Oxide dispersion-strengthened (ODS) steel has excellent high-temperature properties, corrosion resistance, and oxidation resistance, and is expected to be applicable in various fields. Recently, various studies on mechanical alloying (MA) have been conducted for the dispersion of oxide particles in ODS steel with a high number density. In this study, ODS steel is manufactured by introducing a complex milling process in which planetary ball milling, cryogenic ball milling, and drum ball milling are sequentially performed, and the microstructure and high-temperature mechanical properties of the ODS steel are investigated. The microstructure observation revealed that the structure is stretched in the extrusion direction, even after the heat treatment. In addition, transmission electron microscopy (TEM) analysis confirmed the presence of oxide particles in the range of 5 to 10 nm. As a result of the room-temperature and high-temperature compression tests, the yield strengths were measured as 1430, 1388, 418, and 163 MPa at 25, 500, 700, and 900oC, respectively. Based on these results, the correlation between the microstructure and mechanical properties of ODS steel manufactured using the composite milling process is also discussed.
In this study, the effects of Co content on the microstructure and Charpy impact properties of Fe-Cr-W ferritic/martensitic oxide dispersion strengthened (F/M ODS) steels are investigated. F/M ODS steels with 0–5 wt% Co are fabricated by mechanical alloying, followed by hot isostatic pressing, hot-rolling, and normalizing/tempering heat treatment. All the steels commonly exhibit two-phase microstructures consisting of ferrite and tempered martensite. The volume fraction of ferrite increases with the increase in the Co content, since the Co element considerably lowers the hardenability of the F/M ODS steel. Despite the lowest volume fraction of tempered martensite, the F/M ODS steel with 5 wt% Co shows the highest micro-Vickers hardness, owing to the solid solution-hardening effect of the alloyed Co. The high hardness of the steel improves the resistance to fracture initiation, thereby resulting in the enhanced fracture initiation energy in a Charpy impact test at – 40oC. Furthermore, the addition of Co suppresses the formation of coarse oxide inclusions in the F/M ODS steel, while simultaneously providing a high resistance to fracture propagation. Owing to these combined effects of Co, the Charpy impact energy of the F/M ODS steel increases gradually with the increase in the Co content.
Ni-based oxide dispersion strengthened (ODS) alloys have a higher usable temperature and better hightemperature mechanical properties than conventional superalloys. They are therefore being explored for applications in various fields such as those of aerospace and gas turbines. In general, ODS alloys are manufactured from alloy powders by mechanical alloying of element powders. However, our research team produces alloy powders in which the Ni5Y intermetallic phase is formed by an atomizing process. In this study, mechanical alloying was performed using a planetary mill to analyze the milling behavior of Ni-based oxide dispersions strengthened alloy powder in which the Ni5Y is the intermetallic phase. As the milling time increased, the Ni5Y intermetallic phase was refined. These results are confirmed by SEM and EPMA analysis on microstructure. In addition, it is confirmed that as the milling increased, the mechanical properties of Ni-based ODS alloy powder improve due to grain refinement by plastic deformation.
This study investigates the directional recrystallization behavior of Ni based oxide dispersion strengthened (ODS) alloy according to the zone annealing velocity. The zone annealing temperature is set as 1390oC, while the zone velocities are set as 2.5, 4, 6, and 10 cm/h, respectively. The initial microstructure observation of the as-extruded sample shows equiaxed grains of random orientation, with an average grain size of 530 nm. On the other hand, the zone annealed samples show a large deviation in grain size depending on the zone velocities. In particular, grains with a size of several millimeters are observed at 2.5-cm/h zone velocity. It is also found that the preferred orientation varies with the zone annealing velocity. On the basis of these results, this study discusses the role of zone velocities in the directional recrystallization of Ni base ODS alloy.
This study is conducted as a preliminary research to verify the feasibility of Ti-based Oxide dispersion strengthened (ODS) alloy. Pure-Ti powder is mixed with Y2O3 powder and subsequently, mechanically alloyed at -150oC. The Ti-based ODS powder is hot-isostatically pressed and subsequently hot-rolled for recrystallization. The microstructure consists of elongated grains and Y excess fine particles. The oxide particle size is larger than that of the typical Febased ODS steel. Tensile test shows that the tensile ductility is approximately 25%, while the strength is significantly higher than that of pure Ti. The high-temperature hardness of the Ti-ODS alloy is also significantly higher than that of pure Ti at all temperatures, while being lower than that of Ti-6Al-4V. The dimple structure is well developed, and no evidence of cleavage fracture surface is observed in the fracture surface of the tensile specimen.
In order to expand the application of oxide dispersion-strengthened (ODS) steel, a composite material is manufactured by adding mechanically alloyed ODS steel powder to conventional steel and investigated in terms of microstructure and wear properties. For comparison, a commercial automobile part material is also tested. Initial microstructural observations confirm that the composite material with added ODS steel contains i) a pearlitic Fe matrix area and ii) an area with Cr-based carbides and ODS steel particles in the form of a Fe-Fe3C structure. In the commercial material, various hard Co-, Fe-Mo-, and Cr-based particles are present in a pearlitic Fe matrix. Wear testing using the VSR engine simulation wear test confirms that the seatface widths of the composite material with added ODS steel and the commercial material are increased by 24% and 47%, respectively, with wear depths of 0.05 mm and 0.1 mm, respectively. The ODS steel-added composite material shows better wear resistance. Post-wear-testing surface and cross-sectional observations show that particles in the commercial material easily fall off, while the ODS steel-added material has an even, smooth wear surface.
An optimum route to fabricate oxide dispersion strengthened ferritic superalloy with desired microstructure was investigated. Two methods of high energy ball milling or polymeric additive solution route for developing a uniform dispersion of Y2O3 particles in Fe-Cr-Al-Ti alloy powders were compared on the basis of the resulting microstructures. Microstructural observation revealed that the crystalline size of Fe decreased with increases in milling time, to values of about 15-20 nm, and that an FeCr alloy phase was formed. SEM and TEM analyses of the alloy powders fabricated by solution route using yttrium nitrate and polyvinyl alcohol showed that the nano-sized Y-oxide particles were well distributed in the Fe based alloy powders. The prepared powders were sintered at 1000 and 1100 oC for 30 min in vacuum. The sintered specimen with heat treatment before spark plasma sintering at 1100 oC showed a more homogeneous microstructure. In the case of sintering at 1100 oC, the alloys exhibited densified microstructure and the formation of large reaction phases due to oxidation of Al.
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.
Dispersion-strengthened copper with was produced by ball-milling and spark plasma sintering (SPS).Ball-milling was performed at a rotation speed of 300rpm for 30 and 60min in Ar atmosphere by using a planetary ball mill (AGO-2). Spark-plasma sintering was carried out at for 5min under vacuum after mechanical alloying. The hardness of the specimens sintered using powder ball milled for 60min at 300rpm increased from 16.0 to 61.8 HRB than that of specimen using powder mixed with a turbular mixer, while the electrical conductivity varied from 93.40% to 83.34%IACS. In the case of milled powder, hardness increased as milling time increased, while the electrical conductivity decreased. On the other hand, hardness decreased with increasing sintering temperature, but the electrical conductiviey increased slightly
Ultra-fine grained and dispersion-strengthened titanium materials (Ti-Si, Ti-C, Ti-Si-C) have been produced by high energy ball milling and spark plasma sintering (SPS). Silicon or/and carbon were milled together with the titanium powder to form nanometer-sized and homogeneously distributed titanium silicides or/and carbides as dispersoids, that should prevent grain coarsening during the SPS compaction and contribute to strengthening of the material. The microstructures and the mechanical properties showed that strength, hardness and wear resistance of the sintered materials have been significantly improved by the mechanisms of grain refinement and dispersion strengthening. The use of an organic fluid as carrier of the dispersoid forming elements caused a significant increase in ductility.
The alumina dispersion-strengthened (DS) C15715 Cu alloy fabricated by a powder metallurgy route was annealed at temperatures ranging from in the air and in vacuum. The effect of the annealing on microstructural stability and room-temperature mechanical properties of the alloy was investigated. The microstructure of the cold rolled OS alloy remained stable until the annealing at in the air and in vacuum. No recrystallization of original grains occurred, but the dislocation density decreased and newly formed subgrains were observed. The alloy annealed at in the air experienced recrystallization and grain growth took place, however annealing in vacuum at did not cause the microstructural change. The mechanical property of the alloy was changed slightly with the annealing if the microstructure remained stable. However, the strength of the specimen that was recrystallized decreased drastically.