Materials Science Forum Vols. 561-565

Abstract: Electron backscatter diffraction (EBSD) has been developed as a novel technique for characterizing crystallographic textures in recent years. The present paper proposes an “in-situ-tracking” approach using SEM and EBSD to examining the microstructural development and grain boundary variation of stainless steel during elevated 1200 °C service. The results revealed that in addition to the coarsened grains the fraction of low angle grain boundaries (LABG) became increased and flattened obviously during service. Comparing to the regular high temperature service (below 900 °C), the present “recovery and recrystallization” process was accelerated due to dislocation fastened movement and intensive interaction. However, the grain growth mechanism still meet the well-accepted dislocation model of subgrain combination.

Abstract: Al K ELNES of oxide ceramics, which show reverse spinel and garnet structures containing two types of Al sites, are investigated site-selectively using TEM-EELS under electron channeling conditions. We applied a self-modeling curve resolution (SMCR) technique to separate a set of experimental spectra into individual spectra of individual atomic sites. The refined spectra after SMCR were in consistent with the theoretical spectra obtained by the first principles electronic structure calculations. The spectral difference of the six-coordinated aluminum between the two materials was discussed in terms of the cationic coordination.

Abstract: Pt/AlN multilayered films fabricated by alternative sputtering deposition were characterized by X-Ray Reflectometry and X-Ray Diffraction. As-deposited films have (111) and (001) preferred orientation for Pt and AlN, respectively. The X-Ray Reflectivity profiles are assigned to the total reflection and Bragg reflections due to periodic layer structure. The Bragg peaks are observed at the 2Theta range beyond 15 degree and the peak intensities increase after annealing. The reflectivity of the first order Bragg reflection is approximately 65% and is stable after annealing at 873K. Simulation of the reflectivity profile has shown roughnesses of the Pt/AlN interfaces are below 0.4nm. X-Ray Diffraction revealed the development of film texture and formation of superlattice by annealing. The latter indicates periodicity of film is very high.

Abstract: In the present study, pure elemental powders of Fe and S were mixed to give the desired compositions of Fe50S50. A SPEX 8000D high-energy ball mill was used to synthesize iron sulfide powders under an Ar-filled atmosphere. The prepared powders were examined by conventional X-ray diffractometry and synchrotron X-ray absorption spectroscopy. The experimental results revealed that mechanochemical reactions occurred during the ball milling process for all the compositions. The Fe50S50 phase was obtained after ball milling for 20 h. Extended X-ray absorption fine structure (EXAFS) results revealed that the nearest neighbor bond lengths of the radial distribution function (RDF) for iron decreased when iron sulfides formed. X-ray absorption near edge structure (XANES) of S K-edges distinguished better the structural evolution of these iron sulfides.

Abstract: Recently, the study of fine grain steels aimed at achieving into high strength has become active. Welding is one of the most effective methods for connecting the structural components. For those cases, the negative influence of any residual tensile stress induced during the welding process must be considered. It has been proved that shot-peening can effectively solve this problem. However, the influence of the Shot-Peening process on fine grain steels after welding has only been briefly reported up to now. In this study, fine grain steels were used, and specimens were obtained after heat treatment. Residual stress distributions near the surface of the fine grain steel after shot-peening were measured by X-ray diffraction technology. Moreover, the effect of hardness on distributions near the shot-peened surface was also estimated.

Abstract: The effect of tempering process on the microstructure of ultra low carbon bainitic (ULCB) steel produced by relaxation precipitation controlled phase transformation (RPC) has been investigated by transmission electron microscopy (TEM) and electron backscattered diffraction (EBSD). The results showed that the final microstructure mainly contained lath-like bainitic ferrite, granular bainite and martensite-austenite (MA) constituent in ULCB steels. On tempering at 650°C a slight increase was detected in the effective grain size as the strain-induced precipitates pinned up the dislocation walls and subgrains. After tempering at 700°C, bainitic ferrite laths started to coarsen and polygonal ferrite occurred. The effective grain size of ULCB steels in as-rolled condition was 1.5 μm at the tolerance of 10o~15o measured by EBSD technique.

Abstract: The process of phase transformation in individual Fe-Pt and Fe-Pt-Cu nanoparticles synthesized by the reverse micelle method with chemical homogeneity and mono-dispersion has been investigated by in-situ high-resolution electron microscopy (HREM) observation and in-situ nano-beam diffraction (NBD). The Fe-Pt particles, initially polycrystalline with the chemically disordered fcc (A1) phase, were reconstructed into A1 single crystals between 550 and 650°C, followed by a phase transformation from A1 to the chemically ordered fct (L10) phase between 650 and 680°C. The coalescence began almost concurrently with the phase transformation. They were transformed into round-shaped single-crystalline particles between 680 and 720°C. Similar processes were also observed in the Fe-Pt-Cu nanoparticles. The temperatures at which these processes occurred were substantially lower than those required for the Fe-Pt nanoparticles. We investigated the magnetic-field distribution of a submicron-size island comprising isolated L10 Fe-Pt nanoparticles magnetized along one direction by using in-situ electron holography at elevated temperatures. Although the magnetization decreased between 212 and 412°C to 25% of the strength at 25°C, it recovered 67% of the initial strength during cooling. However, when an island was heated to 512°C, the magnetization diminished and did not recover during cooling. The Curie temperature (Tc) was determined to be 350°C and was in good agreement with the Tc determined by bulk measurements, which was approximately 100°C lower than the Tc for bulk Fe55Pt45.

Abstract: The growth and morphology of the intermetallic compounds (IMC) formed at the interface between the solder ( Sn–3.5Ag–0.5Cu ) and the Cu substrate of the lead - free solder joint have been investigated by means of isothermal aging at 125°C. The scalloped Cu6Sn5 intermetallic compound layer was formed at the interface between the solder and Cu substrate upon reflow. The thickness of Cu6Sn5 layer increased with aging time. Cu3Sn appeared between Cu6Sn5 layer and Cu substrate when isothermally aged for 100 hours. Compare to Cu6Sn5 , the thickness of Cu3Sn was rather low, and nearly did not increase with aging time. In this paper, the comparison was made among the Sn-Pb and the Sn-Ag-Cu(SAC) solders which were pre-treated differently before soldering.

Abstract: Welding experiences are demonstrated, which were developed on 2205 type duplex and 2509 type superduplex stainless steels (DSS and SDSS). The welded joints were produced by activated TIG welding and laser beam welding. For the ATIG process, which is a special kind of the TIG-welding, silica powder was used as activating flux. Microstructural characterizations were applied for the measurement of ferrite/austenite phase ratio in the weldments. The welded joints were thermally aged at temperature of 400 °C. The phase transformations produced during thermal ageing were investigated by optical and scanning electron microscopy and thermoelectric power measurement. Investigations show that the thermal ageing induced phase transformations are similar at ATIG-welded weldment and DSS base material, but the incubation time is significantly shorter in the weldment than in the base material when laser welding is applied.

Abstract: This study investigates the phase compositions in gelcast dense alumina and porous alumina that were sintered in an inert atmosphere. Both materials were gelcasted using identical slurry composition except for adding surfactant to slurry intended for porous shaping. The resulting gelcasted samples were dried and then sintered in argon gas at 1700oC. The X-ray photoelectron analysis was used for identifying the phase compositions in sintered samples, which was supported with TG/DTA and electrical measurements. Results showed that, in addition to alumina and carbon phases, the dense sample yielded Al4C3 and Al, while porous sample yielded aluminum oxycarbides. The formation of these phases reduced the carbon content through different chemical reactions to a limited extent because they formed a protective layer on alumina grains, which prevented the direct contact between alumina and carbon. Subsequent measured electrical resistivities of dense and porous alumina were, respectively, 0.20 and 0.32 ,-cm, indicating that the carbon networks are preserved in both materials.