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1.
The combination of in-situ and three-dimensional (3D) in transmission electron microscopy (TEM) is one of the emerging topics of recent advanced electron microscopy research. However, to date, there have been only handful examples of in-situ 3D TEM for material deformation dynamics. In this article, firstly, the authors briefly review technical developments in fast tilt-series dataset acquisition, which is a crucial technique for in-situ electron tomography (ET). Secondly, the authors showcase a recent successful example of in-situ specimen-straining and ET system development and its applications to the deformation dynamics of crystalline materials. The system is designed and developed to explore, in real-time and at sub-microscopic levels, the internal behavior of polycrystalline materials subjected to external stresses, and not specifically targeted for atomic resolution (although it may be possible). Technical challenges toward the in-situ ET observation of 3D dislocation dynamics are discussed for commercial structural crystalline materials, including some of the early studies on in-situ ET imaging and 3D modeling of dislocation dynamics. A short summary of standing technical issues and a proposed guideline for further development in the 3D imaging method for dislocation dynamics are then discussed.  相似文献   

2.
X-ray tomography is a versatile tool in materials research and engineering since it allows for a non-destructive and three-dimensional mapping of the constituents of a heterogeneous material as long as they differ in their interactions with X-rays. Recent developments of the technique have brought down the time needed for the acquisition of a single tomogram by many orders of magnitude compared to what was needed 25 years ago. Nowadays, up to 1000 full tomograms can be recorded in a second, which enables real-time studies of changes in samples caused by reactions or by applied processing operations. The term tomoscopy has been coined for such sequences of 3D images. We review the application of X-ray tomography and tomoscopy on metals and describe each step required and the associated challenges. A selection of representative investigations is presented with a focus on time-resolved phenomena in metals and alloys ranging from mechanical deformation, solidification to metals processing processes such as welding and additive manufacturing. Finally likely future developments are discussed.  相似文献   

3.
Innovations in nanofabrication have expedited advances in hollow‐structured nanomaterials with increasing complexity, which, at the same time, set challenges for the precise determination of their intriguing and complicated 3D configurations. Conventional transmission electron microscopy (TEM) analysis typically yields 2D projections of 3D objects, which in some cases is insufficient to reflect the genuine architectures of these 3D nano‐objects, providing misleading information. Advanced analytical approaches such as focused ion beam (FIB) and ultramicrotomy enable the real slicing of nanomaterials, realizing the direct observation of inner structures but with limited spatial discrimination. Electron tomography (ET) is a technique that retrieves spatial information from a series of 2D electron projections at different tilt angles. As a unique and powerful tool kit, this technique has experienced great advances in its application in materials science, resolving the intricate 3D nanostructures. Here, the exceptional capability of the ET technique in the structural, chemical, and quantitative analysis of hollow‐structured nanomaterials is discussed in detail. The distinct information derived from ET analysis is highlighted and compared with conventional analysis methods. Along with the advances in microscopy technologies, the state‐of‐the‐art ET technique offers great opportunities and promise in the development of hollow nanomaterials.  相似文献   

4.
This review summarizes the recent advances in electron tomography (ET) and its application to polymer nanostructures. Truly quantitative three-dimensional (3D) images of polymer nanostructures can now be obtained by reducing or eliminating the missing tilt range in ET experiments. The reduction of the resulting missing wedge provides sub-nanometer resolution, which is sufficiently small for soft materials. Because soft materials often exhibit hierarchical structures, observation of a large volume with edges several micrometers in length is important to capture the structural elements on a scale larger than tens of nanometers. The introduction of scanning optics to ET has made it possible to obtain 3D data from micrometer-thick polymer specimens by using conventional electron microscopes at a relatively low accelerating voltage of 200 kV. We present some examples of the structural analysis of soft materials, such as nanostructures of self-assembled block copolymers and fuel cell electrodes.  相似文献   

5.
Three-dimensional (3D) imaging has a significant impact on many challenges of life sciences. Three-dimensional matrix-assisted laser desorption/ionization imaging mass spectrometry (MALDI-IMS) is an emerging label-free bioanalytical technique capturing the spatial distribution of hundreds of molecular compounds in 3D by providing a MALDI mass spectrum for each spatial point of a 3D sample. Currently, 3D MALDI-IMS cannot tap its full potential due to the lack efficient computational methods for constructing, processing, and visualizing large and complex 3D MALDI-IMS data. We present a new pipeline of efficient computational methods, which enables analysis and interpretation of a 3D MALDI-IMS data set. Construction of a MALDI-IMS data set was done according to the state-of-the-art protocols and involved sample preparation, spectra acquisition, spectra preprocessing, and registration of serial sections. For analysis and interpretation of 3D MALDI-IMS data, we applied the spatial segmentation approach which is well-accepted in analysis of two-dimensional (2D) MALDI-IMS data. In line with 2D data analysis, we used edge-preserving 3D image denoising prior to segmentation to reduce strong and chaotic spectrum-to-spectrum variation. For segmentation, we used an efficient clustering method, called bisecting k-means, which is optimized for hierarchical clustering of a large 3D MALDI-IMS data set. Using the proposed pipeline, we analyzed a central part of a mouse kidney using 33 serial sections of 3.5 μm thickness after the PAXgene tissue fixation and paraffin embedding. For each serial section, a 2D MALDI-IMS data set was acquired following the standard protocols with the high spatial resolution of 50 μm. Altogether, 512?495 mass spectra were acquired that corresponds to approximately 50 gigabytes of data. After registration of serial sections into a 3D data set, our computational pipeline allowed us to reveal the 3D kidney anatomical structure based on mass spectrometry data only. Finally, automated analysis discovered molecular masses colocalized with major anatomical regions. In the same way, the proposed pipeline can be used for analysis and interpretation of any 3D MALDI-IMS data set in particular of pathological cases.  相似文献   

6.
The integration of nanotechnology into three‐dimensional printing (3DP) offers huge potential and opportunities for the manufacturing of 3D engineered materials exhibiting optimized properties and multifunctionality. The literature relating to different 3DP techniques used to fabricate 3D structures at the macro‐ and microscale made of nanocomposite materials is reviewed here. The current state‐of‐the‐art fabrication methods, their main characteristics (e.g., resolutions, advantages, limitations), the process parameters, and materials requirements are discussed. A comprehensive review is carried out on the use of metal‐ and carbon‐based nanomaterials incorporated into polymers or hydrogels for the manufacturing of 3D structures, mostly at the microscale, using different 3D‐printing techniques. Several methods, including but not limited to micro‐stereolithography, extrusion‐based direct‐write technologies, inkjet‐printing techniques, and popular powder‐bed technology, are discussed. Various examples of 3D nanocomposite macro‐ and microstructures manufactured using different 3D‐printing technologies for a wide range of domains such as microelectromechanical systems (MEMS), lab‐on‐a‐chip, microfluidics, engineered materials and composites, microelectronics, tissue engineering, and biosystems are reviewed. Parallel advances on materials and techniques are still required in order to employ the full potential of 3D printing of multifunctional nanocomposites.  相似文献   

7.
In this paper, we apply electron tomography (ET) to the study of the three-dimensional (3D) morphology of iron oxide nanoparticles (NPs) with reactive concave surfaces. The ability to determine quantitatively the volume and shape of the NP concavity is essential for understanding the key-lock mechanism responsible for the destabilization of gold nanocrystals within the iron oxide NP concavity. We show that quantitative ET is enhanced greatly by the application of compressed sensing (CS) techniques to the tomographic reconstruction. High-fidelity tomograms using a new CS-ET algorithm reveal with clarity the concavities of the particle and enable 3D nanometrology studies to be undertaken with confidence. In addition, the robust performance of the CS-ET algorithm with undersampled data should allow rapid progress with time-resolved 3D nanoscale studies, 3D atomic resolution imaging, and cryo-tomography of nanoscale cellular structures.  相似文献   

8.
The structure of crystalline materials is typically organised hierarchically on several length scales. Hard x-ray microscopy is presented as a collection of modalities that allows to zoom into a mm-sized sample to acquire 3D maps of any embedded region and at essentially all relevant length scales. For coarse mapping of grains, their orientations and average stress state diffraction based tomography methods can sample thousands of grains with a resolution of 2 µm. At the 100 nm scale, domains and dislocations and their associated strain fields can be visualised by diffraction microscopy. Similar to dark field electron microscopy, diffraction and imaging can be combined in several ways. For the ultimate resolution, a bulk version of coherent diffraction imaging is introduced. Hard x-ray microscopy is optimised for acquisition of 3D movies: directly visualising the structural changes during nucleation and growth, deformation or damage. The state of art is provided along with examples of use. I discuss how hard x-ray microscopy studies can enable the formulation and validation of improved multiscale models that account for the entire heterogeneity of materials.  相似文献   

9.
The fabrication and integration of low-resistance carbon nanotubes (CNTs) for interconnects in future integrated circuits requires characterization techniques providing structural and electrical information at the nanometer scale. In this paper we present a slice-and-view approach based on electrical atomic force microscopy. Material removal achieved by successive scanning using doped ultra-sharp full-diamond probes, manufactured in-house, enables us to acquire two-dimensional (2D) resistance maps originating from different depths (equivalently different CNT lengths) on CNT-based interconnects. Stacking and interpolating these 2D resistance maps results in a three-dimensional (3D) representation (tomogram). This allows insight from a structural (e.g.?size, density, distribution, straightness) and electrical point of view simultaneously. By extracting the resistance evolution over the length of an individual CNT we derive quantitative information about the resistivity and the contact resistance between the CNT and bottom electrode.  相似文献   

10.
The creation of three‐dimensional (3D) structures from two‐dimensional (2D) nanomaterial building blocks enables novel chemical, mechanical or physical functionalities that cannot be realized with planar thin films or in bulk materials. Here, we review the use of emerging 2D materials to create complex out‐of‐plane surface topographies and 3D material architectures. We focus on recent approaches that yield periodic textures or patterns, and present four techniques as case studies: (i) wrinkling and crumpling of planar sheets, (ii) encapsulation by crumpled nanosheet shells, (iii) origami folding and kirigami cutting to create programmed curvature, and (iv) 3D printing of 2D material suspensions. Work to date in this field has primarily used graphene and graphene oxide as the 2D building blocks, and we consider how these unconventional approaches may be extended to alternative 2D materials and their heterostructures. Taken together, these emerging patterning and texturing techniques represent an intriguing alternative to conventional materials synthesis and processing methods, and are expected to contribute to the development of new composites, stretchable electronics, energy storage devices, chemical barriers, and biomaterials.  相似文献   

11.
Deterministic transformations of 2D patterns of materials into well-controlled 3D mesostructures serve as the basis for manufacturing methods that can bypass limitations of conventional 3D micro/nanofabrication. Here, guided mechanical buckling processes provide access to a rich range of complex 3D mesostructures in high-performance materials, from inorganic and organic semiconductors, metals and dielectrics, to ceramics and even 2D materials (e.g., graphene, MoS2). Previous studies demonstrate that iterative computational procedures can define design parameters for certain targeted 3D configurations, but without the ability to address complex shapes. A technical need is in efficient, generalized inverse design algorithms that directly yield sets of optimized parameters. Here, such schemes are introduced, where the distributions of thicknesses across arrays of separated or interconnected ribbons provide scalable routes to 3D surfaces with a broad range of targeted shapes. Specifically, discretizing desired shapes into 2D ribbon components allows for analytic solutions to the inverse design of centrally symmetric and even general surfaces, in an approximate manner. Combined theoretical, numerical, and experimental studies of ≈20 different 3D structures with characteristic sizes (e.g., ribbon width) ranging from ≈200 µm to ≈2 cm and with geometries that resemble hemispheres, fire balloons, flowers, concave lenses, saddle surfaces, waterdrops, and rodents, illustrate the essential ideas.  相似文献   

12.
The novel green-emitting phosphors of 12CaO 7Al2O3:Ce3+ , Tb3+ (C12A7:Ce3+, Tb3+) were synthesized by a solid-state reaction. Upon the excitation of Ce3+ at 350 nm, the C12A7:Ce3+, Tb3+ phosphor shows intense green emissions located at 543 nm assigning to 5D4-7F5 transitions of Tb3+ ions, and weak blue emissions centered at 434 nm due to the transitions of Ce3+ 5d-4f. The photoluminescence (PL) intensity of Ce3+ decrease with increasing Tb3+ concentration, indicating the effective energy transfer (ET) occurred from Ce3+ to Tb3+ in C12A7:Ce3+, Tb3+. The ET efficiency between Ce3+ and Tb3+ in the optimum composition reaches to 99%. Based on Dexter's ET theory, we have demonstrated that the efficient ET is a resonant type via dipole-dipole mechanism with an energy transfer critical distance of 4.02 A. Our results suggested that C12A7:Ce3+, Tb3+ phosphor would be a promising green-emitting phosphor for UV-converting white light-emitting diodes.  相似文献   

13.
An ultrahigh vacuum technique using mass spectrometry for in-situ investigations of gas–solid interactions is described in this paper. Examples of chemical reactions (oxidation, hydration) between solids and gas mixtures, dissociation of gases on solid surfaces, outgassing of solid materials and permeation of gases through membranes are discussed where the experimental arrangement is explained in detail. This Gas Phase Analysis (GPA) technique can be used at temperatures from room temperature to 1200 °C and at pressures up to 1 atm. Aspects related to sample preparation, isotopic gas mixture selection, data acquisition, calibration and interpretation of the experimental data are also addressed.  相似文献   

14.
Among perovskite semiconductors, quasi-two-dimensional (2D) materials are attractive for the pursuit of electrically driven lasing given their excellent performance in light-emitting diodes (LEDs) and their recent success in continuous-wave optically pumped lasing. We investigate the spontaneous photoluminescence emission and amplified spontaneous emission (ASE) of a series of quasi-2D emitters, and their directly analogous 3D materials formed by removing the 2D organic spacer by annealing. Although the PL photoluminescence (PL) (at low optical excitation power) from quasi-2D films with high 2D spacer fractions can be much brighter than that from their 3D counterparts, the ASE thresholds of these quasi-2D materials tend to be higher. This counter-intuitive behavior is investigated through time-resolved photophysical studies, which reveal the emission in the high-spacer-content quasi-2D perovskite can be exclusively excitonic, and the exciton–exciton annihilation of quasi-2D perovskite starts to take over the exciton dynamics at a low exciton density (<1016 cm−3). To lower ASE thresholds in quasi-2D materials it is necessary to increase the volume fraction of thick quantum wells, which we achieve by decreasing the spacer content or by utilizing 1-naphthylmethylamine (NMA) linkers. The increase of the volume fraction of thick quantum wells correlates with an increased contribution of free carrier recombination to the emission process of the quasi-2D materials. These results suggest that material development of quasi-2D materials for gain applications should target fast free charge carrier recombination rates by engineering the well thickness and size and not maximum photoluminescence quantum yields under low power excitation.  相似文献   

15.
The purpose of this study was to improve the dissolution properties of a poorly water soluble and bioavailable drug, ethopropazine HCl (ET), by incorporating the drug in three different types of solid dispersion systems. Solid dispersions of ET were prepared using 1:1 (w/w) ratios of (1) phospholipid (1,2 dimyristoyl-sn-glycerophosphocholine) (DMPC), (2) polyethylene glycol 8000 (PEG8000), and (3) a novel combination of both DMPC and PEG8000. Using the solvent method of preparation, ET and DMPC and/or PEG were dissolved in chloroform, and solvent subsequently was evaporated using nitrogen gas. The resulting solid dispersion(s) was passed through a 60-mesh sieve. Characterization of ET/DMPC solid dispersion was performed by differential scanning calorimetry (DSC) and X-ray diffractometry studies. Dissolution studies conducted in phosphate buffered saline (PBS) (pH 7.4, 37°C ± 0.5°C) using the USP type II (paddle) dissolution apparatus showed significant increases in the dissolution rate of ET with all the solid dispersions in this study. Specifically, within the first 5 min (D5), solid dispersions containing ET/DMPC (1:1) showed an eightfold increase in dissolution; in combination with DMPC and PEG8000 (1:1), there was an approximately sixfold increase; and a fourfold increase was observed with PEG8000 (1:1). Complete dissolution of all solid dispersions occurred within 60 min (D60) of the run. Storage of the ET/DMPC sample for over 4.5 months revealed a decrease in the dissolution rate when compared to freshly prepared sample. Overall, it was concluded that the dissolution rate of ET significantly improved when dispersed in all the selected carrier systems. However, the solid dispersion of ET/DMPC was observed to be superior to the other combinations used.  相似文献   

16.
三维(3D)石墨烯及其复合材料具有柔韧性好、比表面积大、功率密度高、力学性能稳定以及离子传输迅速等优良性能,成为材料科学领域备受关注的材料。概述了三维石墨烯材料的基本性质和性能,并对其多元复合材料的制备方法以及在超级电容器储能材料方面的应用研究进展进行了评述。三维(3D)石墨烯常用的制备方法有自组装法、模板导向法和3D打印法等,通过对制备方法进行改进,可以有效调控三维材料的多孔结构、孔径、柔韧性和电子传递速度等性能。三维(3D)石墨烯与过渡金属化合物及导电聚合物复合而成的多元复合物在超级电容器电极材料方面表现出广阔的应用前景。  相似文献   

17.
The purpose of this study was to improve the dissolution properties of a poorly water soluble and bioavailable drug, ethopropazine HCl (ET), by incorporating the drug in three different types of solid dispersion systems. Solid dispersions of ET were prepared using 1:1 (w/w) ratios of (1) phospholipid (1,2 dimyristoyl-sn-glycerophosphocholine) (DMPC), (2) polyethylene glycol 8000 (PEG8000), and (3) a novel combination of both DMPC and PEG8000. Using the solvent method of preparation, ET and DMPC and/or PEG were dissolved in chloroform, and solvent subsequently was evaporated using nitrogen gas. The resulting solid dispersion(s) was passed through a 60-mesh sieve. Characterization of ET/DMPC solid dispersion was performed by differential scanning calorimetry (DSC) and X-ray diffractometry studies. Dissolution studies conducted in phosphate buffered saline (PBS) (pH 7.4, 37°C ± 0.5°C) using the USP type II (paddle) dissolution apparatus showed significant increases in the dissolution rate of ET with all the solid dispersions in this study. Specifically, within the first 5 min (D5), solid dispersions containing ET/DMPC (1:1) showed an eightfold increase in dissolution; in combination with DMPC and PEG8000 (1:1), there was an approximately sixfold increase; and a fourfold increase was observed with PEG8000 (1:1). Complete dissolution of all solid dispersions occurred within 60 min (D60) of the run. Storage of the ET/DMPC sample for over 4.5 months revealed a decrease in the dissolution rate when compared to freshly prepared sample. Overall, it was concluded that the dissolution rate of ET significantly improved when dispersed in all the selected carrier systems. However, the solid dispersion of ET/DMPC was observed to be superior to the other combinations used.  相似文献   

18.
This paper presents a probabilistic object recognition and pose estimation method using multiple interpretation generation in cluttered indoor environments. How to handle pose ambiguity and uncertainty is the main challenge in most recognition systems. In order to solve this problem, we approach it in a probabilistic manner. First, given a three-dimensional (3D) polyhedral object model, the parallel and perpendicular line pairs, which are detected from stereo images and 3D point clouds, generate pose hypotheses as multiple interpretations, with ambiguity from partial occlusion and fragmentation of 3D lines especially taken into account. Different from the previous methods, each pose interpretation is represented as a region instead of a point in pose space reflecting the measurement uncertainty. Then, for each pose interpretation, more features around the estimated pose are further utilized as additional evidence for computing the probability using the Bayesian principle in terms of likelihood and unlikelihood. Finally, fusion strategy is applied to the top ranked interpretations with high probabilities, which are further verified and refined to give a more accurate pose estimation in real time. The experimental results show the performance and potential of the proposed approach in real cluttered domestic environments.  相似文献   

19.
杨建明  汤阳  顾海  刘永加  黄大志  陈劲松 《材料导报》2018,32(15):2672-2683
多孔结构材料具有优异的物理、力学性能,应用领域广泛。目前,已开发出的多孔结构的制备方法种类繁多,然而仅少数可实现批量生产,大多数方法工艺较为复杂,并且在制备过程中难以对多孔结构进行有效控制,以致所得多孔结构仍存在某些性能方面的不足。3D打印技术的发展与应用为多孔结构的制备带来了新的途径,所制备的多孔结构可同时具备宏观孔隙和微观孔隙,其骨架及宏观孔隙可以根据需要进行设计。可用于制备多孔结构的3D打印方法主要有利用激光能量的选择性激光烧结法(SLS)、选择性激光熔化法(SLM)和激光近净成形法(LENS)等方法,利用电子束能量的电子束熔化(EBM)法,喷射粘结剂的三维印刷(3DP)法,材料挤出类中的熔融沉积成形(FDM)法和三维浆丝沉积(3DF)法,以及间接3D打印法。近年来,国内外学者对采用这些方法制备多孔结构开展了一定的研究,以期找到适合具体情况的3D打印方法及相应合理的工艺规范,从而提高制件的性能。采用SLS、SLM和LENS法,通过控制激光扫描轨迹和粉末烧结程度可以获得材料的宏观和微观孔隙。SLS法可制备的多孔结构材料种类较广,SLM和LENS法主要用于制备金属多孔结构。EBM法与SLM法类似,但EBM法需要在真空环境下成形,可用于制备Ti等活泼金属材料。适用于3DP法的粉末材料种类更广,可选用不同的粘结剂和相应的后处理方法,其工艺灵活性大。FDM法一般用于低熔点热塑性材料,通过熔融挤出而堆积成宏观多孔结构。3DF法以粉末浆料的形式挤出成形,适用的材料种类比FDM法广,得到的结构具有宏观和微观孔隙。FDM和3DF法的打印精度和孔隙尺寸受喷嘴打印能力的限制。间接法先利用某种便捷的3D打印方法制备出多孔结构原模,再将该原模经粉末冶金、浇注等方法制得所需的多孔结构材料,这样可以避免3D打印直接制备某些材料的多孔结构在结构特征方面受到的限制。上述这些方法中,由于激光和电子束的能量集中,故SLM和EBM法制备的多孔结构相对于其他方法更精细。3D打印制备多孔结构时孔隙的形成机理可以总结为:制件内打印轨迹未到达的区域形成的宏观设计孔隙、制件骨架内的粘结剂被加热分解或被溶解而去除后形成的孔隙、气体溶解在烧结过程中的熔融金属内形成的孔隙、激光扫描熔迹之间形成的孔隙、粉末颗粒间堆积空隙形成的孔隙。本文对3D打印制备多孔结构的研究与应用现状进行了综述,概述了制备多孔结构的几种主要的3D打印方法,总结了其孔隙的形成机理,介绍了3D打印多孔结构的应用现状,指出了未来需要开展的研究。  相似文献   

20.
Dielectric properties of heterogeneous materials for various condensed-matter systems have been gaining world-wide attention over the past 50 or so years in the design (or engineering) of materials structures for desired properties and functional purposes. These applications range from cable and current limiters to sensors. These multiscale systems lead to challenging problems of connecting micro- or meso-structural features to macroscopic materials response, i.e. permittivity, conductivity. This article first reviews progress made at that time of the underlying physics of dielectric heterostructures and points out the missing elements that have led to a resurgence of interest in these and related materials. Recent advances in computational electromagnetics provide unparalleled control over morphology in this class of materials to produce a seemingly unlimited number of exquisitely structured materials endowed with tailored electromagnetic, and other physical properties. In the text to follow, we illustrate how an ab initio computational technique can be used to accurately characterize structure-dielectric property relationships of periodic heterostructures in the quasistatic limit. More specifically, we have carried out two-dimensional (2D) and three-dimensional (3D) numerical studies of two-component materials in which equal-sized inclusions, with shape and orientation and possibly fused together, are fixed in a periodic square (2D) or cubic (3D) array. Boundary-integral equations (BIE) are derived from Green's theorem and are solved for the local field with appropriate periodicity conditions on a unit cell of the structures using the field calculation package PHI3D. A number of illustrative examples shows how this computational technique can provide very accurate predictions for the complex effective permittivity of translationally-invariant heterostructures. The performance of the method is also compared with those of other computational and analytical techniques. We comment on how this computational method helps identify some important characteristics for rationalizing and predicting the structure of composite materials in terms of the nature, size, shape and orientation of their constituents.  相似文献   

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