总时间之前传送关闭照相机。该研究中使用与每个图像采集服用〜45秒，并读出取额外〜30秒的数据后一种方法。 当以高速率服用扫描，样品台必须旋转比传统扫描要快得多，因此，在芯保持器的电位角应力是很大的。碳纤维，而X射线透明，强调当是灵活的。如果图像获取图像模糊在采样动作可以发生。芯保持套筒被设计成尽可能的短，以减少这些潜在的应力。此外，灵活的polyeth呃醚酮（PEEK）油管在靠近舞台的实验装置中的所有元素使用，以至于阶段是自由转动。使用的PEEK管的一个缺点是，它是可渗透CO 2上扩散的时间尺度。居住在长时间的线流体将逐渐在一段约24小时成为去饱和。所没有的芯保持器附近的所有系由不锈钢制成的并且流体是预平衡在剧烈混合哈氏反应器加热加压，实验条件23，29，30。 实验设备如图1所示。储温度由包裹套管的外部中的X射线透明加热胶带，并通过电池的径向端口并进入限制流体插入热电偶保持在芯保持器。比例积分ðerivative（PID）控制器然后调节温度到1内 C。压力和流量条件，使用三个高压注射泵是精确到0.001毫升/分钟的流速维持。两种盐被用于实验中，将高吸收25％（重量）的KI不反应盐水和低的吸收1重量％的KCl，5％（重量）的NaCl的反应盐水。在衰减的差异使得它很容易看到反应盐水中的制芯死体积计算不必要的到来。

<table><tbody><tr><td>NaCl salt</td><td>Sigma Aldrich</td><td>S7653-1KG</td><td></td></tr><tr><td>KCl salt</td><td>Sigma Aldrich</td><td>P9333-1KG</td><td></td></tr><tr><td>KI salt</td><td>Sigma Aldrich</td><td>30315-1KG</td><td></td></tr><tr><td>Core holder</td><td>Airbourne Composites</td><td>110 mm Core holder</td><td>Constructed in conjunction with Imperial College</td></tr><tr><td>PEEK tubing</td><td>Kinesis</td><td>1560xL</td><td></td></tr><tr><td>Thermocouple</td><td>Omega Engineering</td><td>KMTSS-IM300U-150</td><td></td></tr><tr><td>Flexible Heating Tape</td><td>Omega Engineering</td><td>KH-112/10-P</td><td></td></tr><tr><td>1/16&quot; Needle Valve</td><td>Hydrasun Ltd</td><td>MVE1002</td><td></td></tr><tr><td>High Pressure Syringe Pump</td><td>Teledyne ISCO</td><td>1000D</td><td></td></tr><tr><td>600 mL Parr Reactor</td><td>Parr Instrument Company</td><td>4547A - hastelloy</td><td></td></tr><tr><td>CO&lt;sub&gt;2&lt;/sub&gt; Cylinder</td><td>BOC</td><td>CO2 - size E</td><td></td></tr><tr><td>Viton</td><td>Fisher Scientific</td><td>11572583</td><td></td></tr><tr><td>Aluminium Foil</td><td>Coroplast</td><td>1510AWX</td><td></td></tr><tr><td>ImageJ - image processing</td><td>NIH</td><td>ImageJ</td><td></td></tr><tr><td>Matlab</td><td>Mathworks</td><td>Matlab</td><td>Used for data analysis</td></tr><tr><td>Avizo</td><td>FEI</td><td>Avizo</td><td></td></tr><tr><td>Snoop Leak Detector</td><td>Swagelok</td><td>MS-SNOOP-8OZ</td><td></td></tr></tbody></table>

dynamic pore-scale reservoir-condition imaging of reaction in carbonates using synchrotron fast tomography

地下存储持久性是碳捕获和储存的主要问题。抽的 CO 2成碳酸盐岩储层有权解散地质密封，并允许二氧化碳逃逸的可能性。然而，在油藏条件下溶解过程知之甚少。因此，需要时间分辨实验在孔隙尺度观察和预测溶出的性质和速度。同步加速器快速层析是采取复杂的孔隙结构的高分辨率时间分辨图像的速度远远超过传统的μ-CT的方法。钻石Lightsource粉红色光束被用来以CO 2 -饱和盐水油藏条件下存在的石灰石动态图像溶解。 100次扫描以6.1微米的分辨率超过2小时内服用。的图像进行分割，并使用图像分析和网络萃取测定的孔隙度和渗透性。孔隙沿lengt均匀地提高样品的小时然而，无论是孔隙度和渗透率的增加速率减慢在稍后的时间。

将反应物在毫米直径的4 1.2厘米长的波特兰碳酸芯42方解石和无缓冲SCCO 2饱和盐水之间进行成像。波特兰碳酸盐是相对纯的（&lt;99％）方解石鲕具有复杂异质孔结构43。低能量的X射线通过使光束穿过的Al 2毫米和Au为0.1μm过滤。一个CdWO 4的闪烁体用1.25X物镜和PCO EDGE相机在检测器组件被使用。干扫描，以4000预测收购而动态扫描相依为命1000预测。总采集时间为约1分钟，每次扫描15秒〜100次扫描所历时2小时。 重建和工件的去除采用钻石Lightsource专有软件完成。每个图像由2000年第3体素，WHI沟道然后分级以6.1微米（ 图5）的分辨率，以增加信号到所得的1000 3体素的图像中的噪声。然后，将图像用在Avizo 8.1和ImageJ的节目图像处理模块处理（见补充文件）。每个图像需要大约12个小时CPU和处理3小时GPU采用了3.0 GHz的CPU和特斯拉K20C GPU的计算机上。 分割图像进行分析，作为通过计算孔隙和岩石的体素的数目的孔隙率变化的时间系列。期间随时间溶解孔隙率的增加（ 图6）。划分图像的目视检查（ 图7）示出了一个信道的在流动方向上的存在。当孔隙率被绘制为的时间和从样品的距离的函数入口显然一个信道在第一小时形成，然后加宽作为实验继续（F<html> igure 8）。 划分图像然后作为输入到网络提取模型来分析通透性改变（ 图9）。据发现，有在初始小时期间急剧增加渗透性，但随后的渗透性稳定在稍后的时间。 <img alt="图1" src="/files/ftp_upload/53763/53763fig1.jpg" /> 图1. 原位实验装置。 CO 2由注射泵加压并用于在反应器中平衡盐水洗涤。反应盐水由接收泵通过芯组件拉出。细胞通过在围泵DI水并通过在限制流体的热电偶控制的加热用加热胶带密闭。实验系统被连接在一起用管路和流体流动用阀（V）和联盟（U）的定向。PS://www-jove-com.bdigitaluss.remotexs.co/files/ftp_upload/53763/53763fig1large.jpg"目标="_空白"&gt;点击此处查看该图的放大版本。 <img alt="图2" src="/files/ftp_upload/53763/53763fig2.jpg" /> 图2.使用两个实验调谐曲线和理论镜面反射率和过滤器传输所计算的钻石LightsourceⅠ-13I粉束的X射线谱。镜子吸收超过30千电子伏的能量;铝和Au分别过滤器吸收低于13和22千电子伏的能量。 <a href="https://www-jove-com.bdigitaluss.remotexs.co/files/ftp_upload/53763/53763fig2large.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/53763/53763fig3.jpg" /> 图3.束线成像装置。在Al和Au片过滤粉红光束，而其余的X射线击中第E磁芯装配。 X射线的一部分被样品吸收，而其余穿过样品并击中该荧光在可见光谱的闪烁体。此可见光然后由物镜聚焦到CCD，它转换该光进入其中像素强度值是由该闪烁体所吸收的X射线的数量的函数的像素化的数字图像。 <a href="https://www-jove-com.bdigitaluss.remotexs.co/files/ftp_upload/53763/53763fig3large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图4" src="/files/ftp_upload/53763/53763fig4.jpg" /> 图4.芯保持器内的芯组件。 PEEK管附连到内部端部配件并通过钢端盖螺纹。芯包裹在铝箔和插入套管。套管然后，在端部配件拉伸以创建一个水密本身人与铝箔的两个附加层被添加到保持在适当位置的一切，并防止气体扩散。热电偶被固定到芯组件的外部与粘合剂的铝箔的外层。图从Menke 等改性。 42。 <a href="https://www-jove-com.bdigitaluss.remotexs.co/files/ftp_upload/53763/53763fig4large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图5" src="/files/ftp_upload/53763/53763fig5.jpg" /> （a）之前和（b）后溶解重构图像的图5 2-D切片。较轻的地区是粮食和暗区是孔隙。在晶/孔边界的边缘模糊所用的孔隙空间（B）的反应的部分可以看到。 <a href="https://www-jove-com.bdigitaluss.remotexs.co/files/ftp_upload/53763/53763fig5large.jpg" target="_blank">请点击此处查看该图的放大版本。</a><html><img alt="图6" src="/files/ftp_upload/53763/53763fig6.jpg" /> 图6.孔隙绘出时间。线性溶出的第二个小时的斜率略有减少孔隙增大。图从Menke 等改性。 42。 <a href="https://www-jove-com.bdigitaluss.remotexs.co/files/ftp_upload/53763/53763fig6large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图7" src="/files/ftp_upload/53763/53763fig7.jpg" /> 在60分钟时在孔隙率变化到实验，其中绿色代表孔隙率变化最大和红最少的图7. 3-D呈现。由流体 - 固体化学反应产生一个清晰的多孔通道被看作在溶解是最大的芯的中心。图从Menke 等改性。"外部参照"&gt; 42。 <a href="https://www-jove-com.bdigitaluss.remotexs.co/files/ftp_upload/53763/53763fig7large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图8" src="/files/ftp_upload/53763/53763fig8.jpg" /> 图8概要孔隙率作为距离从样品入口的功能。孔隙率是沿溶出的轴线均匀，但溶解速率的变化作为时间的函数。图从Menke 等改性。 42。 <a href="https://www-jove-com.bdigitaluss.remotexs.co/files/ftp_upload/53763/53763fig8large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图9" src="/files/ftp_upload/53763/53763fig9.jpg" /> 图9（A）上划分图像进行网络提取显示在60分钟，显示大孔隙（球）和它们的连接（管）。 （B）中所计算的渗透性被示出为增加与时间用40至60分钟之间的急剧上升作为宽溶解信道被建立。图从Menke 等改性。 42。 <a href="https://www-jove-com.bdigitaluss.remotexs.co/files/ftp_upload/53763/53763fig9large.jpg" target="_blank">请点击此处查看该图的放大版本。</a>

Watch this Scientific Journal Video about Dynamic Pore-scale Reservoir-condition Imaging of Reaction in Carbonates Using Synchrotron Fast Tomography at JoVE.com

Dynamic Pore-scale Reservoir-condition Imaging of Reaction in Carbonates Using Synchrotron Fast Tomography

同步快速断层扫描是用来以CO 2 -饱和盐水油藏条件下存在的石灰石动态图像溶解。 100次扫描以6.1微米分辨率在一段2小时服用。

用同步快速反应层析成像动态孔隙规模油藏条件下成像碳酸盐

Underground storage permanence is a major concern for carbon capture and storage. Pumping CO2 into carbonate reservoirs has the potential to dissolve ...

dynamic-pore-scale-reservoir-condition-imaging-reaction-carbonates

Universidad San Sebastian

Research

JoVE Journal

Engineering

8.5K 次观看.  Imperial College London. 同步快速断层扫描是用来以CO 2 -饱和盐水油藏条件下存在的石灰石动态图像溶解。 100次扫描以6.1微米分辨率在一段2小时服用。 

视频: Dynamic Pore-scale Reservoir-condition Imaging of Reaction in Carbonates Using Synchrotron Fast Tomography

Revealing Dynamic Processes of Materials in Liquids Using Liquid Cell Transmission Electron Microscopy

The recent development for in situ transmission electron microscopy, which allows imaging through liquids with high spatial resolution, has attracted significant interests across the research fields of materials science, physics, chemistry and biology. The key enabling technology is a liquid cell. We fabricate liquid cells with thin viewing windows through a sequential microfabrication process, including silicon nitride membrane deposition, photolithographic patterning, wafer etching, cell bonding, etc. A liquid cell with the dimensions of a regular TEM grid can fit in any standard TEM sample holder. About 100 nanoliters reaction solution is loaded into the reservoirs and about 30 picoliters liquid is drawn into the viewing windows by capillary force. Subsequently, the cell is sealed and loaded into a microscope for in situ imaging. Inside the TEM, the electron beam goes through the thin liquid layer sandwiched between two silicon nitride membranes. Dynamic processes of nanoparticles in liquids, such as nucleation and growth of nanocrystals, diffusion and assembly of nanoparticles, etc., have been imaged in real time with sub-nanometer resolution. We have also applied this method to other research areas, e.g., imaging proteins in water. Liquid cell TEM is poised to play a major role in revealing dynamic processes of materials in their working environments. It may also bring high impact in the study of biological processes in their native environment.

We have developed a self-contained liquid cell, which allows imaging through liquids using a transmission electron microscope. Dynamic processes of nanoparticles in liquids can be revealed in real time with sub-nanometer resolution.

在液体中使用液体池透射电子显微镜揭示材料的动态过程

The recent development for in situ transmission electron microscopy, which allows imaging through liquids with high spatial resolution, has attracted ...

科研

工程学

Characterization of Electrode Materials for Lithium Ion and Sodium Ion Batteries Using Synchrotron Radiation Techniques

Intercalation compounds such as transition metal oxides or phosphates are the most commonly used electrode materials in Li-ion and Na-ion batteries. During insertion or removal of alkali metal ions, the redox states of transition metals in the compounds change and structural transformations such as phase transitions and/or lattice parameter increases or decreases occur. These behaviors in turn determine important characteristics of the batteries such as the potential profiles, rate capabilities, and cycle lives. The extremely bright and tunable x-rays produced by synchrotron radiation allow rapid acquisition of high-resolution data that provide information about these processes. Transformations in the bulk materials, such as phase transitions, can be directly observed using X-ray diffraction (XRD), while X-ray absorption spectroscopy (XAS) gives information about the local electronic and geometric structures (e.g.&#160;changes in redox states and bond lengths). In situ experiments carried out on operating cells are particularly useful because they allow direct correlation between the electrochemical and structural properties of the materials. These experiments are time-consuming and can be challenging to design due to the reactivity and air-sensitivity of the alkali metal anodes used in the half-cell configurations, and/or the possibility of signal interference from other cell components and hardware. For these reasons, it is appropriate to carry out ex situ experiments (e.g.&#160;on electrodes harvested from partially charged or cycled cells) in some cases. Here, we present detailed protocols for the preparation of both ex situ and in situ samples for experiments involving synchrotron radiation and demonstrate how these experiments are done.

We describe the use of synchrotron X-ray absorption spectroscopy (XAS) and X-ray diffraction (XRD) techniques to probe details of intercalation/deintercalation processes in electrode materials for Li-ion and Na-ion batteries. Both in situ and ex situ experiments are used to understand structural behavior relevant to the operation of devices

正极材料的同步辐射技术锂离子和钠离子电池表征

Intercalation compounds such as transition metal oxides or phosphates are the most commonly used electrode materials in Li-ion and Na-ion batteries. ...

Reservoir Condition Pore-scale Imaging of Multiple Fluid Phases Using X-ray Microtomography

X-ray microtomography was used to image, at a resolution of 6.6 &#181;m, the pore-scale arrangement of residual carbon dioxide ganglia in the pore-space of a carbonate rock at pressures and temperatures representative of typical formations used for CO2 storage. Chemical equilibrium between the CO2, brine and rock phases was maintained using a high pressure high temperature reactor, replicating conditions far away from the injection site. Fluid flow was controlled using high pressure high temperature syringe pumps. To maintain representative in-situ conditions within the micro-CT scanner a carbon fiber high pressure micro-CT coreholder was used. Diffusive CO2 exchange across the confining sleeve from the pore-space of the rock to the confining fluid was prevented by surrounding the core with a triple wrap of aluminum foil. Reconstructed brine contrast was modeled using a polychromatic x-ray source, and brine composition was chosen to maximize the three phase contrast between the two fluids and the rock. Flexible flow lines were used to reduce forces on the sample during image acquisition, potentially causing unwanted sample motion, a major shortcoming in previous techniques. An internal thermocouple, placed directly adjacent to the rock core, coupled with an external flexible heating wrap and a PID controller was used to maintain a constant temperature within the flow cell. Substantial amounts of CO2 were trapped, with a residual saturation of 0.203 &#177; 0.013, and the sizes of larger volume ganglia obey power law distributions, consistent with percolation theory.

We present a methodology for the imaging of multiple fluid phases at reservoir conditions by the use of x-ray microtomography. We show some representative results of capillary trapping in a carbonate rock sample.

多重流体相储层孔隙条件级成像使用X射线微断层

X-ray microtomography was used to image, at a resolution of 6.6 &#181;m, the pore-scale arrangement of residual carbon dioxide ganglia in the pore-space ...

Non-invasive 3D-Visualization with Sub-micron Resolution Using Synchrotron-X-ray-tomography

Little is known about the internal organization of many micro-arthropods with body sizes below 1 mm. The reasons for that are the small size and the hard cuticle which makes it difficult to use protocols of classical histology. In addition, histological sectioning destroys the sample and can therefore not be used for unique material. Hence, a non-destructive method is desirable which allows to view inside small samples without the need of sectioning.
We used synchrotron X-ray tomography at the European Synchrotron Radiation Facility (ESRF) in Grenoble (France) to non-invasively produce 3D tomographic datasets with a pixel-resolution of 0.7&micro;m. Using volume rendering software, this allows us to reconstruct the internal organization in its natural state without the artefacts produced by histological sectioning. These date can be used for quantitative morphology, landmarks, or for the visualization of animated movies to understand the structure of hidden body parts and to follow complete organ systems or tissues through the samples.

We used synchrotron X-ray tomography at the European Synchrotron Radiation Facility (ESRF) to non-invasively produce 3D tomographic datasets with a pixel-resolution of 0.7&micro;m. Using volume rendering software, this allows the reconstruction of internal structures in their natural state without the artefacts produced by histological sectioning.

非侵入性的三维可视化与亚微米分辨率使用同步加速器X射线断层扫描

Little is known about the internal organization of many micro-arthropods with body sizes below 1 mm. The reasons for that are the small size and the hard ...

生物学

Stress Distribution During Cold Compression of Rocks and Mineral Aggregates Using Synchrotron-based X-Ray Diffraction

We report detailed procedures for performing compression experiments on rocks and mineral aggregates within a multi-anvil deformation apparatus (D-DIA) coupled with synchrotron X-radiation. A cube-shaped sample assembly is prepared and compressed, at room temperature, by a set of four X-ray transparent sintered diamond anvils and two tungsten carbide anvils, in the lateral and the vertical planes, respectively. All six anvils are housed within a 250-ton hydraulic press and driven inward simultaneously by two wedged guide blocks. A horizontal energy dispersive X-ray beam is projected through and diffracted by the sample assembly. The beam is commonly in the mode of either white or monochromatic X-ray. In the case of white X-ray, the diffracted X-rays are detected by a solid-state detector array that collects the resulting energy dispersive diffraction pattern. In the case of monochromatic X-ray, the diffracted pattern is recorded using a two-dimensional (2-D) detector, such as an imaging plate or a charge-coupled device (CCD) detector. The 2-D diffraction patterns are analyzed to derive lattice spacings. The elastic strains of the sample are derived from the atomic lattice spacing within grains. The stress is then calculated using the predetermined elastic modulus and the elastic strain. Furthermore, the stress distribution in two-dimensions allow for understanding how stress is distributed in different orientations. In addition, a scintillator in the X-ray path yields a visible light image of the sample environment, which allows for the precise measurement of sample length changes during the experiment, yielding a direct measurement of volume strain on the sample. This type of experiment can quantify the stress distribution within geomaterials, which can ultimately shed light on the mechanism responsible for compaction. Such knowledge has the potential to significantly improve our understanding of key processes in rock mechanics, geotechnical engineering, mineral physics, and material science applications where compactive processes are important.

We report detailed procedures for compression experiments on rocks and mineral aggregates within a multi-anvil deformation apparatus coupled with synchrotron X-radiation. Such experiments allow quantification of the stress distribution within samples, that ultimately sheds light on compaction processes in geomaterials.

基于同步辐射 x 射线衍射的岩石和矿物团聚体冷压缩应力分布

We report detailed procedures for performing compression experiments on rocks and mineral aggregates within a multi-anvil deformation apparatus (D-DIA) ...

环境科学

Atom Probe Tomography Analysis of Exsolved Mineral Phases

Element diffusion rates and temperature/pressure control a range of fundamental volcanic and metamorphic processes. Such processes are often recorded in lamellae exsolved from host mineral phases. Thus, the analysis of the orientation, size, morphology, composition and spacing of exsolution lamellae is an area of active research in the geosciences. The conventional study of these lamellae has been conducted by scanning electron microscopy (SEM) and transmission electron microscopy (TEM), and more recently with focused ion beam (FIB)-based nanotomography, yet with limited chemical information. Here, we explore the use of atom probe tomography (APT) for the nanoscale analysis of ilmenite exsolution lamellae in igneous titanomagnetite from ash deposits erupted from the active Soufri&#232;re Hills Volcano (Montserrat, British West Indies). APT allows the precise calculation of interlamellar spacings (14&#8211;29 &#177; 2 nm) and reveals smooth diffusion profiles with no sharp phase boundaries during the exchange of Fe and Ti/O between the exsolved lamellae and the host crystal. Our results suggest that this novel approach permits nanoscale measurements of lamellae composition and interlamellar spacing that may provide a means to estimate the lava dome temperatures necessary to model extrusion rates and lava dome failure, both of which play a key role in volcanic hazard mitigation efforts.

Analysis of the morphology, composition, and spacing of exsolution lamellae can provide essential information to understand geological processes related to volcanism and metamorphism. We present a novel application of APT for the characterization of such lamellae and compare this approach to the conventional use of electron microscopy and FIB-based nanotomography.

原子探针断层扫描分析的解脱矿物相

Element diffusion rates and temperature/pressure control a range of fundamental volcanic and metamorphic processes. Such processes are often recorded in ...

Pore-scale Imaging and Characterization of Hydrocarbon Reservoir Rock Wettability at Subsurface Conditions Using X-ray Microtomography

In situ wettability measurements in hydrocarbon reservoir rocks have only been possible recently. The purpose of this work is to present a protocol to characterize the complex wetting conditions of hydrocarbon reservoir rock using pore-scale three-dimensional X-ray imaging at subsurface conditions. In this work, heterogeneous carbonate reservoir rocks, extracted from a very large producing oil field, have been used to demonstrate the protocol. The rocks are saturated with brine and oil and aged over three weeks at subsurface conditions to replicate the wettability conditions that typically exist in hydrocarbon reservoirs (known as mixed-wettability). After the brine injection, high-resolution three-dimensional images (2 &#181;m/voxel) are acquired and then processed and segmented. To calculate the distribution of the contact angle, which defines the wettability, the following steps are performed. First, fluid-fluid and fluid-rock surfaces are meshed. The surfaces are smoothed to remove voxel artefacts, and in situ contact angles are measured at the three-phase contact line throughout the whole image. The main advantage of this method is its ability to characterize in situ wettability accounting for pore-scale rock properties, such as rock surface roughness, rock chemical composition, and pore size. The in situ wettability is determined rapidly at hundreds of thousands of points. 
The method is limited by the segmentation accuracy and X-ray image resolution. This protocol could be used to characterize the wettability of other complex rocks saturated with different fluids and at different conditions for a variety of applications. For example, it could help in determining the optimal wettability that could yield an extra oil recovery (i.e., designing brine salinity accordingly to obtain higher oil recovery) and to find the most efficient wetting conditions to trap more CO2 in subsurface formations.

This protocol is presented to characterize the complex wetting conditions of an opaque porous medium (hydrocarbon reservoir rock) using three-dimensional images obtained by X-ray microtomography at subsurface conditions.

利用 X 射线层析在地下条件下油气储层岩石润湿性的孔隙度成像与表征

In situ wettability measurements in hydrocarbon reservoir rocks have only been possible recently. The purpose of this work is to present a protocol to ...

Visualization of Failure and the Associated Grain-Scale Mechanical Behavior of Granular Soils under Shear using Synchrotron X-Ray Micro-Tomography

The rapid development of X-ray imaging techniques with image processing and analysis skills has enabled the acquisition of CT images of granular soils with high-spatial resolutions. Based on such CT images, grain-scale mechanical behavior such as particle kinematics (i.e., particle translations and particle rotations), strain localization and inter-particle contact evolution of granular soils can be quantitatively investigated. However, this is inaccessible using conventional experimental methods. This study demonstrates the exploration of the grain-scale mechanical behavior of a granular soil sample under triaxial compression using synchrotron X-ray micro-tomography (&#956;CT). With this method, a specially fabricated miniature loading apparatus is used to apply confining and axial stresses to the sample during the triaxial test. The apparatus is fitted into a synchrotron X-ray tomography setup so that high-spatial resolution CT images of the sample can be collected at different loading stages of the test without any disturbance to the sample. With the capability of extracting information at the macro scale (e.g., sample boundary stresses and strains from the triaxial apparatus setup) and the grain scale (e.g., grain movements and contact interactions from the CT images), this procedure provides an effective methodology to investigate the multi-scale mechanics of granular soils.

The protocol describes procedures to acquire high-spatial resolution computed tomography (CT) images of a granular soil during triaxial compression, and to apply image processing techniques to these CT images to explore the grain-scale mechanical behavior of the soil under loading.

使用同步加速器 X 射线微断层扫描技术，在剪切下对颗粒土壤的故障和相关的颗粒级机械性能进行可视化

The rapid development of X-ray imaging techniques with image processing and analysis skills has enabled the acquisition of CT images of granular soils ...

Visualization of ATP Synthase Dimers in Mitochondria by Electron Cryo-tomography

Electron cryo-tomography is a powerful tool in structural biology, capable of visualizing the three-dimensional structure of biological samples, such as cells, organelles, membrane vesicles, or viruses at molecular detail. To achieve this, the aqueous sample is rapidly vitrified in liquid ethane, which preserves it in a close-to-native, frozen-hydrated state. In the electron microscope, tilt series are recorded at liquid nitrogen temperature, from which 3D tomograms are reconstructed. The signal-to-noise ratio of the tomographic volume is inherently low. Recognizable, recurring features are enhanced by subtomogram averaging, by which individual subvolumes are cut out, aligned and averaged to reduce noise. In this way, 3D maps with a resolution of 2 nm or better can be obtained. A fit of available high-resolution structures to the 3D volume then produces atomic models of protein complexes in their native environment. Here we show how we use electron cryo-tomography to study the in situ organization of large membrane protein complexes in mitochondria. We find that ATP synthases are organized in rows of dimers along highly curved apices of the inner membrane cristae, whereas complex I is randomly distributed in the membrane regions on either side of the rows. By subtomogram averaging we obtained a structure of the mitochondrial ATP synthase dimer within the cristae membrane.

We present a protocol of how to collect and process electron cryo-tomograms of whole mitochondria. The technique provides detailed insights into the structure, function, and organization of large membrane protein complexes in native biological membranes.

ATP合酶二聚体线粒体通过冷冻电子断层扫描可视化

Electron cryo-tomography is a powerful tool in structural biology, capable of visualizing the three-dimensional structure of biological samples, such as ...

A 3D Cartographic Description of the Cell by Cryo Soft X-ray Tomography

Imaging techniques are fundamental in order to understand cell organization and machinery in biological research and the related fields. Among these techniques, cryo soft X-ray tomography (SXT) allows imaging whole cryo-preserved cells in the water window X-ray energy range (284-543 eV), in which carbon structures have intrinsically higher absorption than water, allowing the 3D reconstruction of the linear absorption coefficient of the material contained in each voxel. Quantitative structural information at the level of whole cells up to 10 &#181;m thick is then achievable this way, with high throughput and spatial resolution down to 25-30 nm half-pitch. Cryo-SXT has proven itself relevant to current biomedical research, providing 3D information on cellular infection processes (virus, bacteria, or parasites), morphological changes due to diseases (such as recessive genetic diseases) and helping us understand drug action at the cellular level, or locating specific structures in the 3D cellular environment. In addition, by taking advantage of the tunable wavelength at synchrotron facilities, spectro-microscopy or its 3D counterpart, spectro-tomography, can also be used to image and quantify specific elements in the cell, such as calcium in biomineralization processes. Cryo-SXT provides complementary information to other biological imaging techniques such as electron microscopy, X-ray fluorescence or visible light fluorescence, and is generally used as a partner method for 2D or 3D correlative imaging at cryogenic conditions in order to link function, location, and morphology.

Here, a protocol describing the sample preparation and data collection steps required in cryo soft X-ray tomography (SXT) to image the ultrastructure of whole cryo-preserved cells at a resolution of 25 nm half pitch, is presented.

通过冷冻软X射线断层扫描对细胞进行3D制图描述

Imaging techniques are fundamental in order to understand cell organization and machinery in biological research and the related fields. Among these ...