Cr Oxide Dispersion Strengthened Research Articles

Characterization of nano-sized particles in 14%Cr oxide dispersion strengthened (ODS) steel using classical and frontier microscopy methods

Oxide dispersion strengthened (ODS) steels exhibit superior mechanical properties and irradiation resistance due to nano-sized oxides, highly dispersed in the metallic matrix. The mechanical properties are affected by the structure, composition, size and density of the nano-sized oxides. Despite numerous reports on the characterization of these oxides, ambiguity regarding their composition, crystallographic structure and orientation relationship with the matrix remains. In the present study, characterization of the crystallographic structure of oxide particles existing in 14%Cr ODS steel was performed using classical and novel transmission electron microscopy (TEM) methods. 3D dispersion, density and composition of these oxides were evaluated by atom probe tomography (APT). Three populations of particles were detected: highly dispersed, 3–20 nm Fe(Cr,Ti,Y)O particles with spinel structure; 50–150 nm YTiO3 and large (100–200 nm) particles identified as cubic TiC.The spinel-type particles displayed Bain and Kurdjumov-Sachs orientation relationships (OR) with the ferritic matrix. Applying electron diffraction tomography, the YTiO3 structure was attributed to the GdFeO3 (distorted perovskite)-type and its lattice parameters were refined as a = 5.46 Å, b = 7.66 Å and c = 5.28 Å. Orientation relationship of the YTiO3 particles and Fe matrix were determined as [110]Fe//[210]oxide and (110)Fe//(002)oxide.

Understanding plasticity in irradiated alloys through TEM in situ compression pillar tests

Depth-sensing transmission electron microscopic (TEM) in situ mechanical testing has become widely utilized for understanding deformation in irradiated materials. Until now, compression pillars have primarily been used to study the elastic properties and yield of irradiated materials. In this study, we utilize TEM in situ compression pillars to investigate plastic deformation in two ion-irradiated alloys: Fe–9% Cr oxide dispersion strengthened (ODS) alloy and nanocrystalline Cu–24% Ta. We develop an algorithm to automate the extraction of instantaneous pillar dimensions from TEM videos, which we use to calculate true stress–strain curves and strain hardening exponents. True stress–strain curves reveal intermitted plastic flow in all specimen conditions. In the Fe–9% Cr ODS, intermitted plastic flow is linked to strain bursts observed in TEM videos. Low strain hardening or strain softening is observed in all specimen conditions. TEM videos link the strain softening in irradiated Fe–9% Cr ODS to dislocation cross-slip, and in Cu–24% Ta to grain boundary sliding.

Long-term thermal-aging stability of oxide-dispersion-strengthened ferritic steels at 753 K

Oxide-dispersion-strengthened (ODS) ferritic steels are promising candidates for structural applications in the future nuclear reactors. The higher chromium contents of ODS ferritic steels, the better the corrosion resistance, which can meet the harsh corrosion environment of the advanced reactors. However, increasing the Cr content may also lead to the brittleness of the ODS steels when serving at high temperatures. The ODS ferritic steels with different Cr contents (12, 16 and 18 wt% Cr, respectively) were fabricated by mechanical alloying, hot isostatic pressing and forging. Mechanical properties and microstructure evolution of the ODS ferritic steels after aging at 753 K for 2000 h were investigated. It is found that both Vickers hardness and yield strength of 18%Cr ODS ferritic steel were strongly increased and the impact energy was decreased after aging at 753 K. In order to explore the reasons for changes in the mechanical properties, the fracture surfaces were characterized by scanning electron microscopy, and microstructures after aging were observed by transmission electron microscopy. The impact fracture of 18%Cr ODS ferritic steel belongs to quasi-cleavage facture, which is consistent with its very low impact energy. The grain size and dispersed oxide particles of different ODS steels are very stable. M23C6 carbide and M2C carbide were found in 12%Cr ODS steel and 16%Cr ODS steels, respectively.

Fracture Resistance of 14Cr ODS Steel Exposed to a High Temperature Gas

This paper studies the impact fracture behavior of the 14%Cr Oxide Dispersion Strengthened (ODS) steel (ODM401) after high temperature exposures in helium and air in comparison to the as-received state. A steel bar was produced by mechanical alloying and hot-extrusion at 1150 °C. Further, it was cut into small specimens, which were consequently exposed to air or 99.9% helium in a furnace at 720 °C for 500 h. Impact energy transition curves are shifted towards higher temperatures after the gas exposures. The transition temperatures of the exposed states significantly increase in comparison to the as-received steel by about 40 °C in He and 60 °C in the air. Differences are discussed in terms of microstructure, surface and subsurface Scanning Electron Microscope (SEM) and Transmission Electron Microscope (TEM) observations. The embrittlement was explained as temperature and environmental effects resulting in a decrease of dislocation level, slight change of the particle composition and interface/grain boundary segregations, which consequently affected the nucleation of voids leading to the ductile fracture.

The comparison of microstructure and nanocluster evolution in proton and neutron irradiated Fe–9%Cr ODS steel to 3 dpa at 500 °C

A model Fe–9%Cr oxide dispersion strengthened (ODS) steel was irradiated with protons or neutrons to a dose of 3 displacements per atom (dpa) at a temperature of 500 °C, enabling a direct comparison of ion to neutron irradiation effects at otherwise fixed irradiation conditions. The irradiated microstructures were characterized using transmission electron microscopy and atom probe tomography including cluster analysis. Both proton and neutron irradiations produced a comparable void and dislocation loop microstructure. However, the irradiation response of the Ti–Y–O oxide nanoclusters varied. Oxides remained stable under proton irradiation, but exhibited dissolution and an increase in Y:Ti composition ratio under neutron irradiation. Both proton and neutron irradiation also induced varying extents of Si, Ni, and Mn clustering at existing oxide nanoclusters. Protons are able to reproduce the void and loop microstructure of neutron irradiation carried out to the same dose and temperature. However, since nanocluster evolution is controlled by both diffusion and ballistic impacts, protons are rendered unable to reproduce the nanocluster evolution of neutron irradiation at the same dose and temperature.

The microstructure and mechanical properties of Al-containing 9Cr ODS ferritic alloy

In this study, a 9Cr oxide-dispersion strengthened (ODS) alloy with additional corrosion resistant element Al was fabricated by mechanical alloying (MA) and hot pressing (HP) to explore the impact of Al on the microstructure and mechanical property of a 9Cr ODS alloy. It is found that the Al completely dissolved into the Fe–Cr matrix after milling for 30 h. The minor phases in the Al-containing 9Cr ODS ferritic alloy were investigated by a high-energy X-ray, and were identified to be orthorhombic-YAlO3 (YAP), bcc-Y3Al5O12 (YAG), monoclinic-Al2Y4O9 (YAM), and hexagonal-YAlO3 (YAH). These phases were further confirmed by selected area diffraction pattern (SADP), energy dispersive spectroscopy (EDS), and high resolution transmission electron microscopy (HRTEM). In addition, their volume fractions were also calculated from the integrated intensities. According to the analysis of the particles and their formation sequences, the larger particles (greater than 100 nm) are identified as mainly YAG and Al2O3 particles, while the particles with small size (less than 30 nm) are likely primarily YAM, YAH, and YAP particles. The yielding strength (YS) and ultimate tensile strength (UTS) at RT are 563 MPa and 744 MPa, respectively, while the YS and UTS at 700 °C are 245 MPa and 276 MPa, respectively. Although the addition Al in ODS alloys decreases the strength at RT, the values at high temperature are similar to those obtained for 9Cr ODS alloys strengthened by fine Y–Ti–O particles.

On anisotropy of ferritic ODS alloys

Ferritic oxide dispersion strengthened (ODS) alloys are candidate materials to be used as cladding for long term fast reactors, due to their high strength at high temperature and good swelling and irradiation resistances. The fabrication of cladding tubes is usually made by a succession of cold deformation steps where a deformation induced anisotropic microstructure could take place, which would affect the mechanical behaviour of the tube. The characterisation of this microstructural anisotropy is one of the key issues in the development of cladding ODS tubes. In this paper, the microstructural anisotropy of a Fe–14Cr–ODS extruded bar and a Fe–12Cr–ODS plate is characterised and its effect on the mechanical properties is analysed by tensile, impact and small punch testing. In both materials, a reduction of the ductility is observed in the transverse specimens. In addition, the fracture behaviour seems to be strongly dependent on the location of the crack plane regarding the elongated grained microstructure.

Diffusion bonding of 9Cr ODS ferritic/martensitic steel with a phase transformation

Diffusion bonding was employed to join oxide-dispersion-strengthened ferritic/martensitic steel under uniaxial hydrostatic pressure using a high vacuum hot press, and the microstructure and tensile properties of the joints were investigated. 9Cr oxide dispersion strengthened (ODS) steel was successfully diffusion bonded at 1150°C for 1h to migrate a residual bonding interface. Following heat treatment, including normalising at 1050°C and tempering at 800°C for 1h, comparable results without inclusions or micro-voids at the bonding interface, or degradation in the base metal were achieved. Transmission electron microscopy (TEM) observation revealed that the nano-oxide particles in the bonding region were uniformly distributed in the matrix. At room temperature, the joint had nearly the same tensile properties with that of the base metal. The tensile strength of the joint region at elevated temperatures was comparable with that of the base metal. The total elongation of the joint region decreased slightly, but reached 80% of the base metal at 700°C, and a ductile fracture occurred far from the bonding interface. Therefore, it is considered that diffusion bonding with a phase transformation can be a very useful joining method for fabricating components in next-generation nuclear systems using 9Cr ODS ferritic/martensitic steel.

Creep Behavior and Microstructure of 8Cr Oxide Dispersion Strengthened Martensitic Steel

In international thermonuclear experimental reactor (ITER), reduced activation ferritic/martensitic steels will be used for plasma-facing materials. However, it is necessary to raise the temperature of operation in order to elevate efficiency of electric power generation by using the material which is more excellent in strength at elevated temperature. Oxide dispersion strengthened (ODS) steels are promising candidate for high temperature materials of a nuclear fusion reactor. There are many reports that ODS steels show very high creep strength, but there are few reports on creep deformation mechanism. In this work, creep deformation behavior of 8 wt% Cr ODS steel was investigated. This ODS steel had high density of fine dispersed Y2Ti2O7 particles and -ferrite grains elongated along the hot-rolling direction. The creep curve showed a low creep strain rate until specimen ruptured. Vickers hardness of the gauge part of specimens in interrupted creep tests decreased with increasing the loading time. However, that of the grip part did not change significantly. Accordingly, although dynamic recovery occurred in the ODS steel, it had not affected the creep deformation rate.

Microstructural examination of oxide layers formed on an oxide dispersion strengthened ferritic steel exposed to supercritical water

A transmission electron microscopy study was carried out on the oxide layers formed on a 9Cr oxide dispersion strengthened (ODS) ferritic steel after exposure to supercritical water at 500 °C with a 25 ppb dissolved oxygen concentration. Compared with the oxide layers formed on a conventional 9Cr steel NF616 ferritic steel with a similar major element composition and exposed to similar test conditions, the 9Cr ODS steel exhibited a different oxide structural morphology and growth mechanism. The most pronounced difference was the development of a substantially thick internal oxidation layer for the ODS steel that is associated with its finer grain size. For the oxidized ODS steel, yttrium and chromium rich oxide ribbons formed at the steel grain boundaries in the internal oxidation layer. The improved overall corrosion resistance of 9Cr ODS steel at elevated temperatures, as measured by weight gain data, may be a result of yttrium acting as a barrier for cation diffusion along oxide/metal grain boundaries. The gradual decrease in scale density with increasing exposure times appears to be caused by depletion of iron, which resulted in more vacancies and pores in the inner (FeCr) 3O 4 spinel layer.