Oxide Dispersion Strengthened FeCrAl Alloys Research Articles

Laser powder bed fusion of oxide dispersion strengthened FeCrAl alloy: Processing and microstructural evolution

Optimizing and regulating the process parameters to form a uniform distribution of nanosized dispersoids remains a major challenge in additive manufacturing oxide dispersion strengthened (ODS) alloys. This study introduces the influence of scanning speed and laser power on the microstructure evolution of laser powder bed fusion (LPBF) ODS FeCrAl alloy. Low laser power and high scanning speed reduce the size of oxide particles and increase their number density. The energy density threshold is 83 J/m3, below which the powder fails to achieve complete melting, leading to the formation of defects during solidification. High density and large number of oxide particles were obtained for the printed samples under the parameters of 140 W laser power and 600 mm/s scanning speed. The average size and number density of oxide particles were ∼ 21.61 nm and ∼ 1.8 × 1020/m3, respectively. High scanning speed have a rapid cooling rate which affects the dislocation density and the average width of the columnar grains. Low laser power significantly weakens the 〈100〉 fiber texture, which is related to the degree of recrystallization in the remelted region. The core-shell oxides consisting of Y-Al-O and Y-Ti-O were distributed in the samples deposited at low and high laser powers, respectively. The formation of core-shell oxide particles in LPBF ODS FeCrAl alloys involves solid-state amorphization and recrystallization. This study can be a guideline to achieve materials with specific microstructure for ODS alloys.

Significant suppression of helium bubbles in oxide dispersion strengthened FeCrAl alloys irradiated by high concentration of helium

Oxide dispersion strengthened (ODS) FeCrAl alloys were successfully fabricated by various mechanical alloying time (10h and 40h), combined with spark plasma sintering (SPS) technique. To understand their helium irradiation resistance, two kinds of ODS FeCrAl alloys were implanted with helium ions at 400 keV in the fluence of 1 × 1021/m2 at 350 °C, 400 °C, and 450 °C to investigate the effect of high concentration helium on the materials in advanced nuclear reactors. The distributions of helium bubbles associated with the microstructural features were characterized by transmission electron microscope (TEM). The experimental results showed that both the helium bubble sizes and volume fractions increased with increasing the irradiation temperatures. The high sink strength of nano-oxides and small inter-oxides distance contributed to the good suppression of helium bubbles growth. In particular, we identified that the high-density nano-oxides with the small sizes (<10 nm) could sequester the helium into several (1–3) tiny bubbles to inhibit bubbles accumulating and coarsening both in elevated temperatures and high helium concentration. Additionally, grain boundaries demonstrated the weaker ability than nano-oxides to disperse helium bubbles, when compared helium irradiation resistance in ODS FeCrAl alloys and FeCrAl alloys. Eventually, ODS FeCrAl alloys in this study revealed the superior helium irradiation resistance than other studied alloys, making it promising to be one of the potential structural materials applicated in advanced nuclear reactors.

Influence of water vapour on the oxidation rate of oxide dispersion strengthened FeCrAl alloys at 1100 °C

Influence of water vapour on the oxidation rate of oxide dispersion strengthened FeCrAl alloys at 1100 °C

In-situ manufacturing of ODS FeCrAlY alloy via laser powder bed fusion

Gas-atomized Fe–24Cr–8Al–0.5Y (wt.%) powder was used as a feedstock in a laser powder bed fusion process with nitrogen atmosphere. Formation of Al–Y–O-enriched nanoparticles with diameters of 10–100 nm implied in-situ precipitation of Al–Y–O-enriched nanoparticles within the ferritic matrix developing an oxide dispersion strengthened FeCrAl alloy without any mechanical alloying. Thermodynamics and kinetics of the internal oxidation during rapid solidification of laser powder bed fusion process are discussed.

Void formation during cyclic oxidation of oxide dispersion strengthened FeCrAl alloys

ABSTRACT Oxide dispersion strengthened FeCrAl alloys are considered for various high-temperature applications due to their excellent mechanical properties and oxidation resistance, but void formation is a concern for component durability. Cyclic oxidation testing was conducted on alloy MA956 and PM2000 at 1100–1200ºC for durations of up to 10,000 h and the void content was determined from optical cross-sections by image analysis. At 1100ºC, 100 h cycle, the low void concentrations measured were consistent with two competing mechanisms proposed in the literature: coalescence of process-induced nano-voids and alloy sintering. At 1200ºC using 1 h cycles, the void concentration was much higher, reaching ~3% to 6% for specimens tested to breakaway oxidation. The void growth was attributed to the high oxidation rates and the annihilation of oxidation-induced vacancies at the surface of the process-induced voids.

Relationships between depth-resolved primary radiation damage, irradiation-induced nanostructure and nanoindentation response of ion-irradiated Fe-Cr and ODS Fe-Cr alloys

• Irradiation-induced loops arise from displacement damage and injected interstitials. • Dislocation loops give rise to depth-dependent hardening. • The depth of maximum hardening and the substrate effect are correctly predicted. • The size of the plastic zone and the superposition rule are varied. • The most appropriate model version is material-specific. Ion irradiations are indispensable for exploring radiation effects on materials, for example, radiation hardening. However, the extraction of radiation hardening as function of displacement damage from the nanoindentation (NI) response of self-ion-irradiated metallic alloys is a challenge. In particular, recent attempts suffer from interference with contributions arising from injected self-interstitial atoms. Moreover, instances of available microstructural evidence and NI results reported for the same material and same irradiation are rare. In order to tackle these issues, the depth-dependent irradiated microstructure and the NI response were analyzed for Fe-9Cr and oxide dispersion strengthened Fe-Cr alloys irradiated with 5 MeV iron ions. Cross-sectional transmission electron microscopy indicated the appearance of irradiation-induced dislocation loops but no other types of visible microstructural changes. NI indicated maxima of the radiation hardening as function of contact depth. Links between the depth-resolved primary radiation damage, the observed depth-dependent characteristics of loops and the measured hardening are considered. As a key point, the link between loops and hardening requires the integration of the local hardening contributions over the indentation plastic zone. Calculations and measurements are compared with respect to both the depth position of maximum hardening and the substrate effect. The role of the model assumptions is discussed with special emphasis on the plastic zone size and the superposition of hardening contributions. The latter is found to be material-specific. The model also allows hardening contributions arising from displacement damage and injected interstitials to be separated.

The effect of Zr on precipitation in oxide dispersion strengthened FeCrAl alloys

Oxide dispersion strengthened (ODS) FeCrAl alloys are promising candidate materials for advanced nuclear reactor applications requiring high-temperature strength, corrosion resistance, and irradiation tolerance. As these alloys have increased in compositional complexity through attempts to use highly reactive elements such as Zr to refine particle sizes and optimize nanoprecipitate dispersion characteristics, much debate has ensued as to the effects of these alloying element additions on alloy properties. In an attempt to reconcile differences in nanoprecipitate distributions reported in the literature over the past decade, a detailed investigation of a recently developed ODS FeCrAl alloy with nominal composition Fe–10Cr-6.1Al-0.3Zr+0.3Y2O3 is presented using a combination of atom probe tomography (APT), scanning/transmission electron microscopy (S/TEM), and computational thermodynamics modeling. It is illustrated that based on the amount of Zr available in the lattice, Zr competes with Al and Cr to form carbides and nitrides as opposed to oxygen-rich precipitates. This alloy system has a high number density (>1023 m−3) of ∼2–4 nm diameter (Y,Al,O)-rich nanoprecipitates, but it is shown that due to the compositional spread and unknown partitioning of Al between the matrix and precipitates, significant challenges still exist for quantifying the exact compositions of these precipitates using APT. However, the noted compositional spread is supported by identified complex oxides yttrium aluminum monoclinic (YAM) and yttrium aluminum garnet (YAG) using S/TEM. As a result of these findings, researchers developing ODS FeCrAl with reactive element additions must pay careful attention to C and N impurities when optimizing reactive element additions.

Characterization of oxide dispersoids and mechanical properties of 14Cr-ODS FeCrAl alloys

Two variants of 14-Cr oxide dispersion strengthened FeCrAl alloys are fabricated by MA method. The morphology, phase and oxide/matrix interface structure of the nano-oxide dispersoids in both alloys are characterized by TEM, HRTEM, TKD and XRD. Almost all the small precipitates in Fe–14Cr-4.5Al–2W-0.4Ti-0.4Y alloy are identified as orthorhombic YAlO3 particles. In Fe–14Cr-4.5Al–2W-0.4Ti-0.3Zr-0.4Y ODS alloy, Y2(Zr0.4Ti0.6)2O7 particle with better coherent relationship with the matrix is found. Almost 23% Y2(Zr0.4Ti0.6)2O7 and YAlO3 particles coexist, resulting in refinement of average diameter of oxide dispersoids and improvement of mechanical strength. Tensile tests from room temperature to 1000 °C demonstrate the attainment of strength-toughness matching in these ODS FeCrAl alloys. The intergranular fracture after the tensile tests at elevated temperature indicates that grain boundary sliding may be the dominant mechanism for deformation.

High temperature properties of AlN coatings deposited by chemical vapor deposition for solar central receivers

There is an increasing interest for tower concentrated solar power (CSP) systems which can work at temperatures higher than 1073 K to optimize the efficiency. One of the challenges is to design the receiver that will be heated at high temperatures in air. On the contrary to coatings in gas turbine engine, the coating/substrate system must have a high thermal conductivity to ensure a good heat transfer to the fluid. Aluminum nitride (AlN) coating, deposited by chemical vapor deposition at 1373 K at a growth rate of 10–50 μm h−1, is selected for its high thermal conductivity, low thermal expansion coefficient, high temperature stability and its ability to develop stable alumina scales above 1273 K. Cast and ODS (Oxide Dispersion Strengthened) FeCrAl alloys, also alumina-formers, are chosen as model substrates to reduce the influencing parameters in real-life receivers and to study the potential of these coatings. Accelerated cyclic oxidation tests and emissivity measurements allow the evaluation of AlN coatings as materials for high temperature CSP receivers. The multilayered systems show low degradation after hundreds of thermal cycles at 1073 K in air and can support higher temperatures (1373 K) for 100 to 500 h depending on the coating thickness. Nevertheless the fast cyclic oxidations in solar furnace generated cracks through the coatings. The measurement of the optical properties also revealed a decrease of the absorptivity after oxidation.

Post-irradiation annealing behaviour of oxide dispersion strengthened Fe-Cr alloys studied by nanoindentation

ABSTRACTTo study the nature of irradiation-induced nanofeatures in oxide dispersion strengthened (ODS) Fe-Cr alloys, post-irradiation isochronal thermal annealing up to 600°C was performed for ODS Fe-9%Cr and Fe-14%Cr alloys ion-irradiated at 300°C and 500°C. Nanoindentation indicated hardening for all as-irradiated alloys and complete hardness recovery upon post-irradiation annealing. Cross-sectional TEM indicated an irradiation-induced defect band near peak damage mainly consisting of dislocation loops. Candidate mechanisms of recovery were critically evaluated. Shrinkage of loops via capture of thermal vacancies was found to correctly reflect the annealing behaviour of ODS Fe-9Cr irradiated at 300°C.

Advanced TEM characterization of oxide nanoparticles in ODS Fe–12Cr–5Al alloys

The oxide nanoparticles present in three oxide-dispersion-strengthened (ODS) Fe–12Cr–5Al alloys containing additions of (1) Y2O3 (125Y), (2) Y2O3 + ZrO2 (125YZ), and (3) Y2O3 + HfO2 (125YH), were investigated using transmission and scanning transmission electron microscopy. In all three alloys nano-sized (<3.5 nm) oxide particles distributed uniformly throughout the microstructure were characterized using advanced electron microscopy techniques. In the 125Y alloy, mainly Al2O3 and yttrium–aluminum garnet (YAG) phases (Y3Al5O12) were present, while in the 125YZ alloy, additional Zr(C,N) precipitates were identified. The 125YH alloy had the most complex precipitation sequence whereby in addition to the YAG and Al2O3 phases, Hf(C,N), Y2Hf2O7, and HfO2 precipitates were also found. The presence of HfO2 was mainly due to the incomplete incorporation of HfO2 powder during mechanical alloying of the 125YH alloy. The alloy having the highest total number density of the oxides, the smallest grain size, and the highest Vickers hardness was the 125YZ alloy indicating, that Y2O3 + ZrO2 additions had the strongest effect on grain size and tensile properties. High-temperature mechanical testing will be addressed in the near future, while irradiation studies are underway to investigate the irradiation resistance of these new ODS FeCrAl alloys.

Grain Boundary Segregation and Core/Shell Structured Nanofeatures in Oxide-Dispersion Strengthened Fe-Cr Alloys

Grain Boundary Segregation and Core/Shell Structured Nanofeatures in Oxide-Dispersion Strengthened Fe-Cr Alloys

Bimodal Grain Size Distribution of Nanostructured Ferritic ODS Fe–Cr Alloys

Oxide dispersion strengthened Fe–Cr alloys produced by mechanical alloying and spark plasma sintering were found to form different heterogeneous hardness distribution and microstructures depending on the milling parameters. Microstructure investigations by means of electron‐diffraction techniques and atom probe tomography revealed the presence of large particle‐free zones in one material, which is, together with the inhomogeneous deformation at short milling times, considered the main reason for the formation of a heterogeneous microstructure. The inhomogeneous temperature distribution in the sample volume during the sintering process is also expected to contribute to the formation of a heterogeneous grain size distribution in the final material.

Development of ODS FeCrAl for Compatibility in Fusion and Fission Energy Applications

Oxide dispersion strengthened (ODS) FeCrAl alloys with 12–15% Cr are being evaluated for improved compatibility with Pb-Li for a fusion energy application and with high temperature steam for a more accident-tolerant light water reactor fuel cladding application. A 12% Cr content alloy showed low mass losses in static Pb-Li at 700°C, where a LiAlO2 surface oxide formed and inhibited dissolution into the liquid metal. All the evaluated compositions formed a protective scale in steam at 1200°C, which is not possible with ODS FeCr alloys. However, most of the compositions were not protective at 1400°C, which is a general and somewhat surprising problem with ODS FeCrAl alloys that is still being studied. More work is needed to optimize the alloy composition, microstructure and oxide dispersion, but initial promising tensile and creep results have been obtained with mixed oxide additions, i.e. Y2O3 with ZrO2, HfO2 or TiO2.

Energetics, structure and composition of nanoclusters in oxide dispersion strengthened Fe–Cr alloys

Extensive first principle calculations on embedded clusters containing few O, Y, Ti and Cr atoms, as well as vacancies, are performed to obtain the interaction parameters to be applied in Metropolis Monte Carlo simulations, within the framework of a rigid lattice model. A novel description using both pair and triple parameters is shown to be more precise than the commonly used pair parameterization. Simulated annealing provides comprehensive data on the energetics, structure and stoichiometry of nanometer-size clusters at T = 0. Additionally, Metropolis Monte Carlo simulations are carried out at high temperature in order to investigate the dependence of nanocluster composition on temperature. The absolute value of the binding energy per O atom unit increases with cluster size and approaches a constant for large clusters. The presence of Ti and/or vacancies increases the value of this quantity. In alloys without vacancies, clusters show a planar structure, whereas the presence of vacancies leads to three-dimensional configurations. Cr is not part of the nanoclusters, except in alloys without Ti but with vacancies. In the latter case, clusters consist of a core containing O, vacancies, as well as Y and a Cr shell, which have also been observed experimentally. A good agreement between the existing experimental data on the ratios (Y + Ti) : O, Y : Ti, (Y + Cr) : O, and Y : Cr and the simulation results is found. The comparison of experimental data with those obtained by simulations demonstrates that the assumption of nanoclusters consisting of nonstoichiometric oxides that are essentially coherent with the bcc lattice of the Fe–Cr matrix leads to reasonable results.

Nanocavity formation and hardness increase by dual ion beam irradiation of oxide dispersion strengthened FeCrAl alloy

Open volume defects generated by ion implantation into oxide dispersion strengthened (ODS) alloy and the related hardness were investigated by positron annihilation spectroscopy and nanoindentation measurements, respectively. Synchronized dual beam implantation of Fe and He ions was performed at room temperature and at moderately enhanced temperature of 300°C. For room temperature implantation a significant hardness increase after irradiation is observed which is more distinctive in heat treated than in as-received ODS alloy. There is also a difference between the simultaneous and sequential implantation mode as the hardening effect for the simultaneously implanted ODS alloy is stronger than for sequential implantation.The comparison of hardness profiles and of the corresponding open volume profiles shows a qualitative agreement between the open volume defects generated on the nanoscopic scale and the macroscopic hardness characteristics.Open volume defects are drastically reduced for performing the simultaneous dual beam irradiation at 300°C which is a more realistic temperature under application aspects. Few remaining defects are clusters of 3–4 vacancies in connection with Y oxide nanoparticles. These defects completely disappear in a shallow layer at the surface. The results are in agreement with hardness measurements showing little hardness increase after irradiation at 300°C.Suitable characteristics of ODS alloy for nuclear applications and the close correlation between He-related open volume defects and the hardness characteristics are verified.

Role of strain heterogeneity on recrystallisation of oxide dispersion strengthened Fe–Cr–Al alloys for high-temperature applications

Mechanically alloyed iron-based oxide dispersion-strengthened alloys have the potential for application in heat exchangers for biomass power plants, with operating temperature and pressure at entry of the gas turbine working fluid being around 1,100 °C and 15–30 bar, respectively. The yttria dispersion in such alloys improves the high-temperature creep and stress rupture life. The strength is further enhanced by the development of a coarse-grained microstructure during recrystallization. Factors controlling the evolution of this desirable microstructure are explored in this study, focusing specifically on PM 2000. The results can be interpreted if it is assumed that anything which makes the microstructure heterogeneous stimulates recrystallization. The combination of these results with finite element modelling is used to interpret the role of strain heterogeneity on the development of recrystallized grain structure. In this sense, larger strain gradients lead to more refined and more isotropic grain structures.

Influence of recrystallization on phase separation kinetics of oxide dispersion strengthened Fe–Cr–Al alloy

The effect of different starting microstructures on the kinetics of Fe-rich (α) and Cr-rich (α′) phase separation during aging of Fe–Cr–Al oxide dispersion strengthened (ODS) alloys has been analyzed with a combination of atom probe tomography and thermoelectric power measurements. The results revealed that the high recrystallization temperature necessary to produce a coarse grained microstructure in Fe-base ODS alloys affects the randomness of Cr-atom distributions and defect density , which consequently affect the phase separation kinetics at low annealing temperatures.

A Study of Nuclear of Interest Martensitic Steels and FeCr ODS Alloys Using Small Angle Neutron Scattering

Small Angle Neutron Scattering (SANS) technique allows to characterize at a nanoscale the microstructure of the ferritic martensitic steels and ODS FeCr alloys which are candidates for the internal structures of future nuclear reactors. Firstly, the microstructure evolution induced by neutron irradiation at high dose in conventional and Reduced Activation Fe9%Cr martensitic steels is presented. Then, a SANS study of Oxide Dispersion Strengthened (ODS) alloys is also presented. The main objective is to control the nano-size oxide particles at the various stages of the fabrication process.

Core/shell structures of oxygen-rich nanofeatures in oxide-dispersion strengthened Fe–Cr alloys

With the significant improvement in high temperature creep properties and resistance to radiation damage by addition of nanoscale oxide features, oxide-dispersion strengthened (ODS) ferritic/martensitic alloys are potential candidates for structural applications in nuclear fusion reactors. The structure of the oxygen-rich nanofeatures was analyzed by atom-probe tomography in three ODS alloys: MA957, ODS Fe–12wt%Cr, and ODS Eurofer-97. Although field evaporation and reconstruction of the precipitates suffer from artefacts, a core/shell structure is found even for very small precipitates. Precipitate cores are Y rich while shell regions are enriched in Ti, Cr, or V depending on alloy composition.