Dynamic processes at the solid-liquid interface are of key importance across broad areas of science and technology. Electrochemical deposition of copper, for example, is used for metallization in integrated circuits, and a detailed understanding of nucleation, growth and coalescence is essential in optimizing the final microstructure. Our understanding of processes at the solid-vapour interface has advanced tremendously over the past decade due to the routine availability of real-time, high-resolution imaging techniques yielding data that can be compared quantitatively with theory. However, the difficulty of studying the solid-liquid interface leaves our understanding of processes there less complete. Here we analyse dynamic observations--recorded in situ using a novel transmission electron microscopy technique--of the nucleation and growth of nanoscale copper clusters during electrodeposition. We follow in real time the evolution of individual clusters, and compare their development with simulations incorporating the basic physics of electrodeposition during the early stages of growth. The experimental technique developed here is applicable to a broad range of dynamic phenomena at the solid-liquid interface.
We investigate the evolution of texture and grain morphology in fine-grained TiN thin films using cross correlation of dark-field images obtained using annular objective apertures with radii that correspond to different low index TiN reflections. This technique enables parallel analyses of the orientations of thousands of grains, with a spatial resolution of order 10 nm. Preferred grain orientations were determined for 40 and 100 nm thick TiN layers grown on SiO2 by magnetically unbalanced reactive magnetron sputter deposition. We find that no single orientation is dominant in the 40 nm films but that a 〈100〉 texture has developed by the time these films reach 100 nm in thickness.
It is difficult to determine the accuracy of NBD measurements for several reasons including, the uncertainty in the actual value of the strain in the reference patterns, uncertainty in the strain of known reference samples due to sample preparation, and uncertainty in the algorithms used measure the reflection positions. In order to quantify the accuracy and sensitivity of NBD analysis several reflection fitting algorithms have been tested using simulated diffraction patterns and experimental data from structures of known composition.
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