Search Results (19)

This review considers the use of fractal concepts to improve the development, fabrication, and characterisation of catalytic materials and supports. First, the theory of fractals is discussed, as well as how it can be used to better describe often highly complex catalytic materials and enhance structural characterisation via a variety of different methods, including gas sorption, mercury porosimetry, NMR, and several imaging modalities. The review then surveys various synthesis and fabrication methods that can be used to create catalytic materials that are fractals or possess fractal character. It then goes on to consider how the fractal properties of catalysts affect their performance, especially their overall activity, selectivity for desired products, and resistance to deactivation. Finally, this review describes how the optimum fractal catalyst material for a given reaction system can be designed on a computer. Full article

Over the years, FIB-SEM tomography has become an extremely important technique for the three-dimensional reconstruction of microscopic structures with nanometric resolution. This paper describes in detail the steps required to perform this analysis, from the experimental setup to the data analysis and final reconstruction. To demonstrate the versatility of the technique, a comprehensive list of applications is also summarized, ranging from batteries to shale rocks and even some types of soft materials. Moreover, the continuous technological development, such as the introduction of the latest models of plasma and cryo-FIB, can open the way towards the analysis with this technique of a large class of soft materials, while the introduction of new machine learning and deep learning systems will not only improve the resolution and the quality of the final data, but also expand the degree of automation and efficiency in the dataset handling. These future developments, combined with a technique that is already reliable and widely used in various fields of research, are certain to become a routine tool in electron microscopy and material characterization. Full article

The specific surface area is an important parameter to characterize pore structure and adsorption properties, however, it is difficult to calculate accurately in shale rock due to its multiscale pore structure. In this paper, the representative 3D gray images of a microfracture sample, micropore subsample and nanopore subsample in shale rock were obtained with computed tomography (CT) scanning and focused ion beam-scanning electron microscopy (FIB-SEM) scanning. The multi-threshold segmentation algorithm with improved maximum inter-class variance method was introduced to construct the platform of multi-scale digital rock. Then, based on the fracture, micropore and nanopore digital rocks, the corresponding network models were extracted to obtain different-scale pore structures, respectively. Finally, based on the digital rock at different scales, the corresponding pore percentage, matrix percentage and specific surface area were calculated respectively. It was found that the specific surface areas of both microfractures and micropores are small, and their specific surface areas are 2~3 orders of magnitude smaller than that of nanopores, and the specific surface area of the shale formation is mainly contributed by nanopores. This paper provides an effective method to calculate the multi-scale specific surface area accurately in shale rock and has an important influence on the adsorption characteristics and swelling properties of the shale matrix. Full article

In shale oil reservoirs, nano-scale pores and micro-scale fractures serve as the primary fluid storage and migration space, while the associated flow mechanism remains vague and is hard to understand. In this research, a three-dimensional (3D) reconstruction of the shale core and micro-pore structure description technique is established; digital core technology for shale reservoirs was developed using X-ray computed tomography (X-CT), scanning electron microscope (SEM) and a focused ion beam scanning electron microscope (FIB-SEM). Microscopic oil–water two-phase flow is mimicked using the lattice Boltzmann method (LBM), a well-acknowledged approach to exploring nanoconfined fluid dynamics. In addition, coupled with digital cores, the flow characteristics of shale reservoirs are characterized. The total porosities of bedding fractures in shale and lamellar shale are 2.042% and 1.085%, respectively. The single-phase oil flow inside bedding fractures follows Darcy’s linear flow principle. This work can deepen the understanding of the microscopic flow characteristics of continental shale reservoirs and provide a reference for similar problems that may be encountered. Full article

Planktonic freshwater filamentous cyanobacterium Trichormus variabilis ATCC 29413 (previously known as Anabaena variabilis) can differentiate heterocysts and akinetes to survive under different stress conditions. Whilst heterocysts enable diazotrophic growth, akinetes are spore-like resting cells that make the survival of the species possible under adverse growth conditions. Under suitable environmental conditions, they germinate to produce new vegetative filaments. Several morphological and physiological changes occur during akinete formation and germination. Here, using scanning electron microscopy (SEM), we found that the mature akinetes had a wrinkled envelope, and the surface of the envelope smoothened as the cell size increased during germination. Thereupon, the akinete envelope ruptured to release the short emerging filament. Focused ion beam–scanning electron microscopy (FIB/SEM) tomography of immature akinetes revealed the presence of cytoplasmic granules, presumably consisting of cyanophycin or glycogen. In addition, the akinete envelope architecture of different layers, the exopolysaccharide and glycolipid layers, could be visualized. We found that this multilayered envelope helped to withstand osmotic stress and to maintain the structural integrity. Furthermore, by fluorescence recovery after photobleaching (FRAP) measurements, using the fluorescent tracer calcein, we found that intercellular communication decreased during akinete formation as compared with the vegetative cells. In contrast, freshly germinating filaments restored cell communication. Full article

Shale reservoir heterogeneity is strong, which seriously affects shale gas reservoir evaluation and reserves estimation. The Longmaxi Formation shale of the Luzhou block in southern Sichuan was taken as an example to characterize the pore distribution of shale over the full scale using micro-computed tomography (CT), focusing on ion beam scanning electron microscopy (FIB-SEM) and small-angle neutron scattering (SANS); further, the heterogeneity of the shale pore distribution over the full scale was explored quantitatively within different scales. The results show that shale micropores are dominated by microfractures that are mainly developed along the bedding direction and associated with organic matter, contributing 1.24% of porosity. Shale nanopores are more developed, contributing 3.57–4.72% porosity and have strong heterogeneity locally at the microscale, but the pore distribution characteristics show lateral homogeneity and vertical heterogeneity at the macroscale. In the same layer, the porosity difference is only 0.1% for the sheet samples with 2 cm adjacent to each other. Therefore, in shale core experiments in which parallel samples are needed for comparison, parallel samples should be in the same bedding position. This paper explores the extent of heterogeneity over the full scale of pore distribution from macro to micro, which has important significance for accurately characterizing the pore distribution of shale and further carrying out reservoir evaluation and estimation of reserves. Full article

The ATI 718Plus^® is a creep-resistant nickel-based superalloy exhibiting high strength and excellent oxidation resistance in high temperatures. The present study is focused on multiscale 2D and 3D characterization (morphological and chemical) of the scale and the layer beneath formed on the ATI 718Plus superalloy during oxidation at 850 °C up to 4000 h in dry and wet air. The oxidized samples were characterized using various microscopic methods (SEM, TEM and STEM), energy-dispersive X-ray spectroscopy and electron diffraction. The 3D visualization of the microstructural features was achieved by means of FIB-SEM tomography. When oxidized in dry air, the ATI 718Plus develops a protective, dense Cr₂O₃ scale with a dual-layered structure. The outer Cr₂O₃ layer is composed of coarser grains with a columnar shape, while the inner one features fine, equiaxed grains. The Cr₂O₃ scale formed in wet air is single-layered and features very fine grains. The article discusses the difference between the structure, chemistry and three-dimensional phase distribution of the oxide scales and near-surface areas developed in the two environments. Electron microscopy/spectroscopy findings combined with the three-dimensional reconstruction of the microstructure provide original insight into the role of the oxidation environment on the structure of the ATI 718Plus at the nanoscale. Full article

The microstructure of alkali-reactive aggregates, especially the spatial distribution of the pore and reactive silica phase, plays a significant role in the process of the alkali silica reaction (ASR) in concrete, as it determines not only the reaction front of ASR but also the localization of the produced expansive product from where the cracking begins. However, the microstructure of the aggregate was either simplified or neglected in the current ASR simulation models. Due to the various particle sizes and heterogeneous distribution of the reactive silica in the aggregate, it is difficult to obtain a representative microstructure at a desired voxel size by using non-destructive computed tomography (CT) or focused ion beam milling combined with scanning electron microscopy (FIB-SEM). In order to fill this gap, this paper proposed a model that simulates the microstructures of the alkali-reactive aggregate based on 2D images. Five representative 3D microstructures with different pore and quartz fractions were simulated from SEM images. The simulated fraction, scattering density, as well as the autocorrelation function (ACF) of pore and quartz agreed well with the original ones. A $40\times 40\times 40$ mm${}^3$ concrete cube with irregular coarse aggregates was then simulated with the aggregate assembled by the five representative microstructures. The average pore (at microscale $\mathsf{\mu }$m) and quartz fractions of the cube matched well with the X-ray diffraction (XRD) and Mercury intrusion porosimetry (MIP) results. The simulated microstructures can be used as a basis for simulation of the chemical reaction of ASR at a microscale. Full article

Segmentation of images from scanning electron microscope, especially multiphase, poses a drawback in their microstructure quantification process. The labeling process must be automatized due to the time consumption and irreproducibility of the manual labeling procedure. Here we show a swarm intelligence-driven filtration methodology performed on raw solid oxide fuel cell anode’s material images to improve the segmentation methods’ performance. The methodology focused on two significant parts of the segmentation process, which are filtering and labeling. During the first one, the images underwent filtering by applying a series of filters, whose operation parameters were determined using Particle Swarm Optimization upon a dedicated cost function. Next, Seeded Region Growing, k-Means Clustering, Multithresholding, and Simple Linear Iterative Clustering Superpixel algorithms were utilized to label the filtered images’ regions into consecutive phases in the microstructure. The improvement was presented for three different metrics: the Misclassification Ratio, Structural Similarity Index Measure, and Mean Squared Error. The obtained distribution of metrics’ performances was based on 200 images, with and without filtering. Results indicate an improvement up to 29%, depending on the metric and method used. The presented work contributes to the ongoing efforts to automatize segmentation processes fully for an increasing number of tomographic measurements, particularly in solid oxide fuel cell research. Full article

Focused Ion Beam Scanning Electron Microscopy (FIB-SEM) tomography provides a stack of images that represent serial slices of the sample. These images are displaced relatively to each other, and an alignment procedure is required. Traditional methods for alignment of a 3D image are based on a comparison of two adjacent slices. However, such algorithms are easily confused by anisotropy in the sample structure or even experiment geometry in the case of porous media. This may lead to significant distortions in the pore space geometry, if there are no stable fiducial marks in the frame. In this paper, we propose a new method, which meaningfully extends existing alignment procedures. Our technique allows the correction of random misalignments between slices and, at the same time, preserves the overall geometrical structure of the specimen. We consider displacements produced by existing alignment algorithms as a signal and decompose it into low and high-frequency components. Final transformations exclude slow variations and contain only high frequency variations that represent random shifts that need to be corrected. The proposed algorithm can operate with not only translations but also with arbitrary affine transformations. We demonstrate the performance of our approach on a synthetic dataset and two real FIB-SEM images of natural rock. Full article

Evolution of additively manufactured (AM) ceramics’ microstructure between manufacturing stages is a hardly explored topic. These data are of high demand for advanced numerical modeling. In this work, 3D microstructural models of Al₂O₃ greenbody, brownbody and sintered material are presented and analyzed, for ceramic samples manufactured with SLA-based AM workflow, using a commercially available ceramic paste and 3D printer. The novel data, acquired at the micro- and mesoscale, using Computed Tomography (CT), Scanning Electron Microscopy (SEM) and Focused Ion-Beam SEM (FIB/SEM) techniques, allowed a deep insight into additive ceramics characteristics. We demonstrated the spatial 3D distribution of ceramic particles, an organic binder and pores at every stage of AM workflow. The porosity of greenbody samples (1.6%), brownbody samples (37.3%) and sintered material (4.9%) are analyzed. Pore distribution and possible originating mechanisms are discussed. The location and shape of pores and ceramic particles are indicative of specific physical processes driving the ceramics manufacturing. We will use the presented microstructural 3D models as input and verification data for advanced numerical simulations developed in the project. Full article

For parenteral controlled drug release, the desired zero order release profile with no lag time is often difficult to achieve. To overcome the undesired lag time of the current commercial risperidone controlled release formulation, we developed PLGA–lipid microcapsules (MCs) and PLGA–lipid microgels (MGs). The lipid phase was composed of middle chain triglycerides (MCT) or isopropylmyristate (IPM). Hydroxystearic acid was used as an oleogelator. The three-dimensional inner structure of Risperidone-loaded MCs and MGs was assessed by using the invasive method of electron microscopy with focused ion beam cutting (FIB-SEM) and the noninvasive method of high-resolution nanoscale X-ray computed tomography (nano-CT). FIB-SEM and nano-CT measurements revealed the presence of highly dispersed spherical structures around two micrometres in size. Drug release kinetics did strongly depend on the used lipid phase and the presence or absence of hydroxystearic acid. We achieved a nearly zero order release without a lag time over 60 days with the MC-MCT formulation. In conclusion, the developed lipid-PLGA microparticles are attractive alternatives to pure PLGA-based particles. The advantages include improved release profiles, which can be easily tuned by the lipid composition. Full article

In this research, a fully three-dimensional, multiphase, microstructure-scale heterogeneous (non-continuous) electrode, Solid Oxide Fuel Cell (SOFC) stack model is implemented in order to assess the impact of homogeneity disturbance in an SOFC anode. The Butler–Volmer model is combined with recent empirical relations for conductivity and aspects of the Maxwell–Boltzmann kinetic theory describing the transport of mass within the porous medium. Methods for the localized quantification of electrode morphology parameters (such as triple phase boundary length) are implemented. The exchange current distribution in the electrode, the partial pressures and the electric potential fields for each phase are computed numerically. In order to simulate heterogeneity, transfer barriers of varying placement and size are added to an otherwise homogeneous, virtual microstructure based on data from FIB-SEM tomography. The results are compared to a model based on the continuous electrode theory, and the points of discrepancy are highlighted. Full article

Biomaterial for tissue engineering is a topic of huge progress with a recent surge in fabrication and characterization advances. Biomaterials for tissue engineering applications or as scaffolds depend on various parameters such as fabrication technology, porosity, pore size, mechanical strength, and surface available for cell attachment. To serve the function of the scaffold, the porous biomaterial should have enough mechanical strength to aid in tissue engineering. With a new manufacturing technology, we have obtained high strength materials by optimizing a few processing parameters such as pressure, temperature, and dwell time, yielding the monolith with porosity in the range of 80%–93%. The three-dimensional interconnectivity of the porous media through scales for the newly manufactured biomaterial has been investigated using newly developed 3D correlative and multi-modal imaging techniques. Multiscale X-ray tomography, FIB-SEM Slice & View stacking, and high-resolution STEM-EDS electronic tomography observations have been combined allowing quantification of morphological and geometrical spatial distributions of the multiscale porous network through length scales spanning from tens of microns to less than a nanometer. The spatial distribution of the wall thickness has also been investigated and its possible relationship with pore connectivity and size distribution has been studied. Full article

Peritubular dentine (PTD) and intertubular dentine (ITD) were investigated by 3D correlative Focused Ion Beam (FIB)-Scanning Electron Microscopy (SEM)-Energy Dispersive Spectroscopy (EDS) tomography, tapping mode Atomic Force Microscopy (AFM) and scattering-type Scanning Near-Field Optical Microscopy (s-SNOM) mapping. The brighter appearance of PTD in 3D SEM-Backscattered-Electron (BSE) imaging mode and the corresponding higher grey value indicate a greater mineral concentration in PTD (~160) compared to ITD (~152). However, the 3D FIB-SEM-EDS reconstruction and high resolution, quantitative 2D map of the Ca/P ratio (~1.8) fail to distinguish between PTD and ITD. This has been further confirmed using nanoscale 2D AFM map, which clearly visualised biopolymers and hydroxyapatite (HAp) crystallites with larger mean crystallite size in ITD (32 ± 8 nm) than that in PTD (22 ± 3 nm). Correlative microscopy reveals that the principal difference between PTD and ITD arises primarily from the nanoscale packing density of the crystallites bonded together by thin biopolymer, with moderate contribution from the chemical composition difference. The structural difference results in the mechanical properties variation that is described by the parabolic stiffness-volume fraction correlation function introduced here. The obtained results benefit a microstructure-based mechano-chemical model to simulate the chemical etching process that can occur in human dental caries and some of its treatments. Full article