Materials Science Forum Vols. 558-559

Abstract: Crystallization behavior of gas atomized and spark plasma sintered (SPS) Cu54Ni6Zr22Ti18 amorphous powders were studied using X-ray diffractometer (XRD), differential scanning calorimeter (DSC) and transmission electron microscope (TEM). By heating to the temperatures of 837K and 909K, the amorphous phases in the powders formed particles such as Cu10Zr7 and Cu51Zr14. The size of crystals devitrified is about 20nm and 50nm, respectively. In order to identify the sintering ability of SPS, the compressive strength was measured with the initial powder size and SPS pressure.

Abstract: Nanoscale BaTiO3 powders were prepared by hydro-thermal synthesis as a function of solvent conditions. The size of the BaTiO3 powders was in the range of 20 ~ 100 nm. The variation in the relative volume fraction of the tetragonal phase was analyzed quantitatively by means of XRD and Raman spectroscopy. It was found that the maximum volume fraction of the tetragonal phase was ~ 29 %; this was obtained when the synthesis was performed at a solvent condition R (H2O/(H2O + EtOH)) = 0.25.

Abstract: The static recrystallization (SRX) behavior of nano grained (NGed) Cu-30mass%Zn alloy processed by Multi-directional forging (MDF) was investigated. The NGed Cu-Zn alloy showed characteristic annealing behavior. The SRX nucleation and its grain growth occurred more readily in the samples deformed to higher cumulative strain at lower temperature. The frequency of new grain formation in the samples MDFed at 77 K was much higher than that at 300 K. The new grains were composed of fine annealing twins with thickness from 10 to 200 nm. The average grain size fully recrystallized was less than 300 nm.

Abstract: ZnO nanopowders were prepared by Solution Combustion Method (SCM). The ZnO nanopowders synthesized using Zn(OH)2 and glycine as an oxidant and a fuel (with fuel/ oxidant ratio, F/O=0.8), showed excellent crystalline and photocatalytic characteristics. To confirm photocatalytic activities of the prepared ZnO powder, total organic carbon (TOC) was tried to remove from aqueous phenol solution. Surprisingly, SCM ZnO nanopowder shows 1.6 fold higher destruction rates of the organic pollutant than P-25 TiO2 nanopowder which is known as a kind of standard photocatalyst.

Abstract: Nanocrystalline ceria-based thin films are of potential interest for use as gas-sensing layers and electrolytes in micro-Solid Oxide Fuel Cells (micro-SOFC) used for energy supply of next generation portables. In these devices the thin films have to be operated at intermediate to high temperatures (500 - 1000 °C) to be sufficiently high electrical conductive. However, only little is known on the nucleation and grain growth kinetics of pure ceria and its solid solutions when present as nanocrystalline thin film microstructures (average grain size < 100 nm). In this study amorphous, dense and crack-free CeO2 and Ce0.8Gd0.2O1.9-x thin films have been deposited by spray pyrolysis on sapphire. These films were crystallized to biphasic amorphous-nanocrystalline and fully nanocrystalline microstructures upon annealing with respect to time, temperature, heating rate and doping. Nucleation and grain growth kinetics were studied by differential scanning calorimetry, Xray diffraction analysis with in-situ heating chamber and scanning electron microscopy.

Abstract: A pure OFHC copper is subjected to severe plastic deformation (SPD) by a well defined high pressure torsion process at ambient temperature. The change in microstructure of samples deformed to different strains, up to ε=64, is investigated in-situ, during annealing at 170°C, within a scanning electron microscope. The spatial distribution of nucleation sites changes significantly with increasing strain from nucleation at triple junctions and grain boundaries to a random distribution of sites for von Mises equivalent strains beyond ε=4. The resulting mean size of recrystallized grains is about 6.75 times larger than the mean microstructural size of the corresponding as-deformed state. For strains larger than ε=16 the recrystallized microstructure appears to be independent of preceding strain. A detailed investigation of the nucleation of recrystallized grains following very large strains shows that certain microstructural elements are favoured as nuclei and were particularly taken into account.

Abstract: The paper deals with the evolution of recrystallization texture during annealing of Equal Channel Angular Extrusion (ECAE) processed copper with different deformation texture that may evolve as a result of different routes of ECAE. The deformation and recrystallization texture components have been separated and corresponding texture analysis has been carried out. An attempt has been made to understand the origin of recrystallization texture.

Abstract: Cu2O conical micron-scale protrusions have been grown on a preoxidized Cu surface by the Ar ion beam irradiation at 9 kV for 5-20 min in the low vacuum. This Ar ion irradiation is based on the ‘Transcription Method’ which has been originated by B.-S. Xu and S.-I. Tanaka in 1996 to form nanoparticles. Ar ion irradiation induced needle-like nanostructures composed of Cu2O and CuO which were randomly nucleated on Cu surface by the oxidation at 623 K for 10 min in the air. The obtained Cu2O conical protrusions have a controllable length of up to 14.6 μm with diameter in the range of 0.8 μm by changing the Ar ion irradiation angle to the surface. The mechanism of the formation of the conical protrusions is proposed that Cu atoms on the Cu surface activated and sputtered by the Ar ion irradiation diffuse on the surface of needle-like oxide as nuclei along the Ar ion track and react with residual oxygen atoms to grow the conical Cu2O protrusions.

Abstract: Studies on lattice change of a nickel-phosphorus amorphous alloy were carried out using not only high temperature X-ray diffraction but also extended X-ray absorption fine structure (EXAFS) analysis. Their thermal properties were characterized by differential scanning calorimetry (DSC). Since the results suggested that lattice relaxation occurred in the amorphous state by annealing, EXAFS measurements were carefully performed for characterizing the local structure of the amorphous alloys. The EXAFS analysis showed that the local structures around Ni atoms, which may be the Ni-Ni and Ni-P correlation, were changed by annealing. High temperature X-ray diffraction showed that small amount of crystal phase appeared by annealing up to 820 K, while clear diffraction peaks of Ni3P were observed above 1100 K. These micro/nanoscale structural changes did not correspond to that obtained by DSC which showed an exothermic reaction of atomistic reordering at 630 K. We need analysis of the nanostructures by small angle X-ray scattering or a high resolution transmission electron microscope.

Abstract: Alloys of CoFe-rich magnetic films are well known as typical soft magnetic alloys. They are used for many kinds of electric and electronic parts such as magnetic recording heads, transformers and inductors. In order to get superior soft magnetic properties of the CoFe-based nanocrystalline thin films, the effect of O2 partial pressure on magnetic properties of Co-Fe-Hf-O nanocrystalline thin films have been investigated. It is found that the soft magnetic properties and electrical property of these films show a dependence on the partial pressure of reactive gases, which presumably changes the microstructure of the films and related magnetic anisotropy. With optimal conditions, thin film exhibit excellent soft magnetic properties: saturation magnetization (4πMs) of 21 kG, magnetic coercivity (Hc) of 0.18 Oe, anisotropy field (Hk) of 49 Oe, and an electrical property is also shown to be as high as 300 μcm. The combination of high 4πMs and relatively high Hk in these films are believed to be partly responsible for the excellent ultra-high-frequency behavior