Experimental transmission electron microscopy analyses

The experimental techniques described above of charge—discharge and impedance are nondestructive. Tear-down analysis or disassembly of spent cells and an examination of the various components using experimental techniques such as Raman microscopy, atomic force microscopy, NMR spectroscopy, transmission electron microscopy, XAS, and the like can be carried out on materials-spent battery electrodes to better understand the phenomena that lead to degradation during use. These techniques provide diagnostic techniques that identify materials properties and materials interactions that limit lifetime, performance, and thermal stabiity. The accelerated rate calorimeter finds use in identifying safety-related situations that lead to thermal runaway and destruction of the battery. 

Figures 5 (a) and (b) show electron micrographs of the RuxSey particles in powder form, Fig. 5.5(a) and in colloidal form, Fig. 5.5(b). The generated particle size in both cases is ca.2 nm. It is, however, interesting that the colloidal route delivers particles with a narrow size distribution. After multiple analysis by EDX performed with transmission electron microscopy (TEM), and/or via Rut-herford backscattering spectroscopy (RBS) we concluded that the stoichiometry of the RuxSey compound corresponds to x 2 and y 1. This is another experimental evidence that the "real" chemical precursor is the intermediate...

Three diblock copolymers of cis-1,4 polyisoprene (IR) and 1,4-polybutadiene (BR) have been studied in dynamic mechanical experiments, transmission electron microscopy, and thermomechanical analysis. The block copolymers had molar ratios of 1/2, 1/1, and 2/1 for the isoprene and butadiene blocks. Homopolymers of polybutadiene and polyisoprene with various diene microstructures also were examined using similar experimental methods. Results indicate that in all three copolymers, the polybutadiene and polyisoprene blocks are essentially compatible whereas blends of homopolymers of similar molecular weights and microstructures were incompatible. 

It is not surprising therefore that the optical properties of small metal particles have received a considerable interest worldwide. Their large range of applications goes from surface sensitive spectroscopic analysis to catalysis and even photonics with microwave polarizers [9-15]. These developments have sparked a renewed interest in the optical characterization of metallic particle suspensions, often routinely carried out by transmission electron microscopy (TEM) and UV-visible photo-absorption spectroscopy. The recent observation of large SP enhancements of the non linear optical response from these particles, initially for third order processes and more recently for second order processes has also initiated a particular attention for non linear optical phenomena [16-18]. Furthermore, the paradox that second order processes should vanish at first order for perfectly spherical particles whereas experimentally large intensities were collected for supposedly near-spherical particle suspensions had to be resolved. It is the purpose of tire present review to describe the current picture on the problem. 

Because of the expected small dimensions of the oxidation products and of the oxide scale after short oxidation times it was necessary to use electron microscopic methods to characterize the samples after oxidation. Besides scanning electron microscopy (SEM) transmission electron microscopy (TEM) was mainly used to describe the morphology of the oxide scale and to identify the oxidation products by energy dispersive X-ray analysis (EDX) as well as electron diffraction. A detailed description of the preparation of TEM cross-sections and of the experimental procedure is given in [12]. 

S., Iwasaki, T, Starke, U., Smet, J.H., and Kaiser, U. (2011) Experimental analysis of charge redistribution due to chemical bonding by high-resolution transmission electron microscopy. Nat. Mater., 10(3), 209-215. 

While the theory presented here has a rather general character, one can report some specific applications of experimental interest for the theoretical approach developed. The origin of the presented results derives from the variation in energy with size and composition. So, one might expect the confirmation of the experimental results by the calculated ones in case of the size- and composition-dependent material properties. In this respect, isolated nanoparticles of Pb-Bi alloys have a loop-like split diagram and size-induced melting behavior, observed by hot-stage transmission electron microscopy [69]. Loops similar to the presented ones are obtained theoretically for separation of the solid nanoparticle [80]. Our recent analysis for Cu-Ni and Au-Cu binary nanoparticles shows the quantitative predictions [82]. 

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