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.
Radioactive mixed waste (RMW) is containing radioactive materials and hazardous materials. Radioactive wastes containing asbestos are include in RMW. These wastes thus must be treated considering both radioactive and hazardous aspects. In this study, a high temperature melt oxidation system consisting of an electric arc furnace and a molten salt oxidation furnace has been developed for the treatment of of radioactive waste containing asbestos. A surrogate waste of the radioactive waste containing asbestos (content of asbestos: 13wt%) was treated in this system. It was melted and fabricated into a glass waste form in the system. Asbestos was not detected in this glass waste form. This means that the asbestos was converted to a glass component in the glass waste form. The waste form was homogeneous glass, and it had a high value of compressive strength (475.13 MPa). It was also confirmed through a leaching test (ANS 16.1) that the waste form had a high chemical durability (Leaching Index > 6). Based on these results, it is considered that the high temperature melt oxidation system will be utilized for the treatment of a significant amount of radioactive waste containing asbestos generated from decommissioning a nuclear power plant.
Stainless steel, a type of steel used for high-temperature parts, may cause damage when exposed to high temperatures, requiring additional coatings. In particular, the Cr2O3 product layer is unstable at 1000oC and higher temperatures; therefore, it is necessary to improve the oxidation resistance. In this study, an aluminide (Fe2Al5 and FeAl3) coating layer was formed on the surface of STS 630 specimens through Al diffusion coatings from 500oC to 700oC for up to 25 h. Because the coating layers of Fe2Al5 and FeAl3 could not withstand temperatures above 1200oC, an Al2O3 coating layer is deposited on the surface through static oxidation treatment at 500oC for 10 h. To confirm the ablation resistance of the resulting coating layer, dynamic flame exposure tests were conducted at 1350oC for 5–15 min. Excellent oxidation resistance is observed in the coated base material beneath the aluminide layer. The conditions of the flame tests and coating are discussed in terms of microstructural variations.
In this study, the high-temperature oxidation properties of austenitic 316L stainless steel manufactured by laser powder bed fusion (LPBF) is investigated and compared with conventional 316L manufactured by hot rolling (HR). The initial microstructure of LPBF-SS316L exhibits a molten pool ~100 μm in size and grains grown along the building direction. Isotropic grains (~35 μm) are detected in the HR-SS316L. In high-temperature oxidation tests performed at 700oC and 900oC, LPBF-SS316L demonstrates slightly superior high-temperature oxidation resistance compared to HR-SS316L. After the initial oxidation at 700oC, shown as an increase in weight, almost no further oxidation is observed for both materials. At 900oC, the oxidation weight displays a parabolic trend and both materials exhibit similar behavior. However, at 1100oC, LPBF-SS316L oxidizes in a parabolic manner, but HR-SS316L shows a breakaway oxidation behavior. The oxide layers of LPBF-SS316L and HR-SS316L are mainly composed of Cr2O3, Febased oxides, and spinel phases. In LPBF-SS316L, a uniform Cr depletion region is observed, whereas a Cr depletion region appears at the grain boundary in HR-SS316L. It is evident from the results that the microstructure and the hightemperature oxidation characteristics and behavior are related.
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.
A metallic oxide layer of a heat-resistant element contributes to the high-temperature oxidation resistance by delaying the oxidation and has a positive effect on the increase in electrical resistivity. In this study, green compacts of Fecralloy powder mixed with amorphous and crystalline silica are oxidized at 950oC for up to 210 h in order to evaluate the effect of metal oxide on the oxidation and electrical resistivity. The weight change ratio increases as per a parabolic law, and the increase is larger than that observed for Fecralloy owing to the formation of Fe-Si, Fe-Cr composite oxide, and Al2O3 upon the addition of Si oxide. Si oxides promote the formation of Al2O3 and Cr oxide at the grain boundary, and obstruct neck formation and the growth of Fecralloy particles to ensure stable electrical resistivity.
This study investigates the oxidation properties of Fe-14Cr ferritic oxide-dispersion-strengthened (ODS) steel at various high temperatures (900, 1000, and 1100°C for 24 h). The initial microstructure shows that no clear structural change occurs even under high-temperature heat treatment, and the average measured grain size is 0.4 and 1.1 μm for the as-fabricated and heat-treated specimens, respectively. Y–Ti–O nanoclusters 10–50 nm in size are observed. High-temperature oxidation results show that the weight increases by 0.27 and 0.29 mg/cm2 for the asfabricated and heat-treated (900°C) specimens, and by 0.47 and 0.50 mg/cm2 for the as-fabricated and heat-treated (1000°C) specimens, respectively. Further, after 24 h oxidation tests, the weight increases by 56.50 and 100.60 mg/cm2 for the as-fabricated and heat-treated (1100°C) specimens, respectively; the latter increase is approximately 100 times higher than that at 1000°C. Observation of the surface after the oxidation test shows that Cr2O3 is the main oxide on a specimen tested at 1000°C, whereas Fe2O3 and Fe3O4 phases also form on a specimen tested at 1100°C, where the weight increases rapidly. The high-temperature oxidation behavior of Fe-14Cr ODS steel is confirmed to be dominated by changes in the Cr2O3 layer and generation of Fe-based oxides through evaporation.
In this study, we report the microstructure and the high-temperature oxidation behavior of Fe-Ni alloys by spark plasma sintering. Structural characterization is performed by scanning electron microscopy and X-ray diffraction. The oxidation behavior of Fe-Ni alloys is studied by means of a high-temperature oxidation test at 1000oC in air. The effect of Ni content of Fe-Ni alloys on the microstructure and on the oxidation characteristics is investigated in detail. In the case of Fe-2Ni and Fe-5Ni alloys, the microstructure is a ferrite (α) phase with body centered cubic (BCC) structure, and the microstructure of Fe-10Ni and Fe-20Ni alloys is considered to be a massive martensite (α’) phase with the same BCC structure as that of the ferrite phase. As the Ni content increases, the micro-Vickers hardness of the alloys also increases. It can also be seen that the oxidation resistance is improved by decreasing the thickness of the oxide film.
In order to improve the high-temperature oxidation stability, sintered 434L stainless steel is studied, focusing on the effect of the addition of metallic oxides to form stable oxide films on the inner particle surface. The green compacts of Fecralloy powder or amorphous silica are added on STS434L and oxidized at 950oC up to 210 h. The weight change ratio of 434L with amorphous silica is higher than that of 434L mixed with Fecralloy, and the weight increase follows a parabolic law, which implies that the oxide film grows according to oxide diffusion through the densely formed oxide film. In the case of 434L mixed with Fecralloy, the elements in the matrix diffuse through the grain boundaries and form Al2O3 and Fe-Cr oxides. Stable high temperature corrosion resistance and electrical resistivity are obtained for STS434L mixed with Fecralloy.
Fe-Cr-Al powder porous metal was manufactured by using new electro-spray process. First, ultra-finefecralloy powders were produced by using the submerged electric wire explosion process. Evenly distributed colloid(0.05~0.5% powders) was dispersed on Polyurethane foam through the electro-spray process. And then degreasing andsintering processes were conduced. In order to examine the effect of cell size (200 µm, 450 µm, 500 µm) in process,pre-samples were sintered for two hours at temperature of 1450˚C, in H₂ atmospheres. A 24-hour thermo gravimetricanalysis test was conducted at 1000˚C in a 79% N₂ + 21% O₂ to investigate the high temperature oxidation behavior ofpowder porous metal. The results of the high temperature oxidation tests showed that oxidation resistance increased withincreasing cell size. In the 200 µm porous metal with a thinner strut and larger specific surface area, the depletion ofthe stabilizing elements such as Al and Cr occurred more quickly during the high-temperature oxidation compared withthe 450, 500 µm porous metals.
In this study, analysis on the oxidation behavior was conducted by a series of high-temperature oxidation tests at both 800oC, 900oC and 1000 in the air with sintered STS 316L. The weight gain of each oxidized specimen was measured, the oxidized surface morphologies and composition of oxidation layer were analyzed with Scanning Electron Microscope-Energy Dispersive x-ray Spectroscopy (SEM-EDS), finally, the phase change and composition of the oxidized specimen were shown by X-Ray Diffraction (XRD). As a result, the weight gain increased sharply at 1000oC when oxidation test was conducted for 210 hours. Also, a plentiful of pores were observed in the surface oxidation layers at 900oC for 210 hours. In addition, the following conclusions on oxidation behavior of sintered STS 316L can be obtained: Cr2O3 can be formed on pores by influxing oxygen through open-pores, (Fe0.6Cr0.4)2O3 can be generated on the inner oxidation layer, and Fe2O3 was on the outer oxidation layer. Also, NiFe2O4 could be precipitated if the oxidation time was kept longer.
A new manufacturing process of Fe-Cr-Al powder porous metal was attempted. First, ultra-fine fecralloy powders were produced by using the submerged electric wire explosion process. Evenly distributed colloid (0.05~0.5% powders) was dispersed on PU (Polyurethane) foam through the electrospray process. And then degreasing and sintering processes were conduced. In order to examine the effect of sintering temperature in process, pre-samples were sintered for two hours at temperatures of , , , and , respectively, in atmospheres. A 24-hour TGA (thermo gravimetric analysis) test was conducted at in a 79% +21% to investigate the high temperature oxidation behavior of powder porous metal. The results of the high temperature oxidation tests showed that oxidation resistance increased with increasing sintering temperature (2.57% oxidation weight gain at sintered specimen). The high temperature oxidation mechanism of newly manufactured Fe-Cr-Al powder porous metal was also discussed.
In this paper, high temperature oxidation behavior of newly developed alloys, Ti-6Al-4Fe and Ti-6Al-1Fe, is examined. To understand the effect of Fe on the air oxidation behavior of the Ti-Al-Fe alloy system, thermal oxidation tests are carried out at 700˚C and 800˚C for 96 hours. Ti-6Al-4V alloy is also prepared and tested under the same conditions for comparison with the developed alloys. The oxidation resistance of the Ti-Al-Fe alloy system is superior to that of Ti-6Al-4V alloy. Ti-6Al-4V shows the worst oxidation resistance for all test conditions. This is not a result of the addition of Fe, but rather it is due to the elimination of V, which has deleterious effects on high temperature oxidation. The oxidation of the Ti-Al-Fe alloy system follows the parabolic rate law. At 700˚C, Fe addition does not have a noticeable influence on the amount of weight gain of all specimens. However, at 800˚C, Ti-6Al-4Fe alloy shows remarkable degradation compared to Ti-6Al-1Fe and Ti-6Al. It is discovered that the formation of Al2O3, a diffusion resistance layer, is remarkably hindered by a relative decrease of the α volume fraction. This is because Fe addition increases the volume fraction of β phase within the Ti-6Al-xFe alloy system. Activities of Al, Ti, and Fe with respect to the formation of oxide layers are calculated and analyzed to explore the oxidation mechanism.
This study investigated the high temperature oxidation behavior of Ni-22.4%Fe-22%Cr-6%Al (wt.%) porous metal. Two types of open porous metals with different pore sizes of 30 PPI and 40 PPI (pore per inch) were used. A 24-hour TGA test was conducted at three different temperatures of , and . The results of the BET analysis revealed that the specific surface area increased as the pore size decreased from 30 PPI to 40 PPI. The oxidation resistance of porous metal decreased with decreasing pore size. As the temperature increased, the oxidation weight gain of the porous metal also increased. Porous metals mainly created oxides such as , , , and . In the 40 PPI porous metal with small pore size and larger specific surface area, the depletion of stabilizing elements such as Al and Cr occurred more quickly during oxidation compared to the 30 PPI porous metal. Ni-Fe-Cr-Al porous metal's high-temperature oxidation micro-mechanism was also discussed.
Zirconium diboride (ZrB2) and mixed diboride of (Zr0.7Ta0.3)B2 containing 30 vol.% silicon carbide (SiC) composites were prepared by hot-pressing at 1800˚C. XRD analysis identified the high crystalline metal diboride-SiC composites at 1800˚C. The TaB2 addition to ZrB2-SiC showed a slight peak shift to a higher angle of 2-theta of ZrB2, which confirmed the presence of a homogeneous solid solution. Elastic modulus, hardness and fracture toughness were slightly increased by addition of TaB2. A volatility diagram was calculated to understand the oxidation behavior. Oxidation behavior was investigated at 1500˚C under ambient and low oxygen partial pressure (pO2~10-8 Pa). In an ambient environment, the TaB2 addition to the ZrB2-SiC improved the oxidation resistance over entire range of evaluated temperatures by formation of a less porous oxide layer beneath the surface SiO2. Exposure of metal boride-SiC at low pO2 resulted in active oxidation of SiC due to the high vapor pressure of SiO (g), and, as a result, it produced a porous surface layer. The depth variations of the oxidized layer were measured by SEM. In the ZrB2-SiC composite, the thickness of the reaction layer linearly increased as a function of time and showed active oxidation kinetics. The TaB2 addition to the ZrB2-SiC composite showed improved oxidation resistance with slight deviation from the linearity in depth variation.