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Comparison of three measurement modalities for 3D characterization of manufactured features and process-induced porosity in titanium alloy additively manufactured parts 钛合金增材制造零件制造特征和工艺诱导孔隙度三维表征的三种测量方式的比较
Pub Date : 2025-06-08 DOI: 10.1016/j.tmater.2025.100070
Andrew Townsend , Chen Yee , Bryce Jolley , Nikola Draganic , Michael Chapman , Daniel Sparkman , Michael D. Uchic
Nondestructive characterization of internal features and defects within complex components is vital for many industrial applications, particularly with the advent of additive manufacturing (AM) technologies. However, community understanding of the limitations of nondestructive methods such as X-ray Computed Tomography (CT) can be limited in certain industrial sectors as these may be emergent applications. In this paper, we investigate the limits of X-ray CT measurements and compare extracted data with mechanical polishing serial sectioning (MPSS) and confocal laser scanning microscopy (CLSM). The test object is an additively manufactured titanium alloy disk that contains both process-induced porosity and machined features, including focused ion beam milled features designed to probe the resolution limits of X-ray CT. Results show that each of these characterization techniques has advantages and disadvantages. We compare data acquisition times, spatial resolution, geometric measurement accuracy and defect visualization fidelity across these modalities to establish a practical framework.
复杂部件内部特征和缺陷的无损表征对于许多工业应用至关重要,特别是随着增材制造(AM)技术的出现。然而,社会对非破坏性方法(如x射线计算机断层扫描(CT))的局限性的理解在某些工业部门可能受到限制,因为这些方法可能是紧急应用。本文研究了x射线CT测量的局限性,并将提取的数据与机械抛光连续切片(MPSS)和共聚焦激光扫描显微镜(CLSM)进行了比较。测试对象是一个增材制造的钛合金圆盘,包含工艺引起的孔隙和加工特征,包括用于探测x射线CT分辨率极限的聚焦离子束铣削特征。结果表明,每种表征技术都有其优缺点。我们比较了这些模式的数据采集时间、空间分辨率、几何测量精度和缺陷可视化保真度,以建立一个实用的框架。
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引用次数: 0
Correlative X-ray and electron tomography for scale-bridging, quantitative analysis of complex, hierarchical particle systems 相关的x射线和电子断层扫描用于规模桥接,复杂的定量分析,分层粒子系统
Pub Date : 2025-06-06 DOI: 10.1016/j.tmater.2025.100069
Alexander Götz , Fabian Lutter , Dennis Simon Possart , Daniel Augsburger , Usman Arslan , Sabrina Pechmann , Carmen Rubach , Moritz Buwen , Umair Sultan , Alexander Kichigin , Johannes Böhmer , Nora Vorlaufer , Peter Suter , Tor Hildebrand , Matthias Thommes , Peter Felfer , Nicolas Vogel , Katharina Breininger , Silke Christiansen , Benjamin Apeleo Zubiri , Erdmann Spiecker
This study presents a comprehensive workflow for investigating particulate materials through combined 360° electron tomography (ET), nano-computed X-ray tomography (nanoCT), and micro-computed X-ray tomography (microCT), alongside a versatile sample preparation routine. The workflow enables the investigation of size, morphology, and pore systems across multiple scales, from individual particles to large hierarchical structures. A customized tapered sample shape is created using focused ion beam milling to optimize the field of view for each imaging technique. This design enables high-resolution analysis of small volumes containing single particles using nanoCT and large-scale studies of thousands of particles for statistical significance using microCT. By correlating data from identical locations across different microCT and nanoCT imaging modalities - without any additional preparation that could affect the sample in between - the presented approach improves the precision of quantitative analyses. The study highlights the importance of cross-scale, correlative three-dimensional microscopy for a comprehensive understanding of complex hierarchical materials. Precise data registration, segmentation using machine learning, and multimodal imaging techniques are crucial for unlocking insights into process-structure-property relationships and thus to optimize functional, hierarchical materials.
本研究通过360°电子断层扫描(ET)、纳米计算机x射线断层扫描(nanoCT)和微计算机x射线断层扫描(microCT)以及通用的样品制备程序,提出了一个全面的工作流程来研究颗粒材料。该工作流程可以跨多个尺度(从单个颗粒到大型分层结构)研究尺寸、形态和孔隙系统。使用聚焦离子束铣削创建定制的锥形样品形状,以优化每种成像技术的视野。该设计可以使用纳米oct对含有单个颗粒的小体积进行高分辨率分析,并使用微ct对数千个颗粒进行大规模研究,以获得统计显著性。通过将来自不同微ct和纳米oct成像模式的相同位置的数据关联起来,而无需任何可能影响两者之间样品的额外准备,所提出的方法提高了定量分析的精度。该研究强调了跨尺度、相关三维显微镜对全面了解复杂分层材料的重要性。精确的数据配准、使用机器学习的分割和多模态成像技术对于了解工艺-结构-属性关系,从而优化功能、分层材料至关重要。
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引用次数: 0
Improving electron tomography of mesoporous silica by Ga intrusion 镓侵入改进介孔二氧化硅电子层析成像
Pub Date : 2025-05-14 DOI: 10.1016/j.tmater.2025.100068
Alexander Kichigin , Johannes Böhmer , Moritz Buwen , Benjamin Apeleo Zubiri , Mingjian Wu , Johannes Will , Dominik Drobek , Alexander Götz , Nora Vorlaufer , Jakob Söllner , Matthias Thommes , Peter Felfer , Thomas Przybilla , Erdmann Spiecker
Electron tomography (ET) offers nanoscale 3D characterization of mesoporous materials but is often limited by their low scattering contrast. Here, we introduce a gallium (Ga) intrusion strategy for mesoporous silica that dramatically improves imaging contrast – a key benefit that enables more accurate 3D reconstructions. By infiltrating Ga through a modified mercury intrusion porosimetry process, the high-angle annular dark-field (HAADF) STEM signal is enhanced by 5 times, resulting in a 34 % improvement in reconstruction resolution and a 49 % enhancement in interface sharpness. In addition, the increased sample conductivity facilitates focused ion beam (FIB) milling by minimizing charging effects and reducing drift. This approach enables precise segmentation and quantitative analysis of pore connectivity and size distribution, thereby extending the applicability of ET to light-element non-conductive materials and advancing structure-property characterization of complex porous systems.
电子断层扫描(ET)提供了介孔材料的纳米级三维表征,但往往受到其低散射对比度的限制。在这里,我们介绍了一种介孔二氧化硅的镓(Ga)侵入策略,该策略显着提高了成像对比度-这是实现更精确的3D重建的关键优势。通过改进的压汞孔隙法渗透Ga,高角环形暗场(HAADF) STEM信号增强了5倍,重建分辨率提高了34 %,界面清晰度提高了49 %。此外,增加的样品电导率通过最小化电荷效应和减少漂移,促进了聚焦离子束(FIB)铣削。该方法能够精确分割和定量分析孔隙连通性和尺寸分布,从而将ET扩展到轻元素非导电材料的适用性,并推进复杂多孔体系的结构-性能表征。
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引用次数: 0
Single-particle geometries of pharmaceutical powders from X-ray tomography; a simple and reliable sample preparation method x射线层析成像药物粉末的单颗粒几何形状一种简单可靠的样品制备方法
Pub Date : 2025-04-26 DOI: 10.1016/j.tmater.2025.100067
Dingeman L.H. van der Haven , Jan L. Andreasen , Umair Zafar , Ioannis S. Fragkopoulos , James A. Elliott
The size and shape of the particles within a powder are critical quality-control attributes in the pharmaceutical industry. These microscopic attributes significantly affect the macroscopic properties of the powder, such as the bulk density and flowability. Methods for determining the particle size distribution (PSD) and characterisation of particle shape are therefore essential but can be extremely challenging, particularly when looking at individual particle shapes. This work introduces a new sample preparation method for X-ray micro-computed tomography (μCT) that is convenient, fast, and produces well-dispersed samples, allowing the identification of individual particles. The resulting contrast is excellent even for organic pharmaceutical powders, which are often challenging to image due to the low attenuation coefficient of their components. Simultaneously, an analysis method is proposed that reliably applies to all tested powders, automatically filtering out artefacts such as bubbles. The combined method unambiguously identifies individual particles, allowing the determination of PSD, particle shape classification, and analysis of the internal morphology of particles. Validation is provided through comparisons with laser diffraction, sieve analysis, and optical microscopy. While this new standardised μCT method is slightly more labour intensive than other characterisation methods, it requires only a minimal amount of material (∼15 mg) and provides superior morphological information, which can be used to help explain or predict bulk properties. This is particularly beneficial in early-phase development, where access to large quantities of powder is limited.
粉末中颗粒的大小和形状是制药工业中关键的质量控制属性。这些微观属性显著影响粉末的宏观性能,如堆积密度和流动性。因此,确定颗粒大小分布(PSD)和颗粒形状表征的方法是必不可少的,但可能极具挑战性,特别是在观察单个颗粒形状时。本工作介绍了一种新的x射线微计算机断层扫描(μCT)样品制备方法,该方法方便、快速、样品分散良好,可以识别单个颗粒。由此产生的对比度是优秀的,甚至有机药物粉末,这往往是具有挑战性的图像,由于其成分的低衰减系数。同时,提出了一种可靠地适用于所有被测粉末的分析方法,自动过滤掉气泡等伪影。该组合方法明确地识别单个颗粒,允许确定PSD,颗粒形状分类,并分析颗粒的内部形态。通过与激光衍射、筛析和光学显微镜的比较验证。虽然这种新的标准化μCT方法比其他表征方法稍微需要更多的劳动密集型,但它只需要最少量的材料(~ 15 mg),并提供优越的形态信息,可用于帮助解释或预测体积性质。这在早期开发阶段尤其有益,因为获得大量粉末是有限的。
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引用次数: 0
Individual component-based parameter-adaptive segmentation approach for improved segmentation of synchrotron µCT data of osteocyte lacunae in bone tissue 基于个体分量的参数自适应分割方法改进骨组织中骨细胞腔隙同步加速器微CT数据的分割
Pub Date : 2025-04-13 DOI: 10.1016/j.tmater.2025.100066
Jan Mölich , Sophie Anuth , Jussi-Petteri Suuronen , Emely Bortel , Javier Gerber , Enni Mattern , Timm Weitkamp , Katja Nelson , Susanne Nahles , Bernhard Hesse
Bone tissue is highly complex and dynamic, capable of adapting to mechanical demands and repairing itself through remodeling processes. This remodeling results in a heterogeneous mineral distribution, with lower mineralization in younger bone regions and higher mineralization in older ones. Osteocytes - bone cells residing in small lacunae within the mineralized bone matrix - orchestrate this remodeling. Additionally, osteocytes actively modify their peri-lacunar mineralized tissue. These characteristics, combined with the high osteocyte density of several tens of thousands per mm³ , make the distribution, size, and shape of osteocyte lacunae highly relevant characteristics of bone tissue. To study osteocyte lacunar properties, synchrotron-based computed tomography (µCT) has become increasingly popular over the past decade due to its combination of high spatial resolution, sensitivity to mineral density variations, and rapid data acquisition. However, segmenting lacunae and quantifying their properties remains challenging. Osteocyte lacunae exhibit diverse shapes and sizes, and their surrounding mineral density can vary significantly between lacunae, even within the same tissue sample. Consequently, no global gray value threshold can provide an equally accurate segmentation across different tissue regions within the same sample. More advanced segmentation techniques, such as those based on top-hat transformations, require the definition of a structuring element whose size must be tailored to the feature size, in this case, the lacunae. In this study, we propose a novel approach to segmentation that adjusts the threshold value and the size of the structuring element for each lacuna individually. This method, referred to as the Kangaroo Segmentation Approach, involves an initial rough segmentation, followed by connected-component analysis and refinement steps applied to each component. The results of this Kangaroo Segmentation Approach are compared with conventional Otsu thresholding and thresholding methods based on top-hat transformations. Our findings demonstrate a significant improvement in segmentation accuracy with the proposed method.
骨组织是高度复杂和动态的,能够适应机械需求并通过重塑过程自我修复。这种重塑导致矿物分布不均匀,年轻骨区矿化程度较低,而年老骨区矿化程度较高。骨细胞-位于矿化骨基质内的小腔隙中的骨细胞-协调这种重塑。此外,骨细胞积极改变腔隙周围矿化组织。这些特征,再加上每毫米³数万个骨细胞的高密度 ,使得骨细胞腔隙的分布、大小和形状与骨组织的特征高度相关。为了研究骨细胞腔隙特性,基于同步加速器的计算机断层扫描(µCT)由于其高空间分辨率、对矿物质密度变化的敏感性和快速数据采集的结合,在过去十年中变得越来越流行。然而,分割腔隙并量化其性质仍然具有挑战性。骨细胞腔隙表现出不同的形状和大小,即使在相同的组织样本中,其周围的矿物质密度在腔隙之间也会有显著差异。因此,没有全局灰度值阈值可以在同一样本内的不同组织区域提供同样准确的分割。更高级的分割技术,比如那些基于顶帽转换的分割技术,需要定义一个结构元素,其大小必须与特征大小相适应,在本例中是指空隙。在这项研究中,我们提出了一种新的分割方法,该方法可以单独调整每个空白的阈值和结构元素的大小。这种方法被称为袋鼠分割方法,包括初始的粗略分割,然后对每个组件进行连接组件分析和细化步骤。将袋鼠分割方法与传统的Otsu阈值分割方法和基于顶帽变换的阈值分割方法进行了比较。我们的研究结果表明,该方法显著提高了分割精度。
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引用次数: 0
Measuring thermal curing induced shrinkage of material extrusion based additive manufacturing silicone elastomer lattices by X-ray computed tomography 用x射线计算机断层扫描测量基于增材制造硅弹性体晶格的材料挤压热固化诱导收缩
Pub Date : 2025-04-11 DOI: 10.1016/j.tmater.2025.100064
Massimiliano Ferrucci , Anne-Françoise Obaton , Robert Cerda , Brian Au , Nicholas Rodriguez , Ziad Ammar , Gabriel Balensiefer , Chuck Divin , Jeremy Lenhardt , Brian Giera
Thermal curing induces shrinkage in material extrusion based additive manufacturing silicone elastomer samples, resulting in discrepancies between as printed and final geometries. Knowing the extent to which the samples change in shape and size allows us to make appropriate modifications to the printing design to better control the geometry of the samples. We present an X-ray computed tomography (CT) based approach to determine filament-level shrinkage due to thermal curing of silicone elastomer samples printed with direct ink writing (DIW). The approach relies on custom-designed build plates that are resistant to the elevated curing temperatures and that have sufficiently distinct X-ray absorption characteristics from the silicone elastomer to ensure adequate segmentation of the latter in X-ray imaging data. We implement the approach to evaluate shrinkage in DIW ‘log pile’ samples with three distinct strand arrangements and demonstrate of how filament-level information can be extracted from the X-ray CT data.
热固化诱导收缩材料挤压为基础的增材制造硅弹性体样品,导致打印和最终几何形状之间的差异。了解样品在形状和尺寸上的变化程度,使我们能够对印刷设计进行适当的修改,以更好地控制样品的几何形状。我们提出了一种基于x射线计算机断层扫描(CT)的方法来确定用直接墨水书写(DIW)打印的硅弹性体样品的热固化引起的长丝级收缩。该方法依赖于定制设计的构建板,这些构建板可以抵抗较高的固化温度,并且与有机硅弹性体具有足够不同的x射线吸收特性,以确保在x射线成像数据中对后者进行充分的分割。我们采用该方法来评估具有三种不同链排列的DIW“原木桩”样品的收缩率,并演示如何从x射线CT数据中提取长丝级信息。
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引用次数: 0
In-depth analysis of CT resolution impact on porosity evaluation in laser powder bed fusion additive manufacturing 深入分析 CT 分辨率对激光粉末床熔融增材制造中孔隙率评估的影响
Pub Date : 2025-04-08 DOI: 10.1016/j.tmater.2025.100065
Jitendra Singh Rathore , Andrew King , Florian Le Bourdais , Jean-Paul Garandet
Accurate porosity determination of Additive Manufacturing (AM) parts remains a key challenge. This study provides an in-depth analysis of how computed tomography (CT) resolution affects porosity detection in Laser Powder Bed Fusion (LPBF) manufactured parts by comparing X-ray based measurements from laboratory and synchrotron sources. To represent a range of porosity levels, three samples were selected from an extensive set of LPBF experiments, of respectively low, medium, and high porosities. A laboratory source based computed tomography system was used for the acquisition at the best resolution considering the size limitation due to the sample geometry. In order to achieve higher resolution, a synchrotron source was additionally utilized. The comparative analysis revealed that the porosity measurements from both the laboratory and synchrotron sources were in good agreement for samples with low and high porosity levels. This indicates that for extreme ends of the studied porosity spectrum, laboratory CT systems can provide reliable measurements. However, for the sample with medium porosity, the limited resolution of the laboratory CT leads to an overestimation compared to the synchrotron CT results. This discrepancy is found to be due to inaccuracies in detecting and clustering neighboring pores, leading to an overestimation of porosity. A comparison of the obtained results with the porosity determinations by the widely used Archimedes method is proposed to show the potential and the limitations of each technique for the assessment of additively manufactured parts.
精确测定增材制造(AM)部件的孔隙率仍然是一项关键挑战。本研究通过比较实验室和同步辐射源的 X 射线测量结果,深入分析了计算机断层扫描(CT)分辨率如何影响激光粉末床熔融(LPBF)制造部件的孔隙率检测。为了代表一定范围的孔隙率水平,我们从大量 LPBF 实验中选取了三个样品,分别为低孔隙率、中孔隙率和高孔隙率。考虑到样品几何形状造成的尺寸限制,我们使用了基于实验室光源的计算机断层扫描系统以最佳分辨率进行采集。为了获得更高的分辨率,还额外使用了同步辐射源。对比分析表明,实验室和同步辐射源对低孔隙度和高孔隙度样品的孔隙度测量结果非常一致。这表明,对于所研究孔隙率频谱的两端,实验室 CT 系统可以提供可靠的测量结果。然而,对于中等孔隙率的样品,由于实验室 CT 的分辨率有限,与同步辐射 CT 的结果相比,高估了样品的孔隙率。研究发现,这种差异是由于在检测和聚类相邻孔隙时存在误差,导致高估了孔隙率。建议将获得的结果与广泛使用的阿基米德方法确定的孔隙率进行比较,以显示每种技术在评估添加制造部件方面的潜力和局限性。
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引用次数: 0
Optimizing µCT resolution in tarsal bones: A comparative study of super-resolution models for trabecular bone analysis 优化跗骨的 µCT 分辨率:用于骨小梁分析的超分辨率模型比较研究
Pub Date : 2025-04-04 DOI: 10.1016/j.tmater.2025.100063
Sascha Senck , Patrick Weinberger , Lukas Nepelius , Andreas Haghofer , Birgit Woegerer , Jonathan Glinz , Miroslav Yosifov , Lukas Behammer , Johann Kastner , Klemens Trieb , Elena Kranioti , Stephan Winkler
Microcomputed tomography (µCT) is an essential tool for analyzing trabecular bone microarchitecture, yet its resolution is constrained by object size and acquisition time. To overcome these limitations, we implement a deep-learning-based super-resolution (SR) approach that enhances µCT image resolution while significantly reducing scan durations. Dry isolated tarsal bones (intermediate cuneiform) from 20 specimens were scanned using µCT at two resolutions, 80 µm voxel size (low resolution, LowRes) and 20 µm voxel size (high resolution, HiRes). Aligned LowRes and HiRes µCT data served as training data for SR reconstruction. In this study, we compare five SR models: 2D U-Net+ +, 3D SRCNN, 3D FSRCNN, 3D U-Net and a modified 3D U-Net model trained with a combined learned perceptual image patch similarity (LPIPS) and structural similarity (SSIM) loss function. The focus of this contribution is the application of these models based on real µCT data, rather than synthetically degraded images. Models were trained to learn volumetric representations for accurate restoration of trabecular bone microstructure. To assess SR image quality, we computed three image quality metrics (peak signal-to-noise ratio, SSIM and LPIPS) and evaluated bone morphometric parameters, i.e. average trabecular thickness (Tb.Th.) and bone volume fraction (BV/TV), across 95 regions of interest (ROI). RMSE was calculated for LowRes data and each SR model relative to HiRes data to quantify prediction accuracy. The results demonstrate that the 3D U-Net (LPIPS & SSIM) model achieves the highest reconstruction accuracy, yielding the lowest RMSE values (12.93 µm for Tb.Th. and 1.3 % for BV/TV), outperforming all other SR models in our evaluation. Compared to standard low-resolution µCT, our approach reduces scan time from 58 min to 7 min per sample while preserving trabecular morphology with high fidelity. These results demonstrate the effectiveness of perceptual loss-based SR to real µCT data for morphological analysis, ensuring accurate trabecular reconstruction and mitigating overestimation artifacts caused by LowRes imaging and partial volume effects. Integrating SR with real µCT scans offers a promising strategy to reduce scan time to improve throughput in bone imaging workflows. Future work will expand the training dataset to enhance model generalization across diverse bone structures and imaging conditions.
微计算机断层扫描(µCT)是分析骨小梁微结构的重要工具,但其分辨率受对象大小和采集时间的限制。为了克服这些限制,我们实现了一种基于深度学习的超分辨率(SR)方法,该方法可以提高微CT图像分辨率,同时显着缩短扫描持续时间。用微CT扫描20个标本的干离体跗骨(中间楔形),两种分辨率分别为80 µm体素大小(低分辨率,LowRes)和20 µm体素大小(高分辨率,HiRes)。对齐的LowRes和HiResµCT数据作为SR重建的训练数据。在这项研究中,我们比较了五种SR模型:2D U-Net+ +,3D SRCNN, 3D FSRCNN, 3D U-Net和一个改进的3D U-Net模型,该模型使用了学习感知图像补丁相似度(LPIPS)和结构相似度(SSIM)损失函数联合训练。这一贡献的重点是基于真实微CT数据的这些模型的应用,而不是综合退化的图像。模型被训练以学习体积表征,以准确地恢复小梁骨微观结构。为了评估SR图像质量,我们计算了三个图像质量指标(峰值信噪比、SSIM和LPIPS),并评估了骨形态测量参数,即95个感兴趣区域(ROI)的平均小梁厚度(Tb.Th.)和骨体积分数(BV/TV)。计算了LowRes数据和每个SR模型相对于HiRes数据的RMSE,以量化预测精度。结果表明,三维U-Net (LPIPS &;SSIM模型的重建精度最高,RMSE值最低(12.93 µm)。BV/TV为1.3 %),在我们的评估中优于所有其他SR模型。与标准的低分辨率微CT相比,我们的方法将每个样品的扫描时间从58 min减少到7 min,同时高保真地保留小梁形态。这些结果证明了基于感知损失的SR对真实微CT数据进行形态学分析的有效性,确保了准确的小梁重建,减轻了由低分辨率成像和部分体积效应引起的高估伪影。将SR与真实的微CT扫描相结合,提供了一种有前途的策略,可以减少扫描时间,提高骨成像工作流程的吞吐量。未来的工作将扩展训练数据集,以增强模型在不同骨骼结构和成像条件下的泛化。
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引用次数: 0
Coupling X-ray µCT, BSE, and QEMSCAN imaging to unravel details of water saturation and oil trapping in a Brazilian Pre-salt carbonate under oil-wet conditions 结合x射线微CT、BSE和QEMSCAN成像,揭示巴西盐下碳酸盐岩含水饱和度和油圈闭的细节
Pub Date : 2025-04-04 DOI: 10.1016/j.tmater.2025.100061
Ronaldo Herlinger Junior , Mark Knackstedt , Benjamin Young , Lydia Knuefing , Alexandre Campane Vidal
The study of fluid saturation and oil entrapment in reservoirs is of great importance for understanding and characterizing multiphase flow, with economically significant implications. In this context, we examine the fluids configuration under oil-wet conditions in particulate carbonate reservoirs of the Brazilian Pre-salt, which host large quantities of oil. Hence, we conducted drainage and imbibition cycles on a grainstone carbonate sample from the Barra Velha Formation of Brazil’s Pre-salt integrating X-ray tomography, backscattered electrons (BSE), and QEMSCAN (quantitative evaluation of minerals by scanning electron microscopy) to understand fluid saturation and oil trapping under oil-wet conditions at pore-scale. The integration of µCT imaging with BSE and QEMSCAN significantly enhances our understanding of fluid saturation within the pore system, particularly in regions where X-ray imaging alone encounters limitations. QEMSCAN imaging, beyond resolving microporosity, provides critical insights into the mineralogical factors influencing fluid distribution, offering a deeper perspective on the saturation controls. Following the drainage and aging cycles, oil effectively displaced nearly all brine within the interparticle macropores, relegating the brine to small, isolated droplets formed through snap-off processes. Additionally, a significant proportion of intraparticle micro and macroporosity was occupied by oil after drainage, with further oil saturation occurring during aging, demonstrating the rock’s oil-wet affinity. Post-forced imbibition imaging revealed that nearly all the oil initially present in the interparticle macropores had been replaced by water, with only minor traces of oil remaining as thin films on mineral surfaces. Conversely, the intraparticle macro and micropores, which are typically less connected, retained most of the oil, highlighting the porous medium’s tendency to trap fluids in poorly connected regions. Finally, our experiments did not reveal any substantial effect of mineralogical variations on fluid saturation during any phase of the cycles. This suggests that the observed oil-wet condition is independent of relative mineralogical variations, particularly given the sample's dominance of calcite and dolomite. These results, although obtained from a facies type common in the Brazilian Pre-salt, elucidate the behavior in oil-wettable reservoirs, a common condition in various reservoirs around the world.
储层中流体饱和度和油的圈闭研究对于认识和表征多相流具有重要意义,具有重要的经济意义。在这种情况下,我们研究了巴西盐下颗粒碳酸盐储层的流体结构,这些储层含有大量的石油。因此,我们对巴西Barra Velha组的粒岩碳酸盐样品进行了排水和渗吸循环,结合x射线断层扫描、背散射电子(BSE)和QEMSCAN(通过扫描电子显微镜对矿物进行定量评价),以了解孔隙尺度下油湿条件下的流体饱和度和油捕获。微CT成像与BSE和QEMSCAN的集成显著增强了我们对孔隙系统内流体饱和度的理解,特别是在单独x射线成像受到限制的区域。QEMSCAN成像,除了解析微孔隙度之外,还提供了对影响流体分布的矿物学因素的重要见解,为饱和度控制提供了更深入的视角。在排水和老化循环之后,油有效地取代了颗粒间大孔隙中的几乎所有卤水,将卤水分解成通过断裂过程形成的小而孤立的液滴。此外,疏水后颗粒内微孔和宏观孔隙中有很大一部分被油占据,在老化过程中进一步发生油饱和,表明岩石具有亲油性。后强迫渗吸成像显示,几乎所有最初存在于颗粒间大孔隙中的油都被水所取代,只有少量油残留在矿物表面的薄膜上。相反,颗粒内的宏观和微孔通常连通性较差,保留了大部分石油,这表明多孔介质倾向于在连通性差的区域捕获流体。最后,我们的实验没有发现在旋回的任何阶段,矿物学变化对流体饱和度的任何实质性影响。这表明观察到的油湿条件与相对矿物学变化无关,特别是考虑到样品中方解石和白云石的优势。虽然这些结果是巴西盐下油藏中常见的一种相类型,但它们阐明了可湿油油藏的行为,这是世界上各种油藏的共同情况。
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引用次数: 0
A review of in-situ mechanical testing combined with X-ray microfocus computed tomography: Application and current challenges for biological tissues 结合x射线微聚焦计算机断层扫描的原位力学测试综述:生物组织的应用和当前挑战
Pub Date : 2025-04-03 DOI: 10.1016/j.tmater.2025.100062
Lara Mazy , Greet Kerckhofs
Biological tissues undergo physiological mechanical loading during their functioning in vivo. To properly respond to these mechanical signals, tissues have a highly complex microstructural organization. However, there is not yet sufficient knowledge about the link between their microstructural organization and their mechanical behaviour. Therefore, there is a need for methods to dynamically assess how the microstructure of biological tissues changes during mechanical loading. 4D-µCT is an imaging technique combining mechanical testing with X-ray microfocus computed tomography (µCT) imaging. It has been extensively used to visualize, at the micro-scale and in full 3D, the deformation of the microstructure of non-biological materials during mechanical loading. Additionally, postprocessing of the 4D-µCT datasets allowed 3D strain field calculations. This review aims to provide an overview of the current state of the art of the use of 4D-µCT specifically for the assessment of the mechanical behavior of biological tissue, and this both for mineralized and unmineralized tissues. We highlighted the advancements as well as the current limitations and challenges to overcome, such as the need for complex loading modes, the effect of X-rays on the mechanical behavior and the need to keep the samples hydrated during testing. We finally conclude with some future perspectives.
生物组织在体内运作时会承受生理机械负荷。为了正确响应这些机械信号,组织具有高度复杂的微结构组织。然而,人们对其微观结构组织与其机械行为之间的联系还缺乏足够的了解。因此,需要采用一些方法来动态评估生物组织的微观结构在机械加载过程中是如何变化的。4D-µCT 是一种将机械测试与 X 射线微焦计算机断层扫描(µCT)成像相结合的成像技术。它已被广泛用于在微观尺度上以全三维方式观察非生物材料在机械加载过程中微观结构的变形。此外,通过对 4D-µCT 数据集进行后处理,还可进行三维应变场计算。本综述旨在概述目前使用 4D-µCT 评估生物组织机械行为的最新技术,包括矿化组织和非矿化组织。我们重点介绍了所取得的进展以及目前需要克服的局限性和挑战,如需要复杂的加载模式、X 射线对力学行为的影响以及在测试过程中保持样本水合状态的必要性。最后,我们对未来进行了展望。
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Tomography of Materials and Structures
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