This study analyzed the influence of ball size and process control agents on the refinement and dehydrogenation behavior of TiH2 powder. Powders milled using ZrO2 balls with diameters of 0.1 mm, 0.3 mm, and 0.3+0.5+1 mm exhibited a bimodal particle size distribution, of which the first mode had the smallest size of 0.23 μm for the 0.3 mm balls. Using ethanol and/or stearic acid as process control agents was effective in particle refinement. Thermogravimetric analysis showed that dehydrogenation of the milled powder started at a relatively low temperature compared to the raw powder, which is interpreted to have resulted from a decrease in particle size and an increase in defects. The dehydrogenation kinetics of the TiH2 powder were evaluated by the magnitude of peak shift with heating rates using thermogravimetric analysis. The activation energy of the dehydrogenation reaction, calculated from the slope of the Kissinger plot, was measured to be 228.6 kJ/mol for the raw powder and 194.5 kJ/mol for the milled powder. TEM analysis revealed that both the milled and dehydrogenated powders showed an angular shape with a size of about 200 nm.
Hydride reorientation is widely known as one of the major degradation mechanisms in Zirconium cladding during dry storage. Some previous theoretical models for hydride reorientation used assumption of an ideal radial basal pole orientation for HCP structure of Zirconium cladding. Under this assumption, circumferential hydride was considered to precipitate in the basal plane while radial hydride was considered to precipitate in the prismatic plane, thereby giving energetical penalty on thermodynamical precipitation of radial hydrides. However, in reality, reactor-grade Zirconium cladding exhibits average 30° tilted texture, adding complexity to the hydride precipitation mechanism. In this study, reactor-grade Zirconium cladding was charged with hydrogen and hydride reorientation -treated specimens were fabricated. Microstructural characterization of hydrides was conducted via following three methods in terms of interface and stored energy. And this study aimed to compare these characteristics between circumferential and radial hydrides. Using Electron Back Scattered Diffraction (EBSD), the interface was investigated assuming that interface lies parallel to the axial axis of the tube. These were further validated with Transmission Electron Microscope (TEM). In addition, Differential Scanning Calorimetry (DSC) analysis was conducted to calculate the stored energy. This investigation is expected to establish fundamental understanding of how hydrides precipitate in Zirconium cladding with different orientations. And it will also increase the predictability of radial hydride formation and help understanding the mechanical behavior of Zirconium cladding with radial hydrides.
The effects of drying temperature on the microstructure of porous W fabricated by the freeze-casting process of tert-butyl alcohol slurry with WO3 powder was investigated. Green bodies were hydrogen-reduced at 800oC for 1 h and sintered at 1000oC for 6 h. X-ray diffraction analysis revealed that WO3 powders were completely converted to W without any reaction phases by hydrogen reduction. The sintered body showed pores aligned in the direction of tertbutyl alcohol growth, and the porosity and pore size decreased as the amount of WO3 increased from 5 to 10v ol%. As the drying temperature of the frozen body increased from -25oC to -10oC, the pore size and thickness of the struts increased. The change in microstructural characteristics based on the amount of powder added and the drying temperature was explained by the growth behavior of the freezing agent and the degree of rearrangement of the solid powder during the solidification of the slurry.
High-entropy alloys have excellent mechanical properties under extreme environments, rendering them promising candidates for next-generation structural materials. It is desirable to develop non-equiatomic high-entropy alloys that do not require many expensive or heavy elements, contrary to the requirements of typical high-entropy alloys. In this study, a non-equiatomic high-entropy alloy powder Fe49.5Mn30Co10Cr10C0.5 (at.%) is prepared by high energy ball milling and fabricated by spark plasma sintering. By combining different ball milling times and ball-topowder ratios, we attempt to find a proper mechanical alloying condition to achieve improved mechanical properties. The milled powder and sintered specimens are examined using X-ray diffraction to investigate the progress of mechanical alloying and microstructural changes. A miniature tensile specimen after sintering is used to investigate the mechanical properties. Furthermore, quantitative analysis of the microstructure is performed using electron backscatter diffraction.
Cr-Si based alloys are not only excellent in corrosion resistance at high temperatures, but also have good wear resistance due to the formation of Cr3Si phase, therefore they are promising as metallic coating materials. Aluminum is often added to Cr-Si alloys to improve the oxidation resistance through which stable alumina surface film is formed. On the other hand, due to the addition of aluminum, various Al-containing phases may be formed and may negatively affect the heat resistance of the Cr-Si-Al alloys, so detailed investigation is required. In this study, two Cr-Si-Al alloys (high-Si & high-Al) were prepared in the form of cast ingots through a vacuum arc melting process and the microstructural changes after high temperature heating process were investigated. In the case of the cast high-Si alloy, a considerable amount of Cr3Si phase was formed, and its hardness was significantly higher than that of the cast high-Al alloy. Also, Al-rich phases (with the high Al/ Cr ratio) were not found much compared to the high-Al alloy. Meanwhile, it was observed that the amount of the Al-rich phases reduced by the annealing heat treatment for both alloys. In the case of the high temperature heating at 1,400 oC, no significant microstructural change was observed in the high Si alloy, but a little more coarse and segregated AlCr phases were found in the high Al alloy compared to the cast state.
In this study, the coating of an Al-Cr layer on the surface of a Zircaloy-4 alloy was carried out through plasma pretreatment coating and a laser surface melting process. Two different conditions for laser treatment, severe or minimal surface melting of the Zr alloy substrate, were applied to form the final coating. When there was significant surface melting of the Zr alloy, the solidification microstructure of the newly formed coating layer was mainly composed of needle-shaped Al3Zr, Al(Cr) and Al7Cr phases. On the other hand, the solidification microstructure of the coating layer was mainly composed of Al(Cr) and Al7Cr phases when there was minimal surface melting of Zr base in the laser process. However, when the coating was maintained at 1100 oC for 2 hours, significant inter-diffusion occurred between the phases in the coating. As a result, the upper part of the coating layer was observed to mainly consist of Al3Zr and Al8Cr5 phases, regardless of the laser treatment conditions.
The aim of this work was to investigate the effects of electrodeposition conditions on the microstructural characteristics of copper thin films. The microstructure of electroplated Cu films was found to be highly dependent on electrodeposition conditions such as system current and current density, as well as the bath solution itself. The current density significantly changed the preferred orientation of electroplated Cu films in a DC system, while the solution itself had very significant effects on microstructural characteristics in a pulse-reverse pulse current system. In the DC system, polarization at high current above 30 mA, changed the preferred orientation of Cu films from (220) to (111). However, Cu films showed (220) preferred orientation for all ranges of current density in the pulse-reverse pulse current system. The grain size decreased with increasing current density in the DC system while it remained relatively constant in the pulse-reverse pulse current system. The sheet resistance increased with increasing current density in the DC system due to the decreased grain size.
In this study, Cu-5Ni-10Sn(wt%) spinodal alloy was manufactured by gas atomization spray forming, and the microstructural features and mechanical properties of Cu-5Ni-10Sn alloy have been investigated during homogenization, cold working and age-hardening. The spray formed Cu-5Ni-10Sn alloy consisted of an equiaxed microstructure with a mixture of solid solution -(CuNiSn) grains and lamellar-structure grains. Homogenization at and subsequent rapid quenching formed a uniform solid solution -(CuNiSn) phase. Direct aging at from the homogenized Cu-5Ni-10Sn alloy promoted the precipitation of finely distributed ' or phase throughout the matrix, resulting in a significant increase in microhardness and tensile strength. Cold working prior to aging was effective in strengthening Cu-5Ni-10Sn alloy, which gave rise to a maximum tensile strength of 1165 MPa. Subsequent aging treatment slightly reduced the tensile strength to 1000-1100 MPa due to annealing effects.
High strength sheet steels for automobile are seriously compromised by hydrogen embrittlement. This issue has been continuously studied, but the field of interest, which lies between microstructural characteristics and hydrogen behavior with hydrogen charging, has not yet been thoroughly investigated. This study was done to investigate the behavior of hydrogen according to the hydrogen volume fraction on 590MPa grade DP steels, which are developed under hydrogen charging conditions as high strength sheet steels for automobiles. The penetration depths and the mechanical properties, according to charging conditions, were investigated through the distribution of micro-hardness and the microstructural observation of the subsurface zone. It was found that the amount of hydrogen trapping in 590MPa DP steels was related to the austenite volume fraction. It was confirmed that the distribution of micro-hardnesses according to the depth of the subsurface zone under the free surface showed the relationship of the depth of the hydrogen saturation between the charging conditions.
The degree of WC decomposition and hardness of thermally sprayed WC-Co coatings are important factors determining the wear resistance of the coatings. In order to minimize the degree of decomposition and to increase hardness, the effects of processing parameters of high velocity oxyfuel(HVOF) spraying on various characteristics of nanostructured WC-12Co coating have been evaluated by an experimental design method. The HVOF sprayed WC-12Co coatings consisted of various carbide phases including WC, and , with a much reduced carbon content. The degree of WC decomposition and decarburization was affected by changing barrel length and spray distance. The hardness of WC-Co coatings was strongly related to droplet temperature at substrate, and increased with increasing fuel addition and/or decreasing spray distance. The effective control of processing parameters was discussed in detail for manufacturing a high performance WC-Co coating.
Oxidation behavior and microstructural characteristics of nano-sized Sn powder were studied. DTA-TG analysis showed that the Sn powder exhibited an endothermic peak at and exothermic peak at with an increase in weight. Based on the phase diagram consideration of Sn-O system and XRD analysis, it was interpreted that the first peak was for the melting of Sn powder and the second peak resulted from the formation of phase. Microstructural observation revealed that the powder, heated to under air atmosphere, consisted of agglomerates with large particle size due to the melting of Sn powder during heat treatment. Finally, fine SnO2 powders with an average size of 50nm can be fabricated by controlled heat treatment and ultrasonic milling process
We manufactured the metal hydrides of using a very easy and cheap way that Ti-12%Mg blending powder was mechanically milled with liquid milling media such as isopropyl alcohol (, containing oxygen) and hexane (, no oxygen) as hydrogen source. The synthesized in isopropyl alcohol contained the high oxygen of 11.2%, while one in hexane had the low oxygen content of 0.7%. Such a difference of oxygen content affected the dehydriding behavior, phase transformation, and microstructural evolution at high temperature, which was investigated through X-ray diffraction and DSC measurements, and electron microscope observations
Cr-C-Ni composites were synthesized in situ from elemental powders of Cr, Ni and C by high energy milling followed by reactive sintering. The milled powders with the grain size in nano-scale were pressed to compacts and sintered. During the following thermal treatment at first the chromium carbide was formed and then the cermets were sintered in one cycle. The interface between the binder phase and the carbide grains of the in situ composite has a good bonding strength as it is not contaminated with oxidation films or other detrimental surface reactions.
Microstructural and mechanical characteristics of P/M 6061 Al alloy subjected to equal channel angular pressing (ECAP) were investigated. The P/M 6061 Al alloy had an intial grain size of approximately . An equiaxed ultra-fine grained structure with the mean grain size of was obtained by four repetitive ECAP at 473 K. The microhardness of P/M 6061 Al alloy was drastically increased from about 40 Hv to 80 Hv by two repetitive ECAP at 373 K. However, the microhardness decreased with increasing ECAP temperature. The tensile stength of as-hot-pressed P/M 6061 Al alloy before ECAP was 95 MPa, whereas it increased to both 248 MPa after two repetitive ECAP at 373 K and 130 MPa after four repetitive ECAP at 473 K. The tensile properties of the ECAPed sample were compared with those of commercial cast 6061-O and 6061-T4 Al alloys.
We compared microstructural features of the ordered cell and disordered leaves in Citrus junos Sieb. by electron microscopy. In the cell of the ordered leaves, many chloroplasts and large vacuoles were particularly observed. Also a lot of vessel, companion cell and big nucleus were presented in vascular bundle regions. The mitochondria and the other organelles were interspersed among the chloroplasts in a thin, peripheral layer of cytoplasm. The chloroplast possessed typical grana and intergranal lamellae, numerous starch grains and a few small osmophilic globules. Besides, microbodies were closely associated with the mitochondria and the chloroplast. The process of the formation of the secondary cell wall from primary cell wall was observed the vessel elements, the tonoplast wall and the secondary cell wall. It was observed that the oil sac with the unique perfume distributed the adjacent cell wall. In the cell of disordered leaves, the all of the organelles were thrust toward the cell wall due to the fusion of vacuoles in the cells. It was observed that a lot of the very small particles spreaded in the cytoplasm. The loss of unique perfume of the leaves was resulted in the destruction of the oil sac. Also, there was not observed grana, lamellae, starch and osmophillic globules in the chloroplast. The small distributed organelles was not observed but the elongation of the cell wall was proceed no longer. Therefore, the plasma membrane diverged from the cell wall. All of organelles in the cell had poor function and deformation. A massive vacuole was fulfilled in single cell and the vacuole contains a lot of large and small particles. The organelles were presented on the side of the cell wall according to the enlargement of vacuole and they were observed to be breakdown.