발간논문

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Dissolution and precipitation behaviors of complex carbonitrides in austenite of a V-Nb microalloyed steel were quantitatively examined through electrical resistivity measurement and transmission electron microscopy. The electrical resistivity increased with solution treatment temperature up to 1240℃ and then was saturated at 225 nΩm for a holding time of 10 min. The electrical resistivity method was also used to quantitatively measure the isothermal precipitation kinetics of the complex carbonitrides in austenite. Nbrich precipitates were observed in austenite at the early stages of precipitation, but Nb was replaced by V up to the equilibrium amount within the precipitates with further holding time. The time-temperatureprecipitation diagram showed a C-type curve; nose temperature and its incubation time were 900℃ and 100 s, respectively.

keyword : metals, thermomechanical processing, carbonitride, precipitation, electrical conductirity resistivity

It is well known that grain boundary cavitation is the main failure mechanism in austenitic stainless steel under tensile hold creep-fatigue interaction conditions. The cavities are nucleated at the grain boundary during cyclic loading and grow to become grain boundary cracks. The attenuation of ultrasound depends on scattering and absorption in polycrystalline materials. Scattering occurs when a propagation wave encounters microstructural discontinuities, such as internal voids or cavities. Since the density of the creepfatigue cavities increases with the fatigue cycles, the attenuation of ultrasound will also be increased with the fatigue cycles and this attenuation can be detected nondestructively. In this study, it is found that individual grain boundary cavities are formed and grow up to about 100 cycles and then, these cavities coalesce to become cracks. The measured ultrasonic attenuation increased with the cycles up to cycle 100, where it reached a maximum value and then decreased with further cycles. These experimental measurements strongly indicate that the open pores of cavities contribute to the attenuation of ultrasonic waves. However, when the cavities develop, at the grain boundary cracks whose crack surfaces are in contact with each other, there is no longer any open space and the ultrasonic wave may propagate across the cracks. Therefore, the attenuation of ultrasonic waves will be decreased. This phenomenon of maximum attenuation is very important to judge the stage of grain boundary crack development, which is the indication of the dangerous stage of the structures.

keyword : alloys, non-destructive test, defects, scanning electron microscopy (SEM), creep-fatigue

In the present study, we show that the addition of Ag, an element having a positive enthalpy of mixing with Cu in the liquid state, enables the simultaneous enhancement of the glass forming ability and the plasticity in Cu-Zr-Ag bulk metallic glasses (BMGs). Rods of 4 mm diameter could be prepared with a fully amorphous structure and values of plastic strain up to 18% were measured under a compression mode for compositions around Cu42.5Zr47.5Ag10. The possible role of Ag in the change of the atomic structure and the enhancement of the plastic strain in the ternary Cu-Zr-Ag BMGs is discussed based on analyses from transmission electron microscopy and EXAFS (extended X-ray absorption fine structure).

keyword : amorphous, Cu-Zr based BMGs, EXAFS, 3D-AP, plasticity

Studies have been carried out in order to reduce fuel-cladding chemical interaction (FCCI) behavior of metallic fuel in sodium-cooled fast reactors (SFR) using an electroplating technique. A 20㎛thick Cr layer has been plated by the electrochemical method in the Sargent bath over the HT9 (12Cr-1Mo) clad material and diffusion couple tests of the U-10Zr metallic fuel as well as the rare earth alloy (70Ce-29La) have been conducted. The results show that the Cr plating can prevent FCCI behavior along the fuel-clad interface. However, cracks developed through the thickness during plating, which resulted in the migration of some fuel constituents. Variation of bath temperature, application of pulse current, and post heat treatment have been conducted to control such cracks. We found out that some conditions like the pulse current and the post heat treatment enhanced the layer property by reducing the internal cracks and improving the diffusion couple test.

keyword : metals, plating, diffusion, scanning electron microscopy (SEM), chromium

The cycling characteristics of MgH2 made by hydriding chemical vapor deposition method have been investigated. The particle size of MgH2 made by HCVD was about 1 μm. The cycling experiment was performed by measuring hydrogen quantity absorbed at 673 K and under 35 atm of hydrogen pressure for 30 min. Up to 3 cycles the hydrogen storage capacity increased, but from 4 to 6 cycles the hydrogen storage capacity decreased rapidly. During this cycling test the particle size increased gradually from 1㎛to 6㎛. This increase was due to sintering by the high reaction temperature and the heat of reaction during hydrogen absorption. From 7 to 30 cycles, the hydrogen storage capacity was maintained at 5.8 wt%. Even after 30 cycles, the plateau pressure was constant.

keyword : hydrogen absorbing materials, vapor deposition, hydrogen, X-ray diffraction, magnesium hydride

In the present study, the formation of hollow Cu oxide nanoparticles through the oxidation process at temperatures from 200 to 300℃ has been studied by transmission electron microscopy with Cu nanoparticles produced by the plasma arc discharge method. The Cu nanoparticles had a thin oxide layer on the surface at room temperature and the thickness of this oxide layer increased during oxidation in atmosphere at 200-300℃ However, the oxide layer consisted of Cu2O and CuO after oxidation at 200℃ whereas this layer was comprised of only CuO after oxidation at 300℃ On the other hand, hollow Cu oxide nanoparticles are obtained as a result of vacancy aggregation in the oxidation processes, resulting from the rapid outward diffusion of metal ions through the oxide layer during the oxidation process.

keyword : oxidation, hollow, nanoparticles, interdiffusion

Bioleaching studies of metals from a spent catalyst were conducted using both adapted and unadapted bacterial cultures. The bacterium used in this experiment was Acidithiobacillus ferrooxidans. A comparison of the kinetics of leaching was made between the two cultures by varying the leaching parameters, including the pulp density, particle size and temperature. Both cultures showed similar effects with respect to the above parameters, but the leaching rates of all metals were higher with the adapted compared to the unadapted bacterial cultures. The leaching reactions were continued for 240 h in the case of the unadapted bacterial culture, but only for 40 h in the case of the adapted bacterial culture. The leaching reactions followed first order kinetics. In addition, the kinetics of leaching was concluded to be a diffusion control model; therefore, the product layers were impervious.

keyword : bioleaching, spent catalyst, adaptation, kinetics, Acidithiobacillus ferrooxidans

Conventional fracture tests of resistance spot welds have been performed without consideration of the paint baking process in the automobile manufacturing line. The aim of this paper is to investigate the effect of the paint baking process on load carrying capacity and fracture mode for resistance spot welded 590 dual phase (DP), 780DP, 980DP, 590 transformation in duced plasticity (TRIP), 780TRIP and 1180 complex phase (CP) steels. With paint baking after resistance spot welding, the l-shape tensile test (LTT) and nano-indentation test were conducted on the as-welded and paint baked samples. Paint baking increased the load-carrying capacity of the resistance spot welded samples and improved the fracture appearance from partial interfacial fracture (PIF) to button fracture (BF). Improvement in fracture appearance after LTT is observed on weldments of 780 MPa grade TRIP steels, especially in the low welding current range with paint baking conditions. The higher carbon contents (or carbon equivalent) are attributed to the low weldability of the resistance spot welding of high strength steels. Improvement of the fracture mode and load carrying ability has been achieved with ferrite hardening and carbide formation during the paint baking process. The average nano-indentation hardness profile for each weld zone shows hardening of the base metal and softening of the heat affected zone (HAZ) and the weld metal, which proves that microstructural changes occur during low temperature heat treatment.

keyword : advanced high strength steels, resistance spot welding, paint baking, nano-indentation, fracture behavior

Migration and interaction of multi-protons in a zinc-doped barium zirconate (Zn-doped BaZrO3) super cell were investigated using a density functional theory. O ions in the super cell form interconnected octahedrons with Zr or Zn ions positioned in their centers and Ba ions positioned among the eight octahedrons. When one proton was added to the super cell, the energy barrier of 0.80 eV for proton transfer from the first to second nearest O ion sites from the Zn ion reached its highest value. When two protons were added to the super cell, the two protons preferred the first nearest O ions from the Zn ion. The two protons were accommodated by pushing the neighboring Zn ion further away from the center of the octahedron. Energy barriers for proton transfer from the Zn-octahedron to the neighboring Zr-octahedron were spread in the range of 0.36 ~ 1.02 eV.

keyword : fuel cells, sintering, conductivity, computer simulation, barium zirconate

Failure analyses of the screws in spinal fixation devices were carried out. The fractured screws were retrieved from a patient who had spinal surgery in the thoracic vertebrae from number 10 to 15. The failure occurred one month after the removal of the braces. Microstructures and fracture surfaces were examined by optical and scanning electron microscopy. The microstructures of the screws corresponded to annealed Ti-6Al-4V bar. However, in the vicinity of the screw surface, there was an insufficient number of fine precipitates. Fracture surfaces showed typical fatigue failure modes. Regarding the fact that no machining defects were detected, fatigue crack initiation might have been caused by the lack of precipitates near the screw surfaces. Only the fourth of five fixed screws was severely stress-concentrated by the action of the spinal bones, while the stress of the 4th screw was decreased to half of its acceptable level when the screw was supplemented by one more, which might have been fixed in the 6th vertebra under the 5th position by the switching of its position. The stress simulation was conducted by ANSYS with 3D CAD of PRO/E in order to understand the stress concentration behavior and to provide an effective spinal surgery guide.

keyword : Ti alloy screw, fractured spines, failure analysis, microstructure, stress simulation