Analysis of Plasmon Loss Peaks of Oxides and Semiconductors with the Energy Loss Function.

This paper highlights the use and applications of the energy loss function (ELF) for materials analysis by using electron energy loss spectroscopy (EELS). The basic Drude-Lindhart theory of the ELF is briefly presented along with reference to reflection electron energy loss (REELS) data for several dielectric materials such as insulating high-k binary oxides and semiconductors. Those data and their use are critically discussed. A comparison is made to the available ab initio calculations of the ELF for these materials. Experimental, high-resolution TEM-EELS data on Si, SiC, and CeO2 obtained using a high-resolution, double-Cs-corrected transmission electron microscope are confronted to calculated spectra on the basis of the ELF theory. Values of plasmon energies of these three dielectric materials are quantitatively analyzed on the basis of the simple Drude's free electron theory. The effects of heavy ion irradiation on the TEM-EELS spectra of Si and SiC are addressed. In particular, the downward shifts of plasmon peaks induced by radiation damage and the subsequent amorphization of Si and SiC are discussed. TEM-EELS data of CeO2 are also analyzed with respect to the ELF data and with comparison to isostructural ZrO2 and PuO2 by using the same background and with reference to ab initio calculations.

Assessment of Ferritic ODS Steels Obtained by Laser Additive Manufacturing.

This study aims to assess the potential of Laser Additive Manufacturing (LAM) for the elaboration of Ferritic/Martensitic ODS steels. These materials are usually manufactured by mechanical alloying of powders followed by hot consolidation in a solid state. Two Fe-14Cr-1W ODS powders are considered for this study. The first powder was obtained by mechanical alloying, and the second was through soft mixing of an atomized Fe-14Cr steel powder with yttria nanoparticles. They are representative of the different types of powders that can be used for LAM. The results obtained with the Laser Powder Bed Fusion (LPBF) process are compared to a non-ODS powder and to a conventional ODS material obtained by Hot Isostatic Pressing (HIP). The microstructural and mechanical characterizations show that it is possible to obtain nano-oxides in the material, but their density remains low compared to HIP ODS steels, regardless of the initial powders considered. The ODS obtained by LAM have mechanical properties which remain modest compared to conventional ODS. The current study demonstrated that it is very difficult to obtain F/M ODS grades with the expected characteristics by using LAM processes. Indeed, even if significant progress has been made, the powder melting stage strongly limits, for the moment, the possibility of obtaining fine and dense precipitation of nano-oxides in these steels.

Synthesis of Nano-Oxide Precipitates by Implantation of Ti, Y and O Ions in Fe-10%Cr: Towards an Understanding of Precipitation in Oxide Dispersion-Strengthened (ODS) Steels.

The properties of oxide dispersion-strengthened steels are highly dependent on the nature and size distribution of their constituting nano-oxide precipitates. A fine control of the processes of synthesis would enable the optimization of pertinent properties for use in various energy systems. This control, however, requires knowledge of the precise mechanisms of nucleation and growth of the nanoprecipitates, which are still a matter of debate. In the present study, nano-oxide precipitates were produced via the implantation of Y, Ti, and O ions in two different sequential orders in an Fe-10%Cr matrix that was subsequently thermally annealed. The results show that the oxides that precipitate are not necessarily favoured thermodynamically, but rather result from complex kinetics aspects related to the interaction between the implanted elements and induced defects. When Y is implanted first, the formation of nanoprecipitates with characteristics similar to those in conventionally produced ODS steels, especially with a core/shell structure, is evidenced. In contrast, when implantation starts with Ti, the precipitation of yttria during subsequent high-temperature annealing is totally suppressed, and corundum Cr2O3 precipitates instead. Moreover, the systematic involvement of {110} matrix planes in orientation relationships with the precipitates, independently of the precipitate nature, suggests matrix restriction effects on the early stages of precipitation.

Radiation-Induced Sharpening in Cr-Coated Zirconium Alloy.

To improve the safety of nuclear power plants, a Cr protective layer is deposited on zirconium alloys to enhance oxidation resistance of the nuclear fuel cladding during both in-service and hypothetical accidental transients at High Temperature (HT) in Light Water Reactors. The formation of the Cr2O3 film on the coating surface considerably helps in reducing the oxidation kinetics of the zirconium alloy, especially during hypothetic Loss of Coolant Accident (LOCA). However, if the Cr coating is successful to increase the oxidation resistance at HT of the zirconium substrate, for in-service conditions, under neutron irradiation, Cr desquamation has to be avoided to guarantee a safe use of the Cr-coated zirconium alloys. Therefore, the adhesion properties have to be maintained despite the structural defects created by sustained neutron irradiation in the reactor environment. This paper proposes to study the behavior of the Zircaloy-Cr interface of a first generation Cr-coated material during a specific in situ ion irradiation. As deposited, the Cr-coated sample presents a f.c.c. C15 Laves-type intermetallic phase at the interface with off-stoichiometric composition. After irradiation and for the specific conditions applied, this interfacial phase has significantly dissolved. Energy Dispersion Spectroscopy revealed that the dissolution was accompanied by a counterintuitive "sharpening" effect.

Nano-Structured Materials under Irradiation: Oxide Dispersion-Strengthened Steels.

Oxide dispersion-strengthened materials are reinforced by a (Y, Ti, O) nano-oxide dispersion and thus can be considered as nanostructured materials. In this alloy, most of the nanoprecipitates are (Y, Ti, O) nano-oxides exhibiting a Y2Ti2O7 pyrochlore-like structure. However, the lattice structure of the smallest oxides is difficult to determine, but it is likely to be close to the atomic structure of the host matrix. Designed to serve in extreme environments-i.e., a nuclear power plant-the challenge for ODS steels is to preserve the nano-oxide dispersion under irradiation in order to maintain the excellent creep properties of the alloy in the reactor. Under irradiation, the nano-oxides exhibit different behaviour as a function of the temperature. At low temperature, the nano-oxides tend to dissolve owing to the frequent ballistic ejection of the solute atoms. At medium temperature, the thermal diffusion balances the ballistic dissolution, and the nano-oxides display an apparent stability. At high temperature, the nano-oxides start to coarsen, resulting in an increase in their size and a decrease in their number density. If the small nano-oxides coarsen through a radiation-enhanced Ostwald ripening mechanism, some large oxides disappear to the benefit of the small ones through a radiation-induced inverse Ostwald ripening. In conclusion, it is suggested that, under irradiation, the nano-oxide dispersion prevails over dislocations, grain boundaries and free surfaces to remove the point defects created by irradiation.

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 La 2 Zr 2 O 7 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.