Effect of thermo-mechanical processing on microstructure and creep properties of the foils of alloy 617

The effect of rolling and annealing on the microstructure and high temperature creep properties of alloy 617 were investigated. Two types of foil specimens with different thickness reductions were prepared by thermo-mechanical processing. Recrystallization and grain growth were readily observed at specimens annealed at 950 and 1100 °C. The uniform coarse grains increase resistance against creep deformation. The grain size effect in creep deformation was dominant up to 900 °C, while dynamic recrystallization effect became dominant at 1000 °C. Dynamic recrystallization was observed in all the creep deformed foils, even though some specimens had already been (statically) recrystallized during annealing. Steady state creep rates decreased with increasing annealing temperature in the less rolled foils. The apparent activation energy Q_app for the creep deformation increased from 271 to 361 kJ/mol as the annealing temperature increased from 950 to 1100 °C.     

Effect of swift heavy ion irradiation on spray deposited CdX (X = S, Te) thin films

Cadmium sulfide and cadmium telluride thin films are irradiated with high energy heavy ion beam to study the irradiation induced effects in these films. The polycrystalline thin film samples deposited by spray pyrolysis are irradiated with 60 MeV Oxygen ions using tandem Pelletron accelerator. The X-ray diffraction patterns exhibit a reduction in peak intensities in both CdS and CdTe films. The grain size decrease with fluence is observed for both CdS and CdTe films, with more decrease for CdTe films. The AFM results support this observation. The films show opposite trend in the variation of electrical resistivity with irradiation fluence. A decrease in resistivity is observed for CdS films due to an increase of carrier concentration arising by the creation of sulfur vacancies during the irradiation. The creation of sulfur vacancies is confirmed by XPS studies. The stoichiometric changes seen from XPS studies support this observation. An enhancement of grain boundary scattering due to the reduction of grain size leads to the increase of electrical resistivity for CdTe films.     

Morphology and interface structure of α-Fe2O3 islands grown on sapphire by ion-implantation and annealing

The morphology and interface structure of α-Fe₂O₃ islands grown on α-Al₂O₃ single crystals (sapphire) by Fe-ion-implantation and annealing in an oxidizing atmosphere have been studied using transmission electron microscopy. The α-Fe₂O₃ islands have the orientation relationship of and with sapphire. The typical outline of α-Fe₂O₃ islands consists of two (0 0 0 1) and six planes. The interfaces between α-Fe₂O₃ islands and sapphire are semicoherent, that is coherent regions separated by misfit dislocations at the interfaces. When imaged along the direction, the projected Burgers vector is determined to be . When imaged along the direction, the projected Burgers vector is determined to be . These misfit dislocations form a network structure at the interface to accommodate the mismatch between the lattices of the α-Fe₂O₃ and the α-Al₂O₃.     

Analyzing the effect of displacement rate on radiation-induced segregation in 304 and 316 stainless steels by examining irradiated EBR-II components and samples irradiated with protons

Recent studies have indicated that, at temperatures relevant to fast reactors and light water reactors, void swelling in austenitic alloys progresses more rapidly when the radiation dose rate is lower. A similar dependency between radiation-induced segregation (RIS) and dose rate is theoretically predicted for pure materials and might also be true in complex engineering alloys. Radiation-induced segregation was measured on 304 and 316 stainless steel, irradiated in the EBR-II reactor at temperatures near 375 °C, to determine if the segregation is a strong function of damage rate. The data taken from samples irradiated in EBR-II is also compared to RIS data generated using proton radiation. Although the operational histories of the reactor irradiated samples are complex, making definitive conclusions difficult, the preponderance of the evidence indicates that radiation-induced segregation in 304 and 316 stainless steels is greater at lower displacement rate.     

Grain boundary influence on displacement cascades in UO2: A molecular dynamics study

The influence of grain boundaries on the primary damage state created by a recoil nucleus in UO₂ matrix is studied here by molecular dynamics simulations. This study is divided in two steps: (1) the study of the structural properties of several symmetrical tilt boundaries for different misorientation angles ranging from 12.7° to 61.9°; and (2) the study of displacement cascades near these grain boundaries. For all the grain boundaries studied, the structure around the interface up to about 2 nm presents a perturbed but stable fluorite lattice. The type of defect at the interface depends directly on the value of the misorientation angles. For the small angles (12.7° and 16.3°) the interface defects correspond to edge dislocations. For higher misorientation angles, a gap of about 0.3 nm exists between the two halves of the bicrystal. This gap is composed of Schottky defects involving numerous vacancies along the interface. About 10 keV displacement cascades were initiated with an uranium projectile close to the interface. In all the cases, numerous point defects are created in the grain boundary core, and the mobility of these defects increases. However, cascade morphologies depend strongly on the grain boundary structure. For grain boundaries with edge dislocations, the evolution of the displacement cascades is similar to those carried out in monocrystals. On the other hand, cascades initiated in grain boundaries with vacancy layer defects present an asymmetry on the number of displaced atoms and the number of point defects created.     

Thermal transport properties of uranium dioxide by molecular dynamics simulations

The thermal conductivities of single crystal and polycrystalline UO₂ are calculated using molecular dynamics simulations, with interatomic interactions described by two different potential models. For single crystals, the calculated thermal conductivities are found to be strongly dependent on the size of the simulation cell. However, a scaling analysis shows that the two models predict essentially identical values for the thermal conductivity for infinite system sizes. By contrast, simulations with the two potentials for identical fine polycrystalline structures yield estimated thermal conductivities that differ by a factor of two. We analyze the origin of this difference.     

First-principles investigation of energetics and site preference of He in a W grain boundary

We perform first-principles calculations based on density functional theory to investigate energetics and site preference of He in a bcc-W Σ = 5 grain boundary (GB). The segregation energy is calculated to be −1.37 eV, indicating that He prefers to segregate in the W GB. The formation energy of He in the W GB is positive and thus He is quite hard to dissolve in the W GB, similar to its behavior in the bulk. Because of its closed-shell electronic structure, He is shown to preferably occupy either interstitial or substitutional site with larger space provided by the GB, changing the GB electronic structure. Moreover, segregation of He gives rise to the W GB expansion. These structure variations can have a large effect on the mechanical properties of the W GB.     

First-principles study of helium effect in a ferromagnetic iron grain boundary: Energetics, site preference and segregation

Using a first-principles method based on density functional theory, we have investigated energetics and site preference of helium (He) in a ferromagnetic bcc-iron (Fe) grain boundary (GB). We calculate the binding energies of He atom in the GB, which show that the substitutional He is energetically favored in comparison with the interstitial He with a small energy difference of 0.06 eV. The segregation energy is calculated to be ∼1.4 eV for the energetically favorable GB substitutional and interstitial sites, which is large enough for the He atoms to segregate to these sites, independent of the temperature and the bulk He concentration. This leads to the conclusion that all the He atoms will segregate into the GB at a typical temperature range of 573-1173 K.     

Large molecular dynamics simulations of collision cascades in single-crystal, bi-crystal, and poly-crystal UO2

Classical molecular dynamics simulations have been carried out to study the primary damage due to α-decay self-irradiations in single-, bi-, and poly-crystal UO₂ matrices. In all the cases no amorphization has been found, only the creation of few point defects is observed. However, in all grain boundary systems numerous point defects are created along the interfaces. Furthermore, cascade morphologies depend strongly on the grain boundary structure. For symmetrical tilt grain boundaries with small misorientation angles (lower than 20°) the structure at the grain boundaries is composed of edge dislocations, whereas for higher misorientation angles is formed by Schottky defects. The grain boundary structure in the poly-crystal is found to be highly disordered. For the last two systems, cascades seem stopped by the interfaces unlike those with edge dislocation grain boundaries. These types of interface act like sink which traps moving atoms.     

Multiscale modelling of bi-crystal grain boundaries in bcc iron

Atomistic simulations have provided much insight into grain boundary (GB) structures and mechanisms which are important in understanding the properties of materials. In this paper, the ∑3{1 1 2}, ∑3{1 1 1} and ∑5{0 1 3} (coincidence site lattice) GBs of bcc iron are investigated using molecular statics (MS) simulations, ab initio DFT calculations and the simulated HRTEM method. For the MS calculations, four empirical potentials, the Ackland potential (1997), Mendelev potentials 2 and 4 and the Dudarev-Derlet potential have been used. The MS results for all three symmetrical grain boundaries show the results to be independent of the empirical potential implemented. After relaxation, the symmetrical structures of the GBs remain, in agreement with ab initio calculation results.     

Evolution of the oxide structure of 9CrODS steel exposed to supercritical water

The corrosion behavior and oxide structure of 9CrODS steel in supercritical water has been studied. Samples were exposed to supercritical water at 500 and 600 °C for times of 2, 4 and 6 weeks. The oxide structure was studied using microbeam synchrotron X-ray diffraction and fluorescence analysis. The 600 °C samples exhibited a three-layer structure with Fe₃O₄ in the outer layer, a mixture of FeCr₂O₄ and Fe₃O₄ in the inner layer, and a mixture of metal and oxide grains (FeCr₂O₄ and Cr₂O₃) in the diffusion layer. Between the 2 and 4-week samples exposed to 600 °C supercritical water, a Cr₂O₃ film appeared at the diffusion layer-metal interface which appears to be associated with slower oxidation of the metal. The 500 °C samples also showed a three-layer structure, but both the outer and inner oxide layers contained mainly Fe₃O₄, and the diffusion layer contained much fewer oxide precipitates and was a solid solution of oxygen ahead of the oxide front.     

Towards a more comprehensive microstructural analysis of Zr-2.5Nb pressure tubing using image analysis and electron backscattered diffraction (EBSD)

Zr-2.5Nb pressure tubes used in CANDU (CANada Deuterium Uranium) reactors have a very complex microstructure, with two major crystallographic phases, α and β. These phases include a fair amount of deformation from the extrusion process and the cold working (∼25%) performed at the end of the manufacturing process. This microstructure (texture, grain aspect ratio, etc.) changes along the tube’s length and differs from tube to tube. In order to better understand the deformation mechanisms, these microstructural differences must be statistically characterized. Scanning electron microscopy combined with direct image analysis or with electron backscattered diffraction (EBSD) are good techniques for carrying out such a measurement. However it is not possible, using specimen preparation methods specific for each of these techniques, to reveal all of the grain and phase boundaries. We have thus developed post-treatment algorithms to be able to partially analyze the revealed Zr-2.5Nb microstructure. The first algorithm was used for image analysis treatments of micrographs taken at 5 kV on the radial-tangential plane of etched samples using a reactive ion etch (RIE, CF₄ + O₂). The second was developed for EBSD grain mapping and can be used to characterize α-Zr grain shape and orientation. The two techniques are complementary: EBSD gives information about the micro-texture and the relationship between the microstructure and micro-texture while image analyses of SEM micrographs reveal the direction and distribution of the α-Zr lamellae more easily and over a greater sample area than EBSD. However, the SEM micrographs that were used did not reveal any grain boundary (only phase boundary). An analysis of EBSD grain maps reveals that the average α-Zr grain size, mainly in the elongated direction (tangential), is smaller than what is normally obtained from an image analysis of SEM micrographs. The grain size distribution of type I α-Zr grains (deformed original (prior) α-Zr) and type II (stress-induced β-Zr → α-Zr phase transformation) is also shown to be different for sizes greater than 0.4 μm².     

Plutonium measurements on the 1 MV AMS system at the Centro Nacional de Aceleradores (CNA)

Plutonium isotopes have been recently added to the list of radionuclides that can be measured with the new generation of compact AMS facilities. In this paper we present first experimental results concerning the development of the plutonium AMS technique at 680 kV on the 1 MV AMS system at the Centro Nacional de Aceleradores (CNA) in Sevilla, Spain. This is the first compact AMS machine designed and manufactured by High Voltage Engineering Europa. As we demonstrate, the obtained backgrounds for ^239,240Pu, of about 10⁶ atoms, and the ²³⁹Pu/²³⁸U mass suppression factor, in the range of 10⁻⁹, compare to the ones achieved on other AMS facilities. With the measurement of reference materials provided by the International Atomic Energy Agency (IAEA-375, IAEA-Soil-6, IAEA-381) and samples already studied on the 600 kV compact ETH/PSI AMS system at Zürich, we show that the CNA system can be perfectly used for the routine measurement of plutonium isotopes at environmental levels.     

Breather mechanism of the void ordering in crystals under irradiation

The void ordering has been observed in very different radiation environments ranging from metals to ionic crystals. In the present paper the ordering phenomenon is considered as a consequence of the energy transfer along the close packed directions provided by self-focusing discrete breathers. The self-focusing breathers are energetic, mobile and highly localized lattice excitations that propagate great distances in atomic-chain directions in crystals. This points to the possibility of atoms being ejected from the void surface by the breather-induced mechanism, which is similar to the focuson-induced mechanism of vacancy emission from voids proposed in our previous paper. The main difference between focusons and breathers is that the latter are stable against thermal motion. There is evidence that breathers can occur in various crystals, with path lengths ranging from 10⁴ to 10⁷ unit cells. Since the breather propagating range can be larger than the void spacing, the voids can shield each other from breather fluxes along the close packed directions, which provides a driving force for the void ordering. Namely, the vacancy emission rate for “locally ordered” voids (which have more immediate neighbors along the close packed directions) is smaller than that for the “interstitial” ones, and so they have some advantage in growth. If the void number density is sufficiently high, the competition between them makes the “interstitial” voids shrink away resulting in the void lattice formation. The void ordering is intrinsically connected with a saturation of the void swelling, which is shown to be another important consequence of the breather-induced vacancy emission from voids.     

First-principles study on electronic structures of BaMoO4 crystals containing F and F color centers

The electronic structures of perfect crystals of barium molybdate (BaMoO₄) and of crystals containing F and F⁺ color centers are studied within the framework of the fully relativistic self-consistent Dirac-Slater theory by using the numerically discrete variational (DV-Xα) method. The calculated results suggest that the donor energy level of the F center as well as F⁺ center is located within the band gap. The respective optical transition energies are 1.86 eV and 2.105 eV corresponding to the wavelength of the absorption band of 668 nm and 590 nm. It is therefore suggested that these bands are originate from the F and F⁺ centers in the crystal.     

Atomistic simulation of helium bubble nucleation in palladium

A palladium crystal has been constructed with 11808 atoms. 55 helium atoms occupied the octahedral position of palladium crystal are introduced and retained in a spherical region. Molecular dynamic simulations are performed in a constant temperature and constant volume ensemble (NVT) with temperature controlled by Nose-Hoover thermostat. The interactions between palladium atoms are described with modified analytic embedded atom method (MAEAM), the interactions between palladium atom and helium atom are in the form of Morse potential, and the interactions between helium atoms are in the form of L-J potential function. With the analysis of the radial distribution function (RDF) and microstructure, it reveals that some of helium atoms form a series of clusters with different size, and the nucleation core is random at low temperature, and which is the embryo of helium bubble. Increasing temperature can accelerate the process of bubble nucleation, and the clusters will aggregate and coalesce into a bigger one in which there are no palladium atoms, and it is considered as a helium bubble.     

Cross-section transmission electron microscopy of the ion implantation damage in annealed diamond

It has formerly been shown that low-damage levels, produced during the implantation doping of diamond as a semiconductor, anneal easily while high levels “graphitize” (above about 5.2 × 10¹⁵ ions/cm²). The difference in the defect types and their profiles, in the two cases, has never been directly observed. We have succeeded in using cross-section transmission electron microscopy to do so. The experiments were difficult because the specimens must be polished to ∼40 μm thickness, then implanted on edge and annealed, before final ion beam thinning to electron transparency. The low-damage micrographs reveal some deeply penetrating dislocations, whose existence had been predicted in earlier work.     

Effect of He on the structure and bonding properties of W: A first-principles computational tensile test

Using a first-principles computational tensile test (FPCTT), we have investigated the effect of helium (He) on the structure and bonding properties of tungsten (W), which is a promising plasma-facing material in nuclear fusion Tokamak. Density of states results reveal the underlying reason that the substitutional site for He is the most energetically favorable, while the tetrahedral interstitial site is more favorable than the octahedral interstitial one. The FPCTT shows that the ideal tensile strength is 29.1 GPa at the strain of 14% along the [0 0 1] direction for intrinsic W, while it decreases to 28.2 GPa at the same strain when one impurity He atom is introduced. A local bond-breaking region around He forms in the tensile process due to the presence of He, which suggests He will have a large effect on the bonding properties of W.     

Oxidation behavior of Incoloy 800 under simulated supercritical water conditions

For a correct design of supercritical water-cooled reactor (SCWR) components, data regarding the behavior of candidate materials in supercritical water are necessary. Corrosion has been identified as a critical problem because the high temperature and the oxidative nature of supercritical water may accelerate the corrosion kinetics. The goal of this paper is to investigate the oxidation behavior of Incoloy 800 exposed in autoclaves under supercritical water conditions for up to 1440 h. The exposure conditions (thermal deaerated water, temperatures of 723, 773, 823 and 873 K and a pressure of 25 MPa) have been selected as relevant for a supercritical power plant concept. To investigate the structural changes of the oxide films, X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (EDX) and electrochemical impedance spectroscopy (EIS) analyses were used. Results show changes in the oxides chemical composition, microstructure and thickness versus testing conditions (pressure, temperature and time). The oxide films are composed of two layers: an outer layer enriched in Fe oxide and an inner layer enriched in Cr and Ni oxides corresponding to small cavities supposedly due to internal oxidation.     

Effect of additive ions on the optical density and stability of the color centers induced by X-ray irradiation in soda-lime silicate glass

To apply radiation-induced coloration of glasses as a reversible glass-coloring technique, we studied the influence of various additive ions incorporated into a soda-lime silicate glass on the optical density and stability of the color induced by X-ray irradiation. Absorption spectra before and after irradiation are discussed in the comparison with those of the undoped soda-lime silicate glass. Additive ions were incorporated as metal oxides, namely TiO₂, V₂O₅, Fe₂O₃, ZnO, Ga₂O₃, GeO₂, ZrO₂, Nb₂O₃, MoO₃, Ag₂O, In₂O₃, SnO, SnO₂, CeO₂, Eu₂O₃, Ta₂O₅, WO₃ and Bi₂O₃. Among them, TiO₂, GeO₂, Nb₂O₃, MoO₃, Ag₂O, In₂O₃, Eu₂O₃, Ta₂O₅, WO₃ and Bi₂O₃ have a large effect on optical density. The optical densities in the visible region for glasses doped with these oxides were much stronger than for undoped soda-lime silicate glass. On the other hand, incorporation of Fe₂O₃, SnO and CeO₂ reduced the optical density. Over longer periods the coloration of the undoped glass was one of the most stable while those of the Fe₂O₃, SnO and CeO₂-doped glasses soon faded.