This study used optical and scanning electron microscopy to analyze the surface oxidation phenomenon that accompanies a γ'-precipitate free zone in a directional solidified CM247LC high temperature creep specimen. Surface oxidation occurs on nickel-based superalloy gas turbine blades due to high temperature during use. Among the superalloy components, Al and Cr are greatly affected by diffusion and movement, and Al is a major component of the surface oxidation products. This out-diffusion of Al was accompanied by γ' (Ni3Al) deficiency in the matrix, and formed a γ'-precipitate free zone at the boundary of the surface oxide layer. Among the components of CM247LC, Cr and Al related to surface oxidation consist of 8 % and 5.6 %, respectively. When Al, the main component of the γ' precipitation phase, diffused out to the surface, a high content of Cr was observed in these PFZs. This is because the PFZ is made of a high Cr γ phase. Surface oxidation of DS CM247LC was observed in high temperature creep specimens, and γ'-rafting occurred due to stress applied to the creep specimens. However, the stress states applied to the grip and gauge length of the creep specimen were different, and accordingly, different γ'-rafting patterns were observed. Such surface oxidation and PFZ and γ'-rafting are shown to affect CM247LC creep lifetime. Mapping the microstructure and composition of major components such as Al and Cr and their role in surface oxidation, revealed in this study, will be utilized in the development of alloys to improve creep life.

High-temperature oxidation of a Ni-based superalloy was analyzed with samples taken from gas turbine blades, where the samples were heat-treated and thermally exposed. The effect of Cr/Ti/Al elements in the alloy on high temperature oxidation was investigated using an optical microscope, SEM/EDS, and TEM. A high-Cr/high-Ti oxide layer was formed on the blade surface under the heat-treated state considered to be the initial stage of high-temperature oxidation. In addition, a PFZ (γ’ precipitate free zone) accompanied by Cr carbide of Cr23C6 and high Cr-Co phase as a kind of TCP precipitation was formed under the surface layer. Pits of several μm depth containing high-Al content oxide was observed at the boundary between the oxide layer and PFZ. However, high temperature oxidation formed on the thermally exposed blade surface consisted of the following steps: ① Ti-oxide formation in the center of the oxide layer, ② Cr-oxide formation surrounding the inner oxide layer, and ③ Al-oxide formation in the pits directly under the Cr oxide layer. It is estimated that the Cr content of Ni-based superalloys improves the oxidation resistance of the alloy by forming dense oxide layer, but produced the σ or μ phase of TCP precipitation with the high-Cr component resulting in material brittleness.

In this study, defects generated in the YSZ coating layer of the IN738LC turbine blade are investigated using an optical microscope and SEM/EDS. The blade YSZ coating layer is composed of a Y-Zr component top coat layer and a Co component bond coat layer. A large amount of Cr/Ni component that diffused from the base is also measured in the bond coat. The blade hot corrosion is concentrated on the surface of the concave part, accompanied by separation of the coating layer due to the concentration of combustion gas collisions here. In the top coating layer of the blade, cracks occur in the vertical and horizontal directions, along with pits in the top coating layer. Combustion gas components such as Na and S are contained inside the pits and cracks, so it is considered that the pits/cracks are caused by the corrosion of the combustion gases. Also, a thermally grown oxide (TGO) layer of several μm thick composed of Al oxide is observed between the top coat and the bond coat, and a similar inner TGO with a thickness of several μm is also observed between the bond coat and the matrix. A PFZ (precipitate free zone) deficient in γ' (Ni3Al) forms as a band around the TGO, in which the Al component is integrated. Although TGO can resist high temperature corrosion of the top coat, it should also be considered that if its shape is irregular and contains pore defects, it may degrade the blade high temperature creep properties. Compositional and microstructural analysis results for hightemperature corrosion and TGO defects in the blade coating layer used at high temperatures are expected to be applied to sound YSZ coating and blade design technology.

Microbiologically Influenced Corrosion (MIC) occurring in underground buried pipes of API 5L X65 steel was investigated. MIC is a corrosion phenomenon caused by microorganisms in soil; it affects steel materials in wet atmosphere. The microstructure and mechanical properties resulting from MIC were analyzed by OM, SEM/EDS, and mapping. Corrosion of pipe cross section was composed of ① surface film, ② iron oxide, and ③ surface/internal microbial corrosive by-product similar to surface corrosion pattern. The surface film is an area where concentrations of C/O components are on average 65 %/ 16 %; the main components of Fe Oxide were measured and found to be 48Fe-42O. The MIC area is divided into surface and inner areas, where high concentrations of N of 6 %/5 % are detected, respectively, in addition to the C/O component. The high concentration of C/O components observed on pipe surfaces and cross sections is considered to be MIC due to the various bacteria present. It is assumed that this is related to the heat-shrinkable sheet, which is a corrosion-resistant coating layer that becomes the MIC by-product component. The MIC generated on the pipe surface and cross section is inferred to have a high concentration of N components. High concentrations of N components occur frequently on surface and inner regions; these regions were investigated and Na/Mg/Ca basic substances were found to have accumulated as well. Therefore, it is presumed that the corrosion of buried pipes is due to the MIC of the NRB (nitrate reducing bacteria) reaction in the soil.

The effect of solidification rate on micro-segregation in investment casting of IN738LC superalloy was studied. In Ni-based superalloys, the micro-segregation of solute atoms is formed due to limited diffusion during cast and solidification. The microstructure of cast Ni-based superalloys is largely divided into dendrite core of initial solidification and interdendrite of final solidification. In particular, mosaic shaped eutectic γ/γ’ and carbides are formed in the interdendrite of the final solidification region in some cases. The micro-segregation phenomena formed in regions of dendrite core and interdendrite including eutectic γ/γ’ and carbides were analyzed using OM, SEM/EDS and micro Vickers hardness. As a result of analysis, the lack of (Cr, W) and the accumulation of Ti were measured in the eutectic γ/γ’, and the accumulation of (Cr, Mo) and the lack of Ti were measured in the interdendrite between dendrite and eutectic. Carbides formed in interdendritic region were composed of (Ti, W, Mo, C). The segregation applied to each microstructure is mainly due to the formation of γ’ with Ni3(Al,Ti) composition. The Ni accumulation accompanied by Cr depletion, and the Ti accumulated in the eutectic region as a γ’ forming elements. The Mo tends to diffuse out from the dendrite core to the interdendrite, and the W diffuse out from the interdendrite to the dendrite core. Therefore, the accumulation of Mo in the interdendrite and the deficiency of W occur in the eutectic region located in the interdendrite. Heat treatment makes the degree of the micro-segregation decrease due to the diffusion during solid solution. This study could be applied to the heat treatment technology for the micro-segregation control in cast Ni-based superalloys.

This study investigated the surface pit corrosion of SS420J2 stainless steel accompanied by intergranular crack. To reveal the causes of surface pits and cracks, OM, SEM, and TEM analyses of the microstructures of the utilized SS420J2 were performed, as was simulated heat treatment. The intergranular cracks were found to have been induced by a grain boundary carbide of (Cr,Fe)23C6, which was identified by SEM/EDS and TEM diffraction analyses. The mechanism of grain boundary sensitization occurred at the position of the carbide, followed by its occurrence at the Cr depleted zone. The grain boundary carbide of (Cr,Fe)23C6 type precipitated during air cooling condition after a 1038 °C solid solution treatment. The carbide precipitate formation also accelerated at the band structure formed by cold working. Therefore, using manufacturing processes of cooling and cold working, it is difficult to protect SS420J2 stainless steel against surface pit corrosion. Several counter plans to fight pit corrosion by sensitization were suggested, involving alloying and manufacturing processes.

The aim of this study is to consider the effect hydrogen on dezincification behavior of Cu-Zn alloys. The investigations include microstructural observations with scanning electron microscope and chemical composition analysis with energy dispersive spectrometer. The dezincification layer was found to occur in high pressure hydrogen atmosphere, not in air atmosphere. In addition, the layers penetrated into the inner side along the grain boundaries in the case of hydrogen condition. The shape of the dezincification layers was porous because of Zn dissolution from the α or β phase. In the case of stress corrosion cracks formed in the Cu-Zn microstructure, the dezincification phenomenon with porous voids was also accompanied by grain boundary cracking.

The aim of this paper is to consider the effect of the manufacturing processes on corrosion and centerline cracking of ancient bronze spoons. The ancient bronze spoons in question were made by several steps of forging, in reheated condition with cast ingots. The manufacturing method is similar to that of the modern spoons. The investigations include observations from light and scanning electron microscopes of the microstructure in terms of the crack propagation. Cracks in the centerline are caused by solute segregation in the center-line region; this solute is solidified in the final stage of bronze spoon manufacture. Centerline cracking is also caused by α phase segregation, accompanied by forged overlapping along the longitudinal direction of the spoons. A vertical stripe with cracks along the centerline of the spoon’s width is formed by folding in the wrought process. The overlapping area causes crack propagation with severe corrosion on the spoon surfaces over a period of a thousand years. The failure mechanisms of ancient bronze spoons may be similar to that of modern spoons, and the estimation of the failure mechanisms of ancient spoons can be appropriate to determine failure causes for such modern spoons.

Microstructural analysis of a (α+β) Ti alloy was investigated to consider phase transformation in each step of thethermo-mechanical process using by SEM and TEM EDS. The TAF (Ti-6Al-4Fe) alloy was thermo-mechanically treated withsolid solution at 880oC, rolling at 880oC and annealing at 800oC. In the STQ state, the TAF microstructure was composedof a normal hcp α and metastable β phase. In a rolled state, it was composed of fine B2 precipitates in an α phase, whichhad high Fe segregation and a coherent relationship with the β matrix. Finally, in the annealing state, the fine B2 precipitateshad disappeared in the α phase and had gone to the boundary of the α and β phase. On the other hand, in a lower rollingtemperature of 704oC, the B2 precipitates were more coarse in both the α and the boundary of α and β phase. We concludedthat microstructural change affects the mechanical properties of formability including rolling defects and cracks.

Metastable phase characteristics of beta Ti alloys were investigated to consider the relationship of the microstructureand diffraction pattern in TEM. TEM analysis showed that the microstructure was mottled as a modulated structure, and thediffraction pattern was composed of spot streaks between the main spots of a stable beta phase with a specific latticerelationship. The modulated structure may be induced by short distance slip or atom movement during a very short intervalof solution treated and quenched (STQ) materials. The athermal ω phase, which could be precipitated at low temperature aging,is also analysed by the metastable phase. The metastable phases including athermal ω phase had a common characteristic ofhardened and brittle behavior because the dislocation slip was restricted by a super lattice effect due to short distance atommovement at the metastable state.

The aim of this paper is to consider the effect of annealing on the coefficient of thermal expansion (CTE) of electroplated Invar Fe-Ni alloy. The CTE of the as-electroplated alloy is lower than those of alloys annealed at 400˚C and 800˚C. XRD peaks become sharper as the as-electroplated alloy is annealed, which means the grain growth. The average grain sizes of as-electroplated and as-annealed alloys at 400˚C and 800˚C are 10 nm, 70 nm, and 2μm, respectively, as determined by TEM and EBSD analyses. The CTE variation for the various grain sizes after annealing may come from the magnetostriction effect, which generates strain due to changes in the magnetization state of the alloys. The thermal expansion coefficient is considered to be affected by nano grain size in electroplated Fe-Ni Invar alloys. As grain size decreases, ferromagnetic forces might change to paramagnetic forces. The effect of lattice vibration damping of nano grain boundaries could lead to the decrease of CTE.

Austenite precipitation behavior was studied with solidification rates and alloying contents, N and Cr, in duplex stainless steels by directional solidification. Directional solidification experiments were carried out with solidification rates, 1~100mm/s, and N and Cr contents, 0~0.27wt.%, 25~28wt.% respectively, in a duplex stainless steel, CD4MCU. As the solidification rate increases, the dendrite spacing reduced and the austenite phase in the ferrite matrix became finer. The volume fraction of austenite phase increased and its shape went to be round with increasing nitrogen contents in duplex stainless alloys. The Cr alloying element, even though it is a ferrite former, showed to enhance the nitrogen solubility in the alloy and caused the austenite round and finer. Also, Cr was supposed to decrease the austenite volume fraction, but it increased the austenite slightly due to increasing nitrogen solubility during solidification.