Superficial amorphization and re-crystallization of silicon in <111> and <100> orientation after irradiation by femtosecond laser pulses (790 nm, 30 fs) are studied using optical imaging and transmission electron microscopy. Spectroscopic imaging ellipsometry (SIE) allows fast data acquisition at multiple wavelengths and provides experimental data for calculating nanometric amorphous layer thickness profiles with micrometric lateral resolution based on a thin-film layer model. For a radially Gaussian laser beam and at moderate peak fluences above the melting and below the ablation thresholds, laterally parabolic amorphous layer profiles with maximum thicknesses of several tens of nanometers were quantitatively attained. The accuracy of the calculations is verified experimentally by high-resolution transmission electron microscopy (HRTEM) and energy dispersive X-ray spectroscopy (STEM-EDX). Along with topographic information obtained by atomic force microscopy (AFM), a comprehensive picture of the superficial re-solidification of silicon after local melting by femtosecond laser pulses is drawn.
The use of focused ion beams, whilst permitting the targetted preparation of thin specimens for Transmission Electron Microscopy, also results in modification of the material to be investigated as a result of energy being transferred into the material. This undesirable effect is normally limited to the surface of the material, which is particularly unfavourably orientated towards the impinging ion beam. If the crystal structure and composition of areas close to the surface of such specimens need to be characterised, protective layers may be used. However, those layers, depending on the applied deposition technique, may interact with the sample surface as well thus affecting the results of the analysis. In the work presented here, the possible interactions which might occur between the various protective coatings of ion-beam deposited Platinum, electron beam deposited Platinum, Silicon Oxide or adhesively bonded Gold foil and the subsequent FIB-preparation of the oxide layers on Ni-Ti alloys are investigated, with respect to and how these might affect the TEM-images obtained of areas close to the surface of such specimens. It is shown that the use of adhesively bonded Gold foil as a protective coating, in particular, permits comprehensive characterisation of the surface, including the use of high-resolution TEM, to be carried out, up to the surface of the Oxide layer itself.
The present work investigates the universal applicability of glow discharge plasmas for the microstructure representation of different materials taking the example of Ni-Ti alloys, Cu-Zn alloys, and the Ni based alloy “Hastelloy C 276”. Results are compared with the results provided by classical etching methods. Microstructures became visible for the previously mechanically polished materials within a few seconds, even without detailed optimization of the excitation conditions of the glow discharge plasma. The results partially significantly outperfomed the results of the classical preparation techniques with respect to the detectability of structural details such as grain and phase boundaries. Due to the demonstrated wide and relatively uncomplicated applicability, the per se established glow discharge technology is expected to have a huge potential for application for a rapid and high-contrast microstructure representation.
In this work, an attempt was made to improve the corrosion resistance of dilute Fe-Al alloys (1.0 mass% Al) by preheating treatment at 1073 K in H2 atmosphere. In comparison with pure Fe and unpreheated Fe-Al alloys, the resistance to oxidation at 673 K in pure O2 and to electrochemical corrosion in 5 wt.% NaCl solution is significantly improved for preheated Fe-Al alloys. This improvement is attributed to the formation of a 20 nm thin, but dense Al2O3 protective layer on the surface of preheated Fe-Al alloys.
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