Pub Date : 2025-06-08DOI: 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.
{"title":"Comparison of three measurement modalities for 3D characterization of manufactured features and process-induced porosity in titanium alloy additively manufactured parts","authors":"Andrew Townsend , Chen Yee , Bryce Jolley , Nikola Draganic , Michael Chapman , Daniel Sparkman , Michael D. Uchic","doi":"10.1016/j.tmater.2025.100070","DOIUrl":"10.1016/j.tmater.2025.100070","url":null,"abstract":"<div><div>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.</div></div>","PeriodicalId":101254,"journal":{"name":"Tomography of Materials and Structures","volume":"9 ","pages":"Article 100070"},"PeriodicalIF":0.0,"publicationDate":"2025-06-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144306752","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-06-06DOI: 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.
{"title":"Correlative X-ray and electron tomography for scale-bridging, quantitative analysis of complex, hierarchical particle systems","authors":"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","doi":"10.1016/j.tmater.2025.100069","DOIUrl":"10.1016/j.tmater.2025.100069","url":null,"abstract":"<div><div>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.</div></div>","PeriodicalId":101254,"journal":{"name":"Tomography of Materials and Structures","volume":"9 ","pages":"Article 100069"},"PeriodicalIF":0.0,"publicationDate":"2025-06-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144298110","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-05-14DOI: 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.
{"title":"Improving electron tomography of mesoporous silica by Ga intrusion","authors":"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","doi":"10.1016/j.tmater.2025.100068","DOIUrl":"10.1016/j.tmater.2025.100068","url":null,"abstract":"<div><div>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.</div></div>","PeriodicalId":101254,"journal":{"name":"Tomography of Materials and Structures","volume":"8 ","pages":"Article 100068"},"PeriodicalIF":0.0,"publicationDate":"2025-05-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144072276","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-04-26DOI: 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.
{"title":"Single-particle geometries of pharmaceutical powders from X-ray tomography; a simple and reliable sample preparation method","authors":"Dingeman L.H. van der Haven , Jan L. Andreasen , Umair Zafar , Ioannis S. Fragkopoulos , James A. Elliott","doi":"10.1016/j.tmater.2025.100067","DOIUrl":"10.1016/j.tmater.2025.100067","url":null,"abstract":"<div><div>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.</div></div>","PeriodicalId":101254,"journal":{"name":"Tomography of Materials and Structures","volume":"8 ","pages":"Article 100067"},"PeriodicalIF":0.0,"publicationDate":"2025-04-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143892256","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-04-13DOI: 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.
{"title":"Individual component-based parameter-adaptive segmentation approach for improved segmentation of synchrotron µCT data of osteocyte lacunae in bone tissue","authors":"Jan Mölich , Sophie Anuth , Jussi-Petteri Suuronen , Emely Bortel , Javier Gerber , Enni Mattern , Timm Weitkamp , Katja Nelson , Susanne Nahles , Bernhard Hesse","doi":"10.1016/j.tmater.2025.100066","DOIUrl":"10.1016/j.tmater.2025.100066","url":null,"abstract":"<div><div>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.</div></div>","PeriodicalId":101254,"journal":{"name":"Tomography of Materials and Structures","volume":"8 ","pages":"Article 100066"},"PeriodicalIF":0.0,"publicationDate":"2025-04-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143847897","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-04-11DOI: 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.
{"title":"Measuring thermal curing induced shrinkage of material extrusion based additive manufacturing silicone elastomer lattices by X-ray computed tomography","authors":"Massimiliano Ferrucci , Anne-Françoise Obaton , Robert Cerda , Brian Au , Nicholas Rodriguez , Ziad Ammar , Gabriel Balensiefer , Chuck Divin , Jeremy Lenhardt , Brian Giera","doi":"10.1016/j.tmater.2025.100064","DOIUrl":"10.1016/j.tmater.2025.100064","url":null,"abstract":"<div><div>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.</div></div>","PeriodicalId":101254,"journal":{"name":"Tomography of Materials and Structures","volume":"8 ","pages":"Article 100064"},"PeriodicalIF":0.0,"publicationDate":"2025-04-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143820724","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-04-08DOI: 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.
{"title":"In-depth analysis of CT resolution impact on porosity evaluation in laser powder bed fusion additive manufacturing","authors":"Jitendra Singh Rathore , Andrew King , Florian Le Bourdais , Jean-Paul Garandet","doi":"10.1016/j.tmater.2025.100065","DOIUrl":"10.1016/j.tmater.2025.100065","url":null,"abstract":"<div><div>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.</div></div>","PeriodicalId":101254,"journal":{"name":"Tomography of Materials and Structures","volume":"8 ","pages":"Article 100065"},"PeriodicalIF":0.0,"publicationDate":"2025-04-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143817483","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-04-04DOI: 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。
{"title":"Optimizing µCT resolution in tarsal bones: A comparative study of super-resolution models for trabecular bone analysis","authors":"Sascha Senck , Patrick Weinberger , Lukas Nepelius , Andreas Haghofer , Birgit Woegerer , Jonathan Glinz , Miroslav Yosifov , Lukas Behammer , Johann Kastner , Klemens Trieb , Elena Kranioti , Stephan Winkler","doi":"10.1016/j.tmater.2025.100063","DOIUrl":"10.1016/j.tmater.2025.100063","url":null,"abstract":"<div><div>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.</div></div>","PeriodicalId":101254,"journal":{"name":"Tomography of Materials and Structures","volume":"8 ","pages":"Article 100063"},"PeriodicalIF":0.0,"publicationDate":"2025-04-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143817482","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-04-04DOI: 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.
{"title":"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","authors":"Ronaldo Herlinger Junior , Mark Knackstedt , Benjamin Young , Lydia Knuefing , Alexandre Campane Vidal","doi":"10.1016/j.tmater.2025.100061","DOIUrl":"10.1016/j.tmater.2025.100061","url":null,"abstract":"<div><div>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.</div></div>","PeriodicalId":101254,"journal":{"name":"Tomography of Materials and Structures","volume":"8 ","pages":"Article 100061"},"PeriodicalIF":0.0,"publicationDate":"2025-04-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143785785","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-04-03DOI: 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。
{"title":"A review of in-situ mechanical testing combined with X-ray microfocus computed tomography: Application and current challenges for biological tissues","authors":"Lara Mazy , Greet Kerckhofs","doi":"10.1016/j.tmater.2025.100062","DOIUrl":"10.1016/j.tmater.2025.100062","url":null,"abstract":"<div><div>Biological tissues undergo physiological mechanical loading during their functioning <em>in vivo</em>. 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.</div></div>","PeriodicalId":101254,"journal":{"name":"Tomography of Materials and Structures","volume":"8 ","pages":"Article 100062"},"PeriodicalIF":0.0,"publicationDate":"2025-04-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143820723","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}