J. Ribis

Electron irradiation-enhanced core/shell organization of Al(Cr, Fe, Mn)Si dispersoids in Al–Mg–Si alloys

The age hardening 6061-T6 aluminium alloy has been chosen as structural material for the core vessel of the material testing Jules Horowitz nuclear reactor. The alloy contains incoherent Al(Cr, Fe, Mn)Si dispersoids whose characterization by energy-filtered transmission electron microscopy (EFTEM) analysis shows a core/shell organization tendency where the core is (Mn, Fe) rich, and the shell is Cr rich. The present work studies the stability of this organization under irradiation. TEM characterization on the same particles, before and after 1 MeV electron irradiation, reveals that the core/shell organization is enhanced after irradiation. It is proposed that the high level of point defects, created by irradiation, ensures a radiation-enhanced diffusion process favourable to the unmixing forces between (Fe, Mn) and Cr. Shell formation may result in the low-energy interface segregation of Cr atoms within the (Fe, Mn) system combined with the unmixing of Cr, Fe and Mn components.

The feasibility of Al-based oxide precipitation in Fe–10%Cr alloy by ion implantation

This paper reports the feasibility of nano-oxide precipitate formation in Fe–Cr alloy by ion implantation synthesis. High contents of Al+ and O+ ions were implanted into thin films of high purity Fe–10%Cr alloy at room temperature and were studied by transmission electron microscopy (TEM) and atom probe tomography (APT). In contrast, to the common two-stage implantation/annealing scheme of precipitate ensemble synthesis by ion beams, cluster formation took place at the implantation stage in our study, requiring no subsequent high-temperature annealing. The post-implantation microstructural examination revealed in the as-implanted thin foil an array of precipitates with diameters in the range of 3–30 nm. The precipitate number density distribution was found to depend on the foil thickness. The precipitate enrichment with both Al and O was confirmed by the energy-filtered TEM analysis. Judging from the electron diffraction pattern and high-resolution TEM analysis, the crystal lattice of precipitates corresponds to some cubic modification of aluminium-rich oxide or pure aluminium oxide. The precipitate lattice alignment with the host matrix was revealed for at least a part of precipitates. The analysis of APT data using cluster detection algorithm indicates the presence of local zones enriched in Al and O, even in those areas of as-implanted samples where no clusters were visible by TEM.

Intricate disorder in defect fluorite/pyrochlore: a concord of chemistry and crystallography

Intuitively scientists accept that order can emerge from disorder and a significant amount of effort has been devoted over many years to demonstrate this. In metallic alloys and oxides, disorder at the atomic scale is the result of occupation at equivalent atomic positions by different atoms which leads to the material exhibiting a fully random or modulated scattering pattern. This arrangement has a substantial influence on the material’s properties, for example ionic conductivity. However it is generally accepted that oxides, such as defect fluorite as used for nuclear waste immobilization matrices and fuel cells, are the result of disorder at the atomic scale. To investigate how order at the atomic scale induces disorder at a larger scale length, we have applied different techniques to study the atomic composition of a homogeneous La2Zr2O7 pyrochlore, a textbook example of such a structure. Here we demonstrate that a pyrochlore, which is considered to be defect fluorite, is the result of intricate disorder due to a random distribution of fully ordered nano-domains. Our investigation provides new insight into the order disorder transformations in complex materials with regards to domain formation, resulting in a concord of chemistry with crystallography illustrating that order can induce disorder.

Identification of monoclinic θ-phase dispersoids in a 6061 aluminium alloy

Abstract Intermetallic dispersoids play an important role in controlling the 6xxx alloy series’ grain distribution and increasing the alloy’s toughness. The dispersoid distribution in a 6061 aluminium alloy (Al–Mg–Si) was analysed by transmission electron microscopy, selected area diffraction and energy-dispersive X-ray spectroscopy. The dispersoids had three unique crystal structures: simple cubic , body-centred cubic and monoclinic (C2/m). While the SC and BCC dispersoids have been well characterized in the literature, a detailed analysis of monoclinic dispersoids has not been presented. Therefore, the current work discusses the chemical composition, crystal structure and morphology of the monoclinic dispersoids.

Atomic-scale interface structure of a Cr-coated Zircaloy-4 material

Highly adherent, thin Cr coatings on Zr-based nuclear fuel claddings can be potentially used for the development of accident-tolerant fuels in light water reactors. To guarantee the successful implementation of Cr-coated Zr alloys as cladding tubes in nuclear power plants, the adhesive strength of the Cr coatings must be assessed. The interface between Cr and Zr was characterized via high-resolution transmission electron microscopy. We observed the formation of nanometer-thick Zr(Fe, Cr)2 poly-type, structured Laves phases at the interfacial region that display both C14 and C15 lattice symmetries. Although the crystallinity was preserved throughout the interfacial region, different atomic configurations were observed for all the interfaces studied. In most cases, coherent or semicoherent crystallographic relationships were observed, ensuring the adhesive strength of the coating.

Oxide dispersion-strengthened/ferrite-martensite steels as core materials for Generation IV nuclear reactors

Abstract Oxide dispersion-strengthened (ODS) steels are the most promising candidate materials for fuel cladding of Generation IV nuclear reactors. The progress and current status for development of ODS/F-M (ferrite-martensite) steels conducted mainly in Japan and France are overviewed. Fabrication routes of cladding tube are mentioned for ferrite-type ODS steels using a recrystallized process and a martensite-type one using α-γ phase transformation. The optimized process is identical for both countries. The joining process between cladding and end-plug has also been developed by using the pressurized resistance upset welding method. The improvements brought by ODS/FM steels in high-temperature strength and irradiation resistance are verified. Finally, the different environmental effects on the ODS behavior, including irradiation, are reviewed.

Thermal annealing behavior of nano-size metal-oxide particles synthesized by ion implantation in Fe-Cr alloy

Oxide dispersion strengthened (ODS) steels are promising structural materials for the next generation nuclear reactors, as well as fusion facilities. The detailed understanding of the mechanisms involved in the precipitation of nano-oxides during ODS steel production would strongly contribute to the improvement of the mechanical properties and the optimization of manufacturing of ODS steels, with a potentially strong economic impact for their industrialization. A useful tool for the experimental study of nano-oxide precipitation is ion implantation, a technique that is widely used to synthesize precipitate nanostructures in well-controlled conditions. Earlier, we have demonstrated the feasibility of synthesizing aluminum-oxide particles in the high purity Fe-10Cr alloy by consecutive implantation with Al and O ions at room temperature. This paper describes the effects of high-temperature annealing after the ion implantation stage on the development of the aluminum based oxide nanoparticle system. Using tr...

Radiation-induced cavities in aluminium alloy imaged by in line electron holography

Abstract In irradiated material, cavities result from the condensation of vacancies induced by collision cascades. The study of their formation is a relevant topic since a high density of cavities may alter significantly the material performance. In this work, a simplified version of in line holography was successfully applied for imaging cavities in ion-irradiated 6061 aluminium alloy. In transmission electron microscopy, the incoming electrons experience a phase shift owing to the potential variation induced by the cavities. The retrieval of this phase shift provides a convenient map to observe and highlight the cavities. Information on density of cavities can be easily obtained. In addition, interstitial clusters may also be detected.