Challenges in quantitative crystallographic characterization of 3D thin films by ACOM-TEM.

Automated crystal orientation mapping for transmission electron microscopy (ACOM-TEM) has become an easy to use method for the investigation of crystalline materials and complements other TEM methods by adding local crystallographic information over large areas. It fills the gap between high resolution electron microscopy and electron back scatter diffraction in terms of spatial resolution. Recent investigations showed that spot diffraction ACOM-TEM is a quantitative method with respect to sample parameters like grain size, twin density, orientation density and others. It can even be used in combination with in-situ tensile or thermal testing. However, there are limitations of the current method. In this paper we discuss some of the challenges and discuss solutions, e.g. we present an ambiguity filter that reduces the number of pixels with a '180° ambiguity problem'. For that an ACOM-TEM tilt series of nanocrystalline Pd thin films with overlapping crystallites was acquired and analyzed.

Comprehensive analysis of TEM methods for LiFePO4/FePO4 phase mapping: spectroscopic techniques (EFTEM, STEM-EELS) and STEM diffraction techniques (ACOM-TEM).

Transmission electron microscopy (TEM) has been used intensively in investigating battery materials, e.g. to obtain phase maps of partially (dis)charged (lithium) iron phosphate (LFP/FP), which is one of the most promising cathode material for next generation lithium ion (Li-ion) batteries. Due to the weak interaction between Li atoms and fast electrons, mapping of the Li distribution is not straightforward. In this work, we revisited the issue of TEM measurements of Li distribution maps for LFP/FP. Different TEM techniques, including spectroscopic techniques (energy filtered (EF)TEM in the energy range from low-loss to core-loss) and a STEM diffraction technique (automated crystal orientation mapping (ACOM)), were applied to map the lithiation of the same location in the same sample. This enabled a direct comparison of the results. The maps obtained by all methods showed excellent agreement with each other. Because of the strong difference in the imaging mechanisms, it proves the reliability of both the spectroscopic and STEM diffraction phase mapping. A comprehensive comparison of all methods is given in terms of information content, dose level, acquisition time and signal quality. The latter three are crucial for the design of in-situ experiments with beam sensitive Li-ion battery materials. Furthermore, we demonstrated the power of STEM diffraction (ACOM-STEM) providing additional crystallographic information, which can be analyzed to gain a deeper understanding of the LFP/FP interface properties such as statistical information on phase boundary orientation and misorientation between domains.

Combination of in situ straining and ACOM TEM: a novel method for analysis of plastic deformation of nanocrystalline metals.

Nanocrystalline metals are expected to exhibit different deformation mechanisms when compared to their coarse grained counterparts because the dislocation storage capacity decreases and the grain boundary mediated processes become more pronounced with decreasing grain size. As a new approach to directly image and quantify the plastic deformation processes in nanocrystalline thin films, a combination of automated crystal orientation mapping in microprobe STEM mode with in situ straining inside a TEM was developed. ACOM-TEM closes the gap between EBSD and BF/DFTEM by providing full orientation maps with nanometer resolution. The novel combination with in situ straining provided for the first time the possibility to directly image and quantify the structural changes of all crystallites in the ensemble of a thin film at the nanometer scale during mechanical deformation. It was used to characterize the metallographic changes during tensile deformation of a nanocrystalline Au thin film prepared by magnetron sputtering. The investigation of the grain size, grain orientation and twinning on a global (grain average over a micron sized area) and local (assembly of selected grains) scale allowed for the development of an in depth picture of the deformation processes. Grain boundary motion and local grain rotation were two of the processes acting to dissipate the applied stress. Additionally, twinning/detwinning occurred simultaneously during straining. These processes, which occurred locally already in the micro-plastic regime, led to global grain growth starting at the transition to the macro-plastic deformation regime.

Strain relaxation and vacancy creation in thin platinum films.

Synchrotron based combined in situ x-ray diffractometry and reflectometry is used to investigate the role of vacancies for the relaxation of residual stress in thin metallic Pt films. From the experimentally determined relative changes of the lattice parameter a and of the film thickness L the modification of vacancy concentration and residual strain was derived as a function of annealing time at 130 °C. The results indicate that relaxation of strain resulting from compressive stress is accompanied by the creation of vacancies at the free film surface. This proves experimentally the postulated dominant role of vacancies for stress relaxation in thin metal films close to room temperature.

Prediction of depth of sedation and anaesthesia by the Narcotrend EEG monitor.

BACKGROUND: The Narcotrend (Monitor Technik, Bad Bramstedt, Germany) assesses sedation by automatic classification of EEG signals, using a scale first used for visual evaluation of the EEG. Limited information is available on its value, and only a few studies of the method exist. We set out to study the performance of the Narcotrend during propofol sedation. METHODS: In 23 ASA I-II patients, aged 18-65 yr, about to have general anaesthesia, we induced anaesthesia in steps using a target-controlled infusion of propofol. After equilibration for 8 min at each predicted propofol concentration (0.5, 1.0, 2.0, 3.0 and 4.0 microg x ml(-1)), sedation was assessed clinically with the modified Observer's Assessment of Alertness/Sedation Scale and the Narcotrend stage was noted. The prediction performance of the Narcotrend was assessed with the prediction probability P(K). A P(K) value of 1.0 means an exact prediction on every occasion, while a P(K) of 0.5 is no better than a 50:50 chance of being correct. RESULTS: In 12 women and 11 men (age 42 (sd 11) yr), a total of 138 measurements were made; 129 were analysed and nine were of poor signal quality. The prediction probability for the corresponding level of sedation was P(K)=0.92 (se 0.01); for the different target concentrations of propofol it was P(K) = 0.91 (se 0.01). CONCLUSIONS: The Narcotrend can monitor sedation with propofol. Other sedatives, anaesthetics and opioids should be used to test this monitor.