Results 1 - 10 of 155665
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[en] This paper provides a broad background for the historical development and modern applications of light optical metallography, scanning and transmission electron microscopy, field-ion microscopy and several forms of scanning probe microscopes. Numerous case examples illustrating especially synergistic applications of these imaging systems are provided to demonstrate materials characterization especially in the context of structure-property-performance issues which define materials science and engineering
[en] The material characterization toolbox has recently experienced a number of parallel revolutionary advances, foreshadowing a time in the near future when material scientists can quantify material structure evolution across spatial and temporal space simultaneously. This will provide insight to reaction dynamics in four-dimensions, spanning multiple orders of magnitude in both temporal and spatial space. This study presents the authors viewpoint on the material characterization field, reviewing its recent past, evaluating its present capabilities, and proposing directions for its future development. Electron microscopy; atom probe tomography; x-ray, neutron and electron tomography; serial sectioning tomography; and diffraction-based analysis methods are reviewed, and opportunities for their future development are highlighted. Advances in surface probe microscopy have been reviewed recently and, therefore, are not included (D.A. Bonnell et al.: Rev. Modern Phys. in Review). In this study particular attention is paid to studies that have pioneered the synergetic use of multiple techniques to provide complementary views of a single structure or process; several of these studies represent the state-of-the-art in characterization and suggest a trajectory for the continued development of the field. Based on this review, a set of grand challenges for characterization science is identified, including suggestions for instrumentation advances, scientific problems in microstructure analysis, and complex structure evolution problems involving material damage. The future of microstructural characterization is proposed to be one not only where individual techniques are pushed to their limits, but where the community devises strategies of technique synergy to address complex multiscale problems in materials science and engineering.
[en] Highlights: • AFM, SEM; TEM and DLS all compared. • Silica, gold, and polymer nanoparticles characterised. • AFM and TEM shown to be most appropriate for small particles. • SEM just as accurate as AFM and TEM for larger particles. • DLS shows dynamic behaviour but cannot characterise mixtures. - Abstract: Nanoparticles have properties that depend critically on their dimensions. There are a large number of methods that are commonly used to characterize these dimensions, but there is no clear consensus on which method is most appropriate for different types of nanoparticles. In this work four different characterization methods that are commonly applied to characterize the dimensions of nanoparticles either in solution or dried from solution are critically compared. Namely, transmission electron microscopy (TEM), scanning electron microscopy (SEM), atomic force microscopy (AFM), and dynamic light scattering (DLS) are compared with one another. The accuracy and precision of the four methods applied nanoparticles of different sizes composed of three different core materials, namely gold, silica, and polystyrene are determined. The suitability of the techniques to discriminate different populations of these nanoparticles in mixtures are also studied. The results indicate that in general, scanning electron microscopy is suitable for large nanoparticles (above 50 nm in diameter), while AFM and TEM can also give accurate results with smaller nanoparticles. DLS reveals details about the particles’ solution dynamics, but is inappropriate for polydisperse samples, or mixtures of differently sized samples. SEM was also found to be more suitable to metallic particles, compared to oxide-based and polymeric nanoparticles. The conclusions drawn from the data in this paper can help nanoparticle researchers choose the most appropriate technique to characterize the dimensions of nanoparticle samples.
[en] We examined thin epitaxial films La5/8-yPryCa3/8MnO3 (LPCMO:y=0.275-0.3) in situ by Lorentz transmission electron microscopy (TEM) and other microscopy methods. Clear evidence was obtained for the competing two-phase coexistence of antiferromagnetic charge-ordered (CO) and ferromagnetic (FM) phases that exhibit mesoscale phase separation below the metal-to-insulator transition (MIT) at -164 K. In addition, we observed some regions of mixed CO- and FM-domain contrast attributed earlier to formation of the new CO-FM phase. Using in situ heating/cooling TEM experiments, we interpret this effect as the interfacial wetting phenomenon inherent to the first-order CO-FM phase transition, rather than to the formation of new CO-FM phase. It is evidenced by the partial magnetic melting of CO phase at interfaces with the FM phase, thereby creating charge-disordered spin-glass metastates. For coexisting CO- and FM-domain configurations, we directly refined the relationship between charge-orbital and spin-ordering vectors, consistent with FM moments pinned by (101)-crystal twins in LPCMO films. We also discuss the striking linear dependence observed below MIT for the log-resistance behavior and the CO fraction in LPCMO directly measured by TEM. Such linear dependence does not follow typical percolation equations, suggesting that percolation model needs further revisions for transport description of manganites.
[en] It is an important challenge to make disk-like polymeric nanostructures. Herein we report a facile method for preparing polymer nanodisks by self-collapse of nanocapsules self-assembled from a statistical copolymer after partial hydrolysis. We find that partial hydrolysis of the statistical copolymer is crucial for the formation of nanodisks as it affords a suitable rigidity for the membrane of nanocapsules. The nanodisk structure has been confirmed by transmission electron microscopy (TEM), scanning electron microscopy (SEM) and atomic force microscopy (AFM) studies with a thickness of 6.3±0.2 nm. Overall, our results demonstrated a new method for making disk-like nano-objects.
[en] We report on Atomic Force Microscopy (AFM) and Scanning Tunneling Microscopy (STM) investigations on chemical vapour deposited heteroepitaxial diamond films. Besides the good macroscopic crystal morphology a statistical tilt up to ± 5.2 of the oriented crystallites has been found relative to the silicon substrates. By optimizing the process conditions, however, the crystal tilt of the films can be reduced, resulting in an improved film perfection. On crystallite (001)-surfaces a substructure of growth facets or islands has been found and high resolution STM images have established a 2 x 1 surface reconstruction on these growth facets. AFM and SEM were applied to study the morphology of diamond nuclei initially grown on the silicon substrate. Strong island like (Volmer-Weber) growth has been found, with a nucleus height to diameter ratio of 1:1. While the islands are growing in size with respect to time of nucleation, its aspect ratio does not change, due to the high surface free energy of the diamond relative to silicon. (orig.)
[en] We have developed a modified sputtering gun for direct synthesis of metallic nanoparticles, and used this system to produce magnetic domain images using high-resolution Bitter microscopy (HRBM). The nanoparticles are produced at 900 mTorr inside the gun and transported to the main vacuum chamber by the pressure difference between the chamber and the gun interior. Fe particles synthesized using the particle gun have been characterized using X-ray diffraction, atomic force microscopy, and transmission electron microscopy techniques. The particles are 15-30 nm in size with a pure BCC phase. Further, we have deposited these Fe nanoparticles on magnetic recording media and observed the domain patterns using optical microscopy, scanning electron microscopy, and atomic force microscopy. We achieve a spatial resolution of at most 80 nm
[en] This paper reviews recent developments of microscopic methods that base on a quantitative analysis of electron micrographs to access subsurface systems at the atomic scale. It focuses on non-equilibrium diffusion processes that are observed in nano structured MBE grown materials if a low growth temperature was used and on local deviations from a stoichiometric composition of materials. As examples we investigate Ga As/Al As and Si/Ge Si heterostructures and Ga N single crystals. The purpose of the research is twofold. On the one hand it helps understanding physical processes at the atomic scale. On the other hand we can use the results to link basic physical knowledge with the performance of semiconductor devices made from nano structured materials. (author). 28 refs., 15 figs