Papers by Author: Katarzyna Berent

Abstract: The nanocrystalline silver powder and the amorphous powders of composition Ni49,5Ti20,5Nb15Zr15 (numbers indicate at%) were prepared by ball milling in the planetary Fritsch mill for 40 hours. TEM studies confirmed almost complete amorphization of milled alloys powders allowed to detect a small fraction of a small intermetallic inclusions within the amorphous matrix. The erosion of composites during contact cycling was similar as in Ag-W composites known as a good contact materials. SEM and TEM studies have shown a low solubility of tungsten in silver after ball milling and no solubility of silver in tungsten. The grain size of silver crystals within powders drastically decreased after milling down to about 30 nm and only a small increase in the grain size up to 200 nm was observed after hot pressing. These results were confirmed using TEM studies of composites after hot pressing. TEM microstructures have shown very narrow transition layer at the amorphous/silver interface (between 10-30 nm thick) containing all elements from the amorphous powders plus silver due to short time of hot pressing. The amorphous part has shown growth of intermetallic phases there, however diffused ring from the amorphous part was still visible. The composites prepared from silver and tungsten have shown presence of coherent tungsten rich precipitates showing typical strain field contrast within fine grains near 100 nm formed most probably during hot pressing of silver solid solution formed during mechanical alloying. The structure of tungsten has shown less defects and consequently less grain refinement than silver particles. SEM studies of the compression tested samples of silver-amorphous composites have shown crack formation at the interfaces of both components most probably due to presence of a brittle transition phase containing all elements.

Abstract: Modern scanning electron microscopes (SEMs) increase the ability to study a wide range of materials. Especially, an application of low vacuum conditions enables characterization of nonconductive samples without complicated preparation procedure. However, the operator must be aware of several problems he may encounter collecting electron diffractions in the SEM with variable pressure. The charge control and quality of the surface are the challenges when running experiments on insulators. Specimen charging obscures forward scatter electrons images and decreases the EBSD pattern quality making indexing difficult or even impossible. Another crucial question is how to limit the influence of so called "skirt effect" caused by ionization of gas molecules followed by electron beam broading above the sample. The influence of several important parameters (gas pressure, a type of gas, working distance and energy of electron beam) on the EBSD pattern quality must also be considered. When it is properly done, a coupling of crystallographic information with the chemical data obtained from Energy Dispersive Spectroscopy (EDS) in the LV-SEM allows to perform phase identification of insulators. The paper presents some ideas how to deal with the (Pb, La)(Zr, Ti)O₃ ceramics in high resolution Quanta 3D SEM (with thermally assisted Schottky type FEG) equipped with EDAX-TSL system in low vacuum environment. The problems occurring during EBSD analysis of the PLZT ceramics are discussed and some solutions are suggested. Paper summarizes the results obtained from PLZT ferroelectric ceramics in the low vacuum FEGSEM and shows how to optimise experimental parameters in order to achieve the best quality of orientation maps acquired from nonconductive samples.