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Preparation of High-Quality Load-Preserved Fabric Clay Samples for Microstructural Characterizations: A Pragmatic Guide Featuring a 3-D-Printed Oedometer

机译:制备用于微观结构表征的高品质负载保留织物黏土样品:实用的指南,包含3D打印的里程表

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High-quality samples are always critical in the meaningful microstructural characterizations of clay. A practical guide, together with a real sample tested as an example, is therefore proposed in this study, aiming to prepare high-quality load-preserved fabric clay samples subjected to 1-D consolidation for the pore size and fabric characterizations. In this guide, several issues often encountered in sample preparations that may induce measurement bias are tackled with feasible solutions proposed. A tailor-made oedometer is also invented and produced using a 3-D printing technique to achieve the goal. First, a homogenous and uniformkaolinite sample is prepared from a slurry state and then positioned in the 3-D-printed oedometer for 1-D consolidation tests. Then, together with the desired load, the whole 3-D-printed oedometer containing the consolidated kaolinite sample is submerged into liquid nitrogen to rapid freeze the sample to preserve the fabric associations not affected by the unloading effects. Afterward, to use the same sample for different tests to facilitate comparisons, the sample is cut in half while frozen. On one hand, this creates an observation plane along the center of the sample with the morphological information preserved for the subsequent scanning electron microscopy (SEM) analyses. On the other hand, each half of the sample individually undergoes the mercury intrusion porosimetry (MIP) and nitrogen adsorption (NA) analyses to obtain complementary information on the pore-size distribution. The samples must be dewatered by freeze drying before conducting these tests. During the freeze-drying process, the cut sample is protected by a 3- D-printed container, which has a reference mark to indicate the sample orientation. In each of the SEM images taken, the associated position and orientation are controlled, and the number of the images taken for analyses is maximized to enhance the statistical representation of the analyzed results.
机译:在有意义的粘土微观结构表征中,高质量的样品始终至关重要。因此,在本研究中提出了实用指南以及经过测试的实际样品作为示例,旨在制备经过一维固结的高质量载荷保持型织物粘土样品,以进行孔径和织物表征。在本指南中,提出了可行的解决方案,解决了样品制备中经常遇到的可能引起测量偏差的问题。还使用3-D打印技术发明并生产了量身定制的里程表,以实现该目标。首先,从浆态制备均质且均匀的高岭土样品,然后将其放置在3-D打印的里程表中进行1-D固结测试。然后,连同所需的载荷一起,将包含固结高岭石样品的整个3D打印里程表浸入液氮中,以快速冷冻样品,以保留不受卸荷影响的织物缔合。然后,为了将同一样品用于不同的测试以方便比较,将样品冷冻时切成两半。一方面,这会沿着样品的中心创建一个观察平面,并保留形态信息以供随后的扫描电子显微镜(SEM)分析。另一方面,样品的每半分别进行压汞法(MIP)和氮吸附(NA)分析,以获得有关孔径分布的补充信息。在进行这些测试之前,必须通过冷冻干燥将样品脱水。在冷冻干燥过程中,切割后的样品由3D打印的容器保护,该容器带有参考标记以指示样品的方向。在拍摄的每张SEM图像中,控制相关的位置和方向,并获取用于分析的图像数量最大化,以增强分析结果的统计表示。

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