Authors: Stanislav Rusz, Jan Dutkiewicz, Marek Faryna, Wojciech Maziarz, Lukasz Rogal, Joanna Bogucka, Karel Malanik, Jan Kedroň, Stanislav Tylšar
Abstract: Commercial brass Ms36, 2mm thick was annealed and deformed in 6 passes in dual rolls equipment with attached equal channel equipment (DRECE). Then, material was deformed again using constrained groove pressing (CGP) by pressing of grooves 4.2 mm thick, and the groove angle of 45 deg. The experiment was performed 8 times (pressing out grooves and straightening at room temperature). Both methods allowed deformation without changing of the thickness of the sample, which was almost constant near 2 mm. The tensile experiment have shown the Yield Strength YS after 8x groove pressing of 210 MPa and Ultimate Tensile Strength UTS increased 27% up to 430 MPa. At the same time total elongation decreased from 34 to 15 %. The structure of the material after DRECE 6 passes was investigated using conventional TEM and have shown only rather uniform distribution of dislocations. After additional 8 groove pressing experiment, frequent, narrow deformation twins were observed accompanied by the formation of subgrains. Orientation imaging microscopy performed have shown average grain size after DRECE process near 5 μm, which decreased after 8 processes of groove pressing down to 2.9 μm. The fraction of low angle boundaries (below 5 deg) decreased after groove pressing down to 73% from 85% after DRECE process and annealing, while the fraction of high angle grain boundaries (>15 deg) increased after groove pressing up to 24% from 14%, however the total length of high angle boundaries increased more than 2 times since grain size decreased. The structure studies have shown rather mild effect on the grain refinement of both methods and they have to be modified to obtain material approaching nanosize range.
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Authors: Lidia Lityńska-Dobrzyńska, Jan Dutkiewicz, Wojciech Maziarz, Marek Faryna, Katarzyna Stan, Adam Kanciruk
Abstract: The alloys Al-12 wt % Zn-3 wt % Mg-1.5 wt % Cu with addition of Zr were melt spun and then hot pressed under 600 MPa pressure at 380 °C. Refinement of the microstructure and reduction of the volume fraction of the η (MgZn2) phase was observed in melt spun ribbon, as compared to the mould cast alloys. Good quality samples without pores and cracks obtained by hot pressing were composed of grains of size 0.2-0.5 µm. The particles of the η phase enriched in Zn, Mg and Cu were homogenously distributed in the matrix, while a few nanometres large precipitates of magnesium oxide were located at grain boundaries. Plate like precipitates of metastable h¢ phase appear after ageing at 120 °C and lead to microhardness increase up to about 195 HV as compared to 145 HV in pressed sample. Hot pressed ribbons showed compression strength of about 450 MPa which increased up to 630 MPa after ageing.
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Authors: Katarzyna Berent, Marek Faryna
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.
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