Atomistic calculations of interface elastic properties in noncoherent metallic bilayers

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mi Changwen; Jun, Sukky; Kouris, Demitris A.

2008-02-15

The paper describes theoretical and computational studies associated with the interface elastic properties of noncoherent metallic bicrystals. Analytical forms of interface energy, interface stresses, and interface elastic constants are derived in terms of interatomic potential functions. Embedded-atom method potentials are then incorporated into the model to compute these excess thermodynamics variables, using energy minimization in a parallel computing environment. The proposed model is validated by calculating surface thermodynamic variables and comparing them with preexisting data. Next, the interface elastic properties of several fcc-fcc bicrystals are computed. The excess energies and stresses of interfaces are smaller than those on free surfacesmore » of the same crystal orientations. In addition, no negative values of interface stresses are observed. Current results can be applied to various heterogeneous materials where interfaces assume a prominent role in the systems' mechanical behavior.« less

Surface diffusivity measurements on 8mol.% yttrium oxide-zirconia bicrystals via grain boundary grooving experiments

NASA Astrophysics Data System (ADS)

Nassirou, Maissarath

Thermal grooving at grain boundaries (GBs) is a capillary-driven evolution of surface topography in the region where the grain boundary emerges at a free surface. The study of these topographic changes can provide insight into surface energetics, and in our particular case, the measurement of surface diffusivity. We have measured the surface diffusion coefficient of 8mol% Y 2O3-ZrO2 by studying the formation of thermal grooves. We studied a total of five bicrystals, with well defined orientation relationships; random [110] -60°, random [001] -30°, Sigma13 [001]/{510}, Sigma13 [001]/{320}, Sigma5 [001]/{210}. Our calculations employed the Herring relation (1951), in which the variation in the chemical potential is related to changes in topography. The samples were annealed at 1300°C and 1400°C for various period of time. Atomic Force Microscopy was used to determine the exact geometry of the thermal grooves. A first approach consisted of estimating the diffusion coefficient by using Mullins' equation. yx=0= dsDs1/ 4gb2g s12G 5/4( WkTgs) 1/4t 1/4 Where y(x =0) is the groove depth at the GB triple junction, O is the atomic volume, gs is the surface tension, gb is the grain boundary surface energy, ds is the thickness of the diffusion layer, t is the annealing time, and Ds is the surface diffusion coefficient. In Mullins' derivation, the atomic structure of the surface was ignored and it was assumed that the surface energy is independent of crystallographic orientation. In the case of zirconia, the surface energy is anisotropic. We will describe in this work a new approach to measuring surface diffusivity which accounts for the surface energy anisotropy. The study of these bicrystals will emphasize the effect of grain boundary structure on the surface diffusion coefficient, and it is for that purpose that we selected bicrystals with different tilt axes and angles. The results obtained using the equation set we have developed will be compared to those obtained by Mullins, and we show that the anisotropic groove evolution, even when perfectly symmetrical, is much slower than the corresponding isotropic case.

Effect of grain boundaries on shock-induced phase transformation in iron bicrystals

NASA Astrophysics Data System (ADS)

Zhang, Xueyang; Wang, Kun; Zhu, Wenjun; Chen, Jun; Cai, Mengqiu; Xiao, Shifang; Deng, Huiqiu; Hu, Wangyu

2018-01-01

Non-equilibrium molecular-dynamic simulations with a modified analytic embedded-atom model potential have been performed to investigate the effect of three kinds of grain boundaries (GBs) on the martensitic transformation in iron bicrystals with three different GBs under shock loadings. Our results show that the phase transition was influenced by the GBs. All three GBs provide a nucleation site for the α → ɛ transformation in samples shock-loaded with up = 0.5 km/s, and in particular, the elastic wave can induce the phase transformation at Σ3 ⟨110⟩ twist GB, which indicates that the phase transformation can occur at Σ3 ⟨110⟩ twist GB with a much lower pressure. The effect of GBs on the stress assisted transformation (SAT) mechanisms is discussed. All variants nucleating at the vicinity of these GBs meet the maximum strain work (MSW) criterion. Moreover, all of the variants with the MSW nucleate at Σ5 ⟨001⟩ twist GB and Σ3 ⟨110⟩ tilt GB, but only part of them nucleate at Σ3 ⟨110⟩ twist GB. This is because the coincident planes between both sides of the GB would affect the slip process, which is the second stage of the martensitic transformation and influences the selection of variant. We also find that the martensitic transformation at the front end of the bicrystals would give rise to stress attenuation in samples shock-loaded with up = 0.6 km/s, which makes the GBs seem to be unfavorable to the martensitic transformation. Our findings have the potential to affect the interface engineering and material design under high pressure conditions.

Atomic and electronic structure of Lomer dislocations at CdTe bicrystal interface

PubMed Central

Sun, Ce; Paulauskas, Tadas; Sen, Fatih G.; Lian, Guoda; Wang, Jinguo; Buurma, Christopher; Chan, Maria K. Y.; Klie, Robert F.; Kim, Moon J.

2016-01-01

Extended defects are of considerable importance in determining the electronic properties of semiconductors, especially in photovoltaics (PVs), due to their effects on electron-hole recombination. We employ model systems to study the effects of dislocations in CdTe by constructing grain boundaries using wafer bonding. Atomic-resolution scanning transmission electron microscopy (STEM) of a [1–10]/(110) 4.8° tilt grain boundary reveals that the interface is composed of three distinct types of Lomer dislocations. Geometrical phase analysis is used to map strain fields, while STEM and density functional theory (DFT) modeling determine the atomic structure at the interface. The electronic structure of the dislocation cores calculated using DFT shows significant mid-gap states and different charge-channeling tendencies. Cl-doping is shown to reduce the midgap states, while maintaining the charge separation effects. This report offers novel avenues for exploring grain boundary effects in CdTe-based solar cells by fabricating controlled bicrystal interfaces and systematic atomic-scale analysis. PMID:27255415

Measurement of the cleavage energy of graphite

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Wen; Dai, Shuyang; Li, Xide

Here, the basal plane cleavage energy (CE) of graphite is a key material parameter for understanding many of the unusual properties of graphite, graphene and carbon nanotubes. Nonetheless, a wide range of values for the CE has been reported and no consensus has yet emerged. Here we report the first direct, accurate experimental measurement of the CE of graphite using a novel method based on the self-retraction phenomenon in graphite. The measured value, 0.37±0.01 J m –2 for the incommensurate state of bicrystal graphite, is nearly invariant with respect to temperature (22 °C≤T≤198 °C) and bicrystal twist angle, and insensitivemore » to impurities from the atmosphere. The CE for the ideal ABAB graphite stacking, 0.39±0.02 J m –2, is calculated based on a combination of the measured CE and a theoretical calculation. These experimental measurements are also ideal for use in evaluating the efficacy of competing theoretical approaches.« less

Measurement of the cleavage energy of graphite

DOE PAGES

Wang, Wen; Dai, Shuyang; Li, Xide; ...

2015-08-28

Here, the basal plane cleavage energy (CE) of graphite is a key material parameter for understanding many of the unusual properties of graphite, graphene and carbon nanotubes. Nonetheless, a wide range of values for the CE has been reported and no consensus has yet emerged. Here we report the first direct, accurate experimental measurement of the CE of graphite using a novel method based on the self-retraction phenomenon in graphite. The measured value, 0.37±0.01 J m –2 for the incommensurate state of bicrystal graphite, is nearly invariant with respect to temperature (22 °C≤T≤198 °C) and bicrystal twist angle, and insensitivemore » to impurities from the atmosphere. The CE for the ideal ABAB graphite stacking, 0.39±0.02 J m –2, is calculated based on a combination of the measured CE and a theoretical calculation. These experimental measurements are also ideal for use in evaluating the efficacy of competing theoretical approaches.« less

A hierarchical dislocation-grain boundary interaction model based on 3D discrete dislocation dynamics and molecular dynamics

NASA Astrophysics Data System (ADS)

Gao, Yuan; Zhuang, Zhuo; You, XiaoChuan

2011-04-01

We develop a new hierarchical dislocation-grain boundary (GB) interaction model to predict the mechanical behavior of polycrystalline metals at micro and submicro scales by coupling 3D Discrete Dislocation Dynamics (DDD) simulation with the Molecular Dynamics (MD) simulation. At the microscales, the DDD simulations are responsible for capturing the evolution of dislocation structures; at the nanoscales, the MD simulations are responsible for obtaining the GB energy and ISF energy which are then transferred hierarchically to the DDD level. In the present model, four kinds of dislocation-GB interactions, i.e. transmission, absorption, re-emission and reflection, are all considered. By this methodology, the compression of a Cu micro-sized bi-crystal pillar is studied. We investigate the characteristic mechanical behavior of the bi-crystal compared with that of the single-crystal. Moreover, the comparison between the present penetrable model of GB and the conventional impenetrable model also shows the accuracy and efficiency of the present model.

Atomic and electronic structure of Lomer dislocations at CdTe bicrystal interface

DOE PAGES

Sun, Ce; Paulauskas, Tadas; Sen, Fatih G.; ...

2016-06-03

Extended defects are of considerable importance in determining the electronic properties of semiconductors, especially in photovoltaics (PVs), due to their effects on electron-hole recombination. We employ model systems to study the effects of dislocations in CdTe by constructing grain boundaries using wafer bonding. Atomic-resolution scanning transmission electron microscopy (STEM) of a [1–10]/ (110) 4.8° tilt grain boundary reveals that the interface is composed of three distinct types of Lomer dislocations. Geometrical phase analysis is used to map strain fields, while STEM and density functional theory (DFT) modeling determine the atomic structure at the interface. The electronic structure of the dislocationmore » cores calculated using DFT shows significant mid-gap states and different charge-channeling tendencies. Cl-doping is shown to reduce the midgap states, while maintaining the charge separation effects. In conclusion, this report offers novel avenues for exploring grain boundary effects in CdTe-based solar cells by fabricating controlled bicrystal interfaces and systematic atomic-scale analysis.« less

The effect of low angle boundary misorientation on creep deformation in the superalloy CM 247 LC

NASA Astrophysics Data System (ADS)

Kirsch, Mathew

The effect of low angle boundary misorientation on the creep properties of superalloy CM 247LC bicrystals has been investigated in the medium temperature - medium stress creep regime. Constant load tensile creep tests were performed on mixed Low Angle Boundary (LAB) samples with misorientations ranging from 3o-16o; the LABs where the boundaries were oriented approximately transverse to the tensile axis. Five repeats of each LAB sample were ruptured with an initial stress of 300 MPa and three repeats of each LAB sample were ruptured with an initial stress of 200 MPa, both at 950°C. A drastic decrease in creep rupture life and strain to failure was observed in bicrystals with misorientations greater than ˜10°. Fractography of the fracture surfaces indicated that a transition from ductile transgranular fracture to intergranular fracture coincided with the decrease in creep properties. The decrease in strain to failure was correlated to a decrease in the slip compatibility factor m'. Specimens of several misorientations were also interrupted prior to failure at strains of 2%, 5% and 10% and examined by electron microscopy techniques in an effort to better understand the sequences leading to failure. For samples that fractured intergranularly, voids formed adjacent to large MC carbides located at the LABs and propagated along the boundary, ultimately linking to cracks that initiated at the specimen edge. Electron Back Scattered Diffraction (EBSD) scans were performed and Crystal reference Orientation (CO) maps were generated from the partially crept specimens. An increase in misorientation from the crystal reference orientation was observed with increasing LAB misorientation for a given interrupted strain level indicative of the poorer slip compatibility at the higher misorientations Two bicrystals with nearly identical scalar misorientation, both ˜10°, exhibited surprisingly different behavior with one failing intergranularly at low strain to failure and the other failing transgranularly at high strain to failure; these differences were related to the different slip compatibilities as determined by an analysis of the nature of their misorientations. In addition, grain boundary migration was prevalent in the samples that fractured transgranularly, but was rarely observed on any specimen that fractured intergranularly. Based on the collective observations, it is concluded that (1) it is necessary to consider more than just the scalar misorientation when considering whether a single crystal containing LABs should be rejected and (2) characterization of the properties of superalloy bicrystals grown using traditional Bridgman methods is difficult due to the complex, non-planar nature of the resulting LABs that is associated with their dendritic growth.

Initiation and growth of the discontinuous precipitation reaction at [0 1 1] symmetric tilt boundaries in Cu-Be alloy bicrystals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Monzen, R.; Watanabe, C.; Mino, D.

2005-02-01

The initiation and growth of discontinuous precipitation (DP) at [0 1 1] symmetric tilt boundaries in Cu-0.75 wt% Be alloy bicrystals have been studied. Transmission electron microscopy revealed that {gamma} precipitates tended to nucleate at a boundary in such a manner that their habit plane, (1 1 2){sub {alpha}} or (4 4 5){sub {alpha}}, with one of the adjoining grains lay as close as possible to the boundary. The habit plane with a low energy formed on both sides of the precipitates behind an initially migrating boundary, indicating the importance of the existence of the low-energy habit plane for themore » initial boundary migration. The incubation period to initiate DP and cell growth rate for a boundary show a good correlation with the energy of the boundary. A kinetic analysis of DP using the models of Turnbull, and Petermann and Hornbogen has yielded boundary diffusion data. A higher-energy boundary has a higher diffusivity with a smaller activation energy.« less

Cohesive finite element modeling of the delamination of HTPB binder and HMX crystals under tensile loading

DOE Office of Scientific and Technical Information (OSTI.GOV)

Walters, David J.; Luscher, Darby J.; Yeager, John D.

Accurately modeling the mechanical behavior of the polymer binders and the degradation of interfaces between binder and crystal is important to science-based understanding of the macro-scale response of polymer bonded explosives. The paper presents a description of relatively a simple bi-crystal HMX-HTPB specimen and associated tensile loading experiment including computed tomography imaging, the pertinent constitutive theory, and details of numerical simulations used to infer the behavior of the material during the delamination process. Within this work, mechanical testing and direct numerical simulation of this relatively simple bi-crystal system enabled reasonable isolation of binder-crystal interface delamination, in which the effects ofmore » the complicated thermomechanical response of explosive crystals were minimized. Cohesive finite element modeling of the degradation and delamination of the interface between a modified HTPB binder and HMX crystals was used to reproduce observed results from tensile loading experiments on bi-crystal specimens. Several comparisons are made with experimental measurements in order to identify appropriate constitutive behavior of the binder and appropriate parameters for the cohesive traction-separation behavior of the crystal-binder interface. This research demonstrates the utility of directly modeling the delamination between binder and crystal within crystal-binder-crystal tensile specimen towards characterizing the behavior of these interfaces in a manner amenable to larger scale simulation of polycrystalline PBX materials. One critical aspect of this approach is micro computed tomography imaging conducted during the experiments, which enabled comparison of delamination patterns between the direct numerical simulation and actual specimen. In addition to optimizing the cohesive interface parameters, one important finding from this investigation is that understanding and representing the strain-hardening plasticity of HTPB binder is important within the context of using a cohesive traction-separation model for the delamination of a crystal-binder system.« less

Cohesive finite element modeling of the delamination of HTPB binder and HMX crystals under tensile loading

DOE PAGES

Walters, David J.; Luscher, Darby J.; Yeager, John D.; ...

2018-02-27

Accurately modeling the mechanical behavior of the polymer binders and the degradation of interfaces between binder and crystal is important to science-based understanding of the macro-scale response of polymer bonded explosives. The paper presents a description of relatively a simple bi-crystal HMX-HTPB specimen and associated tensile loading experiment including computed tomography imaging, the pertinent constitutive theory, and details of numerical simulations used to infer the behavior of the material during the delamination process. Within this work, mechanical testing and direct numerical simulation of this relatively simple bi-crystal system enabled reasonable isolation of binder-crystal interface delamination, in which the effects ofmore » the complicated thermomechanical response of explosive crystals were minimized. Cohesive finite element modeling of the degradation and delamination of the interface between a modified HTPB binder and HMX crystals was used to reproduce observed results from tensile loading experiments on bi-crystal specimens. Several comparisons are made with experimental measurements in order to identify appropriate constitutive behavior of the binder and appropriate parameters for the cohesive traction-separation behavior of the crystal-binder interface. This research demonstrates the utility of directly modeling the delamination between binder and crystal within crystal-binder-crystal tensile specimen towards characterizing the behavior of these interfaces in a manner amenable to larger scale simulation of polycrystalline PBX materials. One critical aspect of this approach is micro computed tomography imaging conducted during the experiments, which enabled comparison of delamination patterns between the direct numerical simulation and actual specimen. In addition to optimizing the cohesive interface parameters, one important finding from this investigation is that understanding and representing the strain-hardening plasticity of HTPB binder is important within the context of using a cohesive traction-separation model for the delamination of a crystal-binder system.« less

Atomic resolution characterization of a SrTiO{sub 3} grain boundary in the STEM

DOE Office of Scientific and Technical Information (OSTI.GOV)

McGibbon, M.M.; Browning, N.D.; Chisholm, M.F.

This paper uses the complementary techniques of high resolution Z-contrast imaging and PEELS (parallel detection electron energy loss spectroscopy) to investigate the atomic structure and chemistry of a 25 degree symmetric tilt boundary in a bicrystal of the electroceramic SrTiO{sub 3}. The gain boundary is composed of two different boundary structural units which occur in about equal numbers: one which contains Ti-O columns and the other without.

Multiscale Modeling for the Analysis for Grain-Scale Fracture Within Aluminum Microstructures

NASA Technical Reports Server (NTRS)

Glaessgen, Edward H.; Phillips, Dawn R.; Yamakov, Vesselin; Saether, Erik

2005-01-01

Multiscale modeling methods for the analysis of metallic microstructures are discussed. Both molecular dynamics and the finite element method are used to analyze crack propagation and stress distribution in a nanoscale aluminum bicrystal model subjected to hydrostatic loading. Quantitative similarity is observed between the results from the two very different analysis methods. A bilinear traction-displacement relationship that may be embedded into cohesive zone finite elements is extracted from the nanoscale molecular dynamics results.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Meiser, Jerome; Urbassek, Herbert M., E-mail: urbassek@rhrk.uni-kl.de

Using classical molecular dynamics simulations and the Meyer-Entel interaction potential, we study the martensitic transformation pathway in a pure iron bi-crystal containing a symmetric tilt grain boundary. Upon cooling the system from the austenitic phase, the transformation starts with the nucleation of the martensitic phase near the grain boundary in a plate-like arrangement. The Kurdjumov-Sachs orientation relations are fulfilled at the plates. During further cooling, the plates expand and merge. In contrast to the orientation relation in the plate structure, the complete transformation proceeds via the Pitsch pathway.

Shear response of grain boundaries with metastable structures by molecular dynamics simulations

NASA Astrophysics Data System (ADS)

Zhang, Liang; Lu, Cheng; Shibuta, Yasushi

2018-04-01

Grain boundaries (GBs) can play a role as the favored locations to annihilate point defects, such as interstitial atoms and vacancies. It is thus highly probable that different boundary structures can be simultaneously present in equilibrium with each other in the same GB, and thus the GB achieves a metastable state. However, the structural transition and deformation mechanism of such GBs are currently not well understood. In this work, molecular dynamics simulations were carried out to study the multiple structures of a Σ5(310)/[001] GB in bicrystal Al and to investigate the effect of structural multiplicity on the mechanical and kinetic properties of such a GB. Different GB structures were obtained by changing the starting atomic configuration of the bicrystal model, and the GB structures had significantly different atomic density. For the Σ5(310) GB with metastable structures, GB sliding was the dominant mechanism at a low temperature (T = 10 K) under shear stress. The sliding mechanism resulted from the uncoordinated transformation of the inhomogeneous structural units. The nucleation of voids was observed during GB sliding at the low temperature, and the voids subsequently evolved to a nanocrack at the boundary plane. Increasing the temperature can induce the structural transition of local GB structures and can change their overall kinetic properties. GB migration with occasional GB sliding dominated the deformation mechanism at elevated temperatures (T = 300 and 600 K), and the migration process of the metastable GB structures is closely related to the thermally assisted diffusion mechanism.

A molecular dynamics study of tilt grain boundary resistance to slip and heat transfer in nanocrystalline silicon

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, Xiang; Chen, Youping; Xiong, Liming

2014-12-28

We present a molecular dynamics study of grain boundary (GB) resistance to dislocation-mediated slip transfer and phonon-mediated heat transfer in nanocrystalline silicon bicrystal. Three most stable 〈110〉 tilt GBs in silicon are investigated. Under mechanical loading, the nucleation and growth of hexagonal-shaped shuffle dislocation loops are reproduced. The resistances of different GBs to slip transfer are quantified through their constitutive responses. Results show that the Σ3 coherent twin boundary (CTB) in silicon exhibits significantly higher resistance to dislocation motion than the Σ9 GB in glide symmetry and the Σ19 GB in mirror symmetry. The distinct GB strengths are explained bymore » the atomistic details of the dislocation-GB interaction. Under thermal loading, based on a thermostat-induced heat pulse model, the resistances of the GBs to transient heat conduction in ballistic-diffusive regime are characterized. In contrast to the trend found in the dislocation-GB interaction in bicrystal models with different GBs, the resistances of the same three GBs to heat transfer are strikingly different. The strongest dislocation barrier Σ3 CTB is almost transparent to heat conduction, while the dislocation-permeable Σ9 and Σ19 GBs exhibit larger resistance to heat transfer. In addition, simulation results suggest that the GB thermal resistance not only depends on the GB energy but also on the detailed atomic structure along the GBs.« less

An extended 3D discrete-continuous model and its application on single- and bi-crystal micropillars

NASA Astrophysics Data System (ADS)

Huang, Minsheng; Liang, Shuang; Li, Zhenhuan

2017-04-01

A 3D discrete-continuous model (3D DCM), which couples the 3D discrete dislocation dynamics (3D DDD) and finite element method (FEM), is extended in this study. New schemes for two key information transfers between DDD and FEM, i.e. plastic-strain distribution from DDD to FEM and stress transfer from FEM to DDD, are suggested. The plastic strain induced by moving dislocation segments is distributed to an elementary spheroid (ellipsoid or sphere) via a specific new distribution function. The influence of various interfaces (such as free surfaces and grain boundaries (GBs)) on the plastic-strain distribution is specially considered. By these treatments, the deformation fields can be solved accurately even for dislocations on slip planes severely inclined to the FE mesh, with no spurious stress concentration points produced. In addition, a stress correction by singular and non-singular theoretical solutions within a cut-off sphere is introduced to calculate the stress on the dislocations accurately. By these schemes, the present DCM becomes less sensitive to the FE mesh and more numerically efficient, which can also consider the interaction between neighboring dislocations appropriately even though they reside in the same FE mesh. Furthermore, the present DCM has been employed to model the compression of single-crystal and bi-crystal micropillars with rigid and dislocation-absorbed GBs. The influence of internal GB on the jerky stress-strain response and deformation mode is studied in detail to shed more light on these important micro-plastic problems.

The role of surfaces, chemical interfaces, and disorder on plutonium incorporation in pyrochlores

DOE PAGES

Perriot, Romain; Dholabhai, Pratik P.; Uberuaga, Blas P.

2016-07-27

Pyrochlores, a class of complex oxides with formula A 2B 2O 7, are one of the candidates for nuclear waste encapsulation, due to the natural occurrence of actinide-bearing pyrochlore minerals and laboratory observations of high radiation tolerance. In this work, we use atomistic simulations to determine the role of surfaces, chemical interfaces, and cation disorder on the plutonium immobilization properties of pyrochlores as a function of pyrochlore chemistry. We find that both Pu 3+ and Pu 4+ segregate to the surface for the four low-index pyrochlore surfaces considered, and that the segregation energy varies with the chemistry of the compound.more » We also find that pyrochlore/pyrochlore bicrystals A 2B 2O 7/A 2'B 2'O 7 can be used to immobilize Pu 3+ and Pu 4+ either in the same or separate phases of the compound, depending on the chemistry of the material. Finally, we find that Pu 4+ segregates to the disordered phase of an order/disorder bicrystal, driven by the occurrence of local oxygen-rich environments. However, Pu 3+ is weakly sensitive to the oxygen environment, and therefore only slightly favors the disordered phase. This behavior suggests that, at some concentration, Pu incorporation can destabilize the pyrochlore structure. Together, these results provide new insight into the ability of pyrochlore compounds to encapsulate Pu and suggest new considerations in the development of waste forms based on pyrochlores. Particularly, the phase structure of a multi-phase pyrochlore composite can be used to independently getter decay products based on their valence and size.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Perriot, Romain; Dholabhai, Pratik P.; Uberuaga, Blas P.

Pyrochlores, a class of complex oxides with formula A 2B 2O 7, are one of the candidates for nuclear waste encapsulation, due to the natural occurrence of actinide-bearing pyrochlore minerals and laboratory observations of high radiation tolerance. In this work, we use atomistic simulations to determine the role of surfaces, chemical interfaces, and cation disorder on the plutonium immobilization properties of pyrochlores as a function of pyrochlore chemistry. We find that both Pu 3+ and Pu 4+ segregate to the surface for the four low-index pyrochlore surfaces considered, and that the segregation energy varies with the chemistry of the compound.more » We also find that pyrochlore/pyrochlore bicrystals A 2B 2O 7/A 2'B 2'O 7 can be used to immobilize Pu 3+ and Pu 4+ either in the same or separate phases of the compound, depending on the chemistry of the material. Finally, we find that Pu 4+ segregates to the disordered phase of an order/disorder bicrystal, driven by the occurrence of local oxygen-rich environments. However, Pu 3+ is weakly sensitive to the oxygen environment, and therefore only slightly favors the disordered phase. This behavior suggests that, at some concentration, Pu incorporation can destabilize the pyrochlore structure. Together, these results provide new insight into the ability of pyrochlore compounds to encapsulate Pu and suggest new considerations in the development of waste forms based on pyrochlores. Particularly, the phase structure of a multi-phase pyrochlore composite can be used to independently getter decay products based on their valence and size.« less

Elementary Mechanisms of Shear-Coupled Grain Boundary Migration

NASA Astrophysics Data System (ADS)

Rajabzadeh, A.; Mompiou, F.; Legros, M.; Combe, N.

2013-06-01

A detailed theoretical study of the elementary mechanisms occurring during the shear-coupled grain boundary (GB) migration at low temperature is performed focusing on both the energetic and structural characteristics. The migration of a Σ13(320) GB in a copper bicrystal in response to external shear displacements is simulated using a semiempirical potential. The minimum energy path of the shear-coupled GB migration is computed using the nudge elastic band method. The GB migration occurs through the nucleation and motion of GB steps identified as disconnections. Energy barriers for the GB and disconnection migrations are evaluated.

Electronic Properties of Grain Boundaries in GaAs: A Study of Oriented Bicrystals Prepared by Epitaxial Lateral Overgrowth.

DTIC Science & Technology

1984-05-10

overgrowth from a spoke 90 pattern of radial stripe openings at 1 intervals on an Si0 2 coated (110) surface. Bright regions are GaAs and dark regions are Si0...the dark current for such an ideal device is given by Idark - Io[exp(eVbi/AokT) - 1] , (11-l) where Io is a proportionality constant describing the...recombination and leakage currents which contribute to an increased dark current. The value of Voc is determined by the built-in junction barrier height and the

Iron Silicide Formation by Precipitation in a Silicon Bicrystal

NASA Astrophysics Data System (ADS)

Portier, X.; Ihlal, A.; Rizk, R.

1997-05-01

Segregation and precipitation of iron in a = 25 silicon bicrystal have been carefully investigated by means of high resolution electron microscopy and energy dispersive X-ray analyses, in combination with capacitance and electron beam induced current measurements. After intentional incorporation of iron in the bicrystal by a simple heating procedure, it was shown that a non-equilibrium segregation of iron has occurred after rapid cooling whereas iron precipitates have been produced upon slow cooling. The silicides are formed mainly at the grain boundary area and they were found to belong to the -FeSi cubic or -FeSi2 tetragonal phases. Each precipitate is simply oriented with respect to one of the two grains without any preference between them. The orientation relationships were found in perfect agreement with those observed for the corresponding iron silicides that are epitaxially grown on oriented silicon substrates. Barrier and recombinative effects on the contaminated (1200 °C) and slowly cooled samples have been detected. These effects have been associated with the formation of iron silicides at the grain boundary. La ségrégation ainsi que la précipitation de siliciures de fer au joint de grains = 25 de silicium ont été etudiées en utilisant la dispersion d'énergie des électrons, la microscopie électronique en transmission haute résolution ainsi que des mesures électriques capacitives et des mesures de courants induits par faisceau d'électrons. A la suite d'une contamination volontaire par diffusion thermique du fer au sein du bicristal, nous avons montré qu'une ségrégation hors-équilibre d'atomes de fer est obtenue après un refroidissement rapide alors qu'un refroidissement lent a pour conséquence la formation de siliciures de fer. Ces petits cristaux de siliciures croissent de préférence au niveau du joint de grains et ils ont pour phase, la phase cubique -FeSi ou la phase quadratique α-FeSi2. Chaque précipité est orienté simplement par rapport à l'un ou à l'autre des deux grains et leurs relations d'orientation coincident avec celles observées pour ces mêmes siliciures épitaxiés sur des surfaces de silicium. Les échantillons contaminés (1200 °C) et refroidis lentement présentent des barrières de potentiel et des effets recombinants. Ces activités électriques ont été associées à la présence de siliciures au niveau du joint.

Study of grain boundary transparency in (Y b1 -xC ax) B a2C u3O bicrystal thin films over a wide temperature, field, and field orientation range

NASA Astrophysics Data System (ADS)

Li, Pei; Abraimov, Dmytro; Polyanskii, Anatolii; Kametani, Fumitake; Larbalestier, David

2015-03-01

The residual low-angle grain boundary (GB) network is still the most important current-limiting mechanism operating in biaxially textured rare-earth barium-copper-oxide (REBCO) coated conductors. While Ca doping is well established to improve supercurrent flow across low-angle GBs in weak fields at high temperatures, Ca doping also depresses Tc, making it so far impractical for high-temperature applications of REBCO coated conductors. On the other hand, high-field-magnet applications of REBCO require low temperatures. Here we systematically evaluate the effectiveness of Ca doping in improving the GB transparency, rGB=JcGB/ Jcgrain , of low-angle Y b1 -xC axBaCuO [001] tilt bicrystal films down to 10 K and with magnetic fields perpendicular and parallel to the film surfaces, while varying the Ca and oxygen doping level. Using low-temperature scanning laser microscopy and magneto-optical imaging, we found rGB to strongly depend on the angle between magnetic field and the GB plane and clearly identified regimes in which JcGB can exceed Jcgrain(rGB>1 ) where the GB pinning is optimized by the field being parallel to the GB dislocations. However, even in this favorable situation, we found that rGB became much smaller at lower temperatures. Calculations of the GB Ca segregation profile predict that the high-Jc channels between the GB dislocation cores are almost Ca free. It may be therefore that the positive effects of Ca doping seen by many authors near Tc are partly a consequence of the higher Tc of these Ca-free channels.

Pore and grain boundary migration under a temperature gradient: A phase-field model study

DOE PAGES

Biner, S. B.

2016-03-16

In this study, the collective migration behavior of pores and grain boundaries under a temperature gradient is studied for simple single crystal, bi-crystal and polycrystal configurations with a phase-field model formulism. For simulation of the microstructure of solids, composed of pores and grain boundaries, the results indicate that not only the volume fraction of pores, but also its spatial partitioning between the grain boundary junctions and the grain boundary segments appears to be important. In addition to various physical properties, the evolution kinetics, under given temperature gradients, will be strongly influenced with the initial morphology of a poly-crystalline microstructure.

Molecular Dynamics Simulations of Grain Boundary and Bulk Diffusion in Metals.

NASA Astrophysics Data System (ADS)

Plimpton, Steven James

Diffusion is a microscopic mass transport mechanism that underlies many important macroscopic phenomena affecting the structural, electrical, and mechanical properties of metals. This thesis presents results from atomistic simulation studies of diffusion both in bulk and in the fast diffusion paths known as grain boundaries. Using the principles of molecular dynamics single boundaries are studied and their structure and dynamic properties characterized. In particular, tilt boundary bicrystal and bulk models of fcc Al and bcc alpha-Fe are simulated. Diffusion coefficients and activation energies for atomic motion are calculated for both models and compared to experimental data. The influence of the interatomic pair potential on the diffusion is studied in detail. A universal relation between the melting temperature that a pair potential induces in a simulated bulk model and the potential energy barrier height for atomic hopping is derived and used to correlate results for a wide variety of pair potentials. Using these techniques grain boundary and bulk diffusion coefficients for any fcc material can be estimated from simple static calculations without the need to perform more time-consuming dynamic simulations. The influences of two other factors on grain boundary diffusion are also studied because of the interest of the microelectronics industry in the diffusion related reliability problem known as electromigration. The first factor, known to affect the self diffusion rate of Al, is the presence of Cu impurity atoms in Al tilt boundaries. The bicrystal model for Al is seeded randomly with Cu atoms and a simple hybrid Morse potential used to model the Al-Cu interaction. While some effect due to the Cu is noted, it is concluded that pair potentials are likely an inadequate approximation for the alloy system. The second factor studied is the effect of the boundary orientation angle on the diffusion rate. Symmetric bcc Fe boundaries are relaxed to find optimal structures and their diffusion coefficients calculated. Good agreement is found with the dislocation pipe model for tilt boundary diffusion.

Low-temperature growth and photoluminescence property of ZnS nanoribbons.

PubMed

Zhang, Zengxing; Wang, Jianxiong; Yuan, Huajun; Gao, Yan; Liu, Dongfang; Song, Li; Xiang, Yanjuan; Zhao, Xiaowei; Liu, Lifeng; Luo, Shudong; Dou, Xinyuan; Mou, Shicheng; Zhou, Weiya; Xie, Sishen

2005-10-06

At a low temperature of 450 degrees C, ZnS nanoribbons have been synthesized on Si and KCl substrates by a simple chemical vapor deposition (CVD) method with a two-temperature-zone furnace. Zinc and sulfur powders are used as sources in the different temperature zones. X-ray diffraction (XRD), selected area electron diffraction (SEAD), and transmission electron microscopy (TEM) analysis show that the ZnS nanoribbons are the wurtzite structure, and there are two types-single-crystal and bicrystal nanoribbons. Photoluminescence (PL) spectrum shows that the spectrum mainly includes two parts: a purple emission band centering at about 390 nm and a blue emission band centering at about 445 nm with a weak green shoulder around 510 nm.

On the role of weak interface in crack blunting process in nanoscale layered composites

NASA Astrophysics Data System (ADS)

Li, Yi; Zhou, Qing; Zhang, Shuang; Huang, Ping; Xu, Kewei; Wang, Fei; Lu, Tianjian

2018-03-01

Heterointerface in a nanoscale metallic layered composite could improve its crack resistance. However, the influence of metallic interface structures on crack propagation has not been well understood at atomic scale. By using the method of molecular dynamics (MD) simulation, the crack propagation behavior in Cu-Nb bilayer is compared with that in Cu-Ni bilayer. We find that the weak Cu-Nb interface plays an important role in hindering crack propagation in two ways: (i) dislocation nucleation at the interface releases stress concentration for the crack to propagate; (ii) the easily sheared weak incoherent interface blunts the crack tip. The results are helpful for understanding the interface structure dependent crack resistance of nanoscale bicrystal interfaces.

A first principles study of commonly observed planar defects in Ti/TiB system

DOE PAGES

Nandwana, Peeyush; Gupta, Niraj; Srinivasan, Srivilliputhur G.; ...

2018-04-20

Here, TiB exhibits a hexagonal cross-section with growth faults on (1 0 0) planes and contains B27-B f bicrystals. The hexagonal cross-section is presently explained by surface free energy minimization principle. We show that interfacial energy calculations explain the longer (1 0 0) facet compared to (1 0 1) type facets whereas free surface energy arguments do not provide the true picture. No quantitative explanation of stacking faults and B27-B f interfaces in TiB exists. We show that the low formation energy of stacking faults and B27-B f interfaces explain their abundance. The low energy barrier for B f formationmore » is shown to be responsible for their presence in TiB.« less

Role of interfaces in deformation and fracture of ordered intermetallics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yoo, M.H.; Fu, C.L.

1996-12-31

While sub- and grain-boundaries are the primary dislocation sources in Ll{sub 2} alloys, yield and flow stresses are strongly influenced by the multiplication and exhaustion of mobile dislocations from the secondary sources. The concept of enhanced microplasticity at grain boundaries due to chemical disordering is well supported by theoretical modeling, but no conclusive direct evidence exist for Ni{sub 3}Al bicrystals. The strong plastic anisotropy reported in TiAl PST (polysynthetically twinned) crystals is attributed in part to localized slip along lamellar interfaces, thus lowering the yield stress for soft orientations. Calculations of work of adhesion suggest that, intrinsically, interfacial cracking ismore » more likely to initiate on {gamma}/{gamma}-type interfaces than on the {alpha}{sub 2}/{gamma} boundary. 70 refs, 5 tabs, 5 figs.« less

Intrinsically higher fatigue cracking resistance of the penetrable and movable incoherent twin boundary

NASA Astrophysics Data System (ADS)

Li, L. L.; Zhang, P.; Zhang, Z. J.; Zhang, Z. F.

2014-01-01

Incoherent twin boundaries (ITBs) are widespread and play a crucial role in unidirectional deformation behavior of materials, however, the intrinsic role of individual ITB under cyclic loading remains elusive. Here we show the fatigue cracking behavior of Cu bicrystal with an ITB as its sole interface for the first time. The slip bands (SBs) could transfer through the ITB; meanwhile, the ITB could migrate with the motion of partial dislocations. Both the penetrability and mobility contribute to the higher fatigue cracking resistance of the ITB and hence the fatigue crack nucleates along the SBs preferentially. These new findings not only shed light on the fatigue cracking mechanisms of a penetrable boundary with direct evidence but also could provide important implications for future interfacial optimization of metallic materials.

A first principles study of commonly observed planar defects in Ti/TiB system

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nandwana, Peeyush; Gupta, Niraj; Srinivasan, Srivilliputhur G.

Here, TiB exhibits a hexagonal cross-section with growth faults on (1 0 0) planes and contains B27-B f bicrystals. The hexagonal cross-section is presently explained by surface free energy minimization principle. We show that interfacial energy calculations explain the longer (1 0 0) facet compared to (1 0 1) type facets whereas free surface energy arguments do not provide the true picture. No quantitative explanation of stacking faults and B27-B f interfaces in TiB exists. We show that the low formation energy of stacking faults and B27-B f interfaces explain their abundance. The low energy barrier for B f formationmore » is shown to be responsible for their presence in TiB.« less

Effect of Grain Boundary Misorientation on Electromigration in Lead-Free Solder Joints

NASA Astrophysics Data System (ADS)

Tasooji, Amaneh; Lara, Leticia; Lee, Kyuoh

2014-12-01

Reduction in microelectronic interconnect size gives rise to solder bumps consisting of few grains, approaching a single- or bicrystal grain morphology in C4 bumps. Single grain anisotropy, individual grain orientation, presence of easy diffusion paths along grain boundaries, and the increased current density in these small solder bumps aggravate electromigration. This reduces the reliability of the entire microelectronic system. This paper focuses on electromigration behavior in Pb-free solder, specifically the Sn-0.7 wt.%Cu alloy. We discuss the effects of texture, grain orientation, and grain boundary misorientation angle on electromigration (EM) and intermetallic compound formation in EM-tested C4 bumps. The detailed electron backscatter diffraction (EBSD) analysis used in this study reveals the greater influence of grain boundary misorientation on solder bump electromigration compared with the effect associated with individual grain orientation.

Grain boundary crystallography in polycrystalline yttria-stabilised cubic zirconia

NASA Astrophysics Data System (ADS)

Kini, Maya K.

2018-07-01

Properties of grain boundaries such as grain boundary energy, mobility and diffusion are reported to depend strongly on their crystallography. While studies on ceramic bicrystals with low Σ misorientations have shown highly ordered structures and low energies, studies on dense polycrystalline ceramics often show the significance of grain boundary planes. In the present study, grain boundary plane distributions were studied for yttria-stabilised cubic zirconia with varying grain sizes using Electron Back Scattered Diffraction technique combined with a stereological approach. Despite nearly isotropic grain boundary plane distributions, a highly anisotropic grain boundary character distribution is observed for specific misorientations. Certain low-energy symmetric tilts such as Σ3 and Σ11 are found to occur with high frequencies across the grain size range studied, leading to an inverse correlation between GB energy and frequency of occurrence, consistent with other ceramics studied in literature.

Influence of Alloying upon Grain-Boundary Creep

NASA Technical Reports Server (NTRS)

Rhines, F N; Bond, W E; Kissel, M A

1957-01-01

Grain-boundary displacement, occurring in bicrystals during creep at elevated temperature (350 degrees c), has been measured as a function of the copper content (0.1 to 3 percent) in a series of aluminum-rich aluminum-copper solid-solution alloys. The minimums in stress and temperature, below which grain-boundary motion does not occur, increase regularly with the copper content as would be expected if recovery is necessary for movement. Otherwise, the effects, if any, of the copper solute upon grain-boundary displacement and its rate are too small for identification by the experimental technique employed. It was shown, additionally, that grain-boundary displacement appears regular and proceeds at a constant rate if observed parallel to the stress axis, whereas the motion is seen to occur in a sequence of surges and the rate to diminish with time if the observations are made perpendicular to the stress axis.

Disconnections kinks and competing modes in shear-coupled grain boundary migration

NASA Astrophysics Data System (ADS)

Combe, N.; Mompiou, F.; Legros, M.

2016-01-01

The response of small-grained metals to mechanical stress is investigated by a theoretical study of the elementary mechanisms occurring during the shear-coupled migration of grain boundaries (GB). Investigating a model Σ 17 (410 ) GB in a copper bicrystal, both <110 > and <100 > GB migration modes are studied focusing on both the structural and energetic characteristics. The minimum energy paths of these shear-coupled GB migrations are computed using the nudge elastic band method. For both modes, the GB migration occurs through the nucleation and motion of disconnections. However, the atomic mechanisms of both modes qualitatively differ: While the <110 > mode presents no metastable state, the <100 > mode shows multiple metastable states, some of them evidencing some kinks along the disconnection lines. Disconnection kinks nucleation and motion activation energies are evaluated. Besides, the activation energies of the <100 > mode are smaller than those of the <110 > one except for very high stresses. These results significantly improve our knowledge of the GB migration mechanisms and the conditions under which they occur.

Depth Resolution Dependence on Sample Thickness and Incident Energy in On-Axis Transmission Kikuchi Diffraction in Scanning Electron Microscope (SEM).

PubMed

Brodu, Etienne; Bouzy, Emmanuel

2017-12-01

Transmission Kikuchi diffraction is an emerging technique aimed at producing orientation maps of the structure of materials with a nanometric lateral resolution. This study investigates experimentally the depth resolution of the on-axis configuration, via a twinned silicon bi-crystal sample specifically designed and fabricated. The measured depth resolution varies from 30 to 65 nm in the range 10-30 keV, with a close to linear dependence with incident energy and no dependence with the total sample thickness. The depth resolution is explained in terms of two mechanisms acting concomitantly: generation of Kikuchi diffraction all along the thickness of the sample, associated with continuous absorption on the way out. A model based on the electron mean free path is used to account for the dependence with incident energy of the depth resolution. In addition, based on the results in silicon, the use of the mean absorption coefficient is proposed to predict the depth resolution for any atomic number and incident energy.

Dislocation structures and electrical conduction properties of low angle tilt grain boundaries in LiNbO{sub 3}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Furushima, Yuho; Nakamura, Atsutomo, E-mail: nakamura@numse.nagoya-u.ac.jp; Toyoura, Kazuaki

Dislocations in crystalline materials constitute unique, atomic-scale, one-dimensional structure and have a potential to induce peculiar physical properties that are not found in the bulk. In this study, we fabricated LiNbO{sub 3} bicrystals with low angle tilt grain boundaries and investigated the relationship between the atomic structure of the boundary dislocations and their electrical conduction properties. Observations by using transmission electron microscopy revealed that dislocation structures at the (0001) low angle tilt grain boundaries depend on the tilt angle of the boundaries. Specifically, the characteristic dislocation structures with a large Burgers vector were formed in the boundary with the tiltmore » angle of 2°. It is noteworthy that only the grain boundary of 2° exhibits distinct electrical conductivity after reduction treatment, although LiNbO{sub 3} is originally insulating. This unique electrical conductivity is suggested to be due to the characteristic dislocation structures with a large Burgers vector.« less

Epitaxy of semiconductor-superconductor nanowires

NASA Astrophysics Data System (ADS)

Krogstrup, P.; Ziino, N. L. B.; Chang, W.; Albrecht, S. M.; Madsen, M. H.; Johnson, E.; Nygård, J.; Marcus, C. M.; Jespersen, T. S.

2015-04-01

Controlling the properties of semiconductor/metal interfaces is a powerful method for designing functionality and improving the performance of electrical devices. Recently semiconductor/superconductor hybrids have appeared as an important example where the atomic scale uniformity of the interface plays a key role in determining the quality of the induced superconducting gap. Here we present epitaxial growth of semiconductor-metal core-shell nanowires by molecular beam epitaxy, a method that provides a conceptually new route to controlled electrical contacting of nanostructures and the design of devices for specialized applications such as topological and gate-controlled superconducting electronics. Our materials of choice, InAs/Al grown with epitaxially matched single-plane interfaces, and alternative semiconductor/metal combinations allowing epitaxial interface matching in nanowires are discussed. We formulate the grain growth kinetics of the metal phase in general terms of continuum parameters and bicrystal symmetries. The method realizes the ultimate limit of uniform interfaces and seems to solve the soft-gap problem in superconducting hybrid structures.

Theoretical study of the properties of X-ray diffraction moiré fringes. I

PubMed Central

Yoshimura, Jun-ichi

2015-01-01

A detailed and comprehensive theoretical description of X-ray diffraction moiré fringes for a bicrystal specimen is given on the basis of a calculation by plane-wave dynamical diffraction theory. Firstly, prior to discussing the main subject of the paper, a previous article [Yoshimura (1997 ▸). Acta Cryst. A53, 810–812] on the two-dimensionality of diffraction moiré patterns is restated on a thorough calculation of the moiré interference phase. Then, the properties of moiré fringes derived from the above theory are explained for the case of a plane-wave diffraction image, where the significant effect of Pendellösung intensity oscillation on the moiré pattern when the crystal is strained is described in detail with theoretically simulated moiré images. Although such plane-wave moiré images are not widely observed in a nearly pure form, knowledge of their properties is essential for the understanding of diffraction moiré fringes in general. PMID:25970298

Chemical reactions and morphological stability at the Cu/Al2O3 interface.

PubMed

Scheu, C; Klein, S; Tomsia, A P; Rühle, M

2002-10-01

The microstructures of diffusion-bonded Cu/(0001)Al2O3 bicrystals annealed at 1000 degrees C at oxygen partial pressures of 0.02 or 32 Pa have been studied with various microscopy techniques ranging from optical microscopy to high-resolution transmission electron microscopy. The studies revealed that for both oxygen partial pressures a 20-35 nm thick interfacial CuAlO2 layer formed, which crystallises in the rhombohedral structure. However, the CuAlO2 layer is not continuous, but interrupted by many pores. In the samples annealed in the higher oxygen partial pressure an additional reaction phase with a needle-like structure was observed. The needles are several millimetres long, approximately 10 microm wide and approximately 1 microm thick. They consist of CuAlO2 with alternating rhombohedral and hexagonal structures. Solid-state contact angle measurements were performed to derive values for the work of adhesion. The results show that the adhesion is twice as good for the annealed specimen compared to the as-bonded sample.

Thermal fatigue and oxidation data of superalloys including directionally solidified eutectics

NASA Technical Reports Server (NTRS)

Hill, V. L.; Humphreys, V. E.

1977-01-01

Thermal fatigue and oxidation data were obtained on 61 specimens, representing 15 discrete alloy compositions or fabricating techniques and three coating systems. Conventionally fabricated alloys included V57, MM 200, Rene 77, Rene 125, MM 246, MM 509, IN-738, IN-792 + Hf, and MM 200 + Hf. The directionally solidified alloys were MM 200, MM 200 single crystal, MM 200 bicrystal, cellular gamma/gamma' - delta) and lamellar gamma/gamma' - delta. The coatings systems included NiCrAlY on IN-738, In-792 + Hf, MM 200 DS, MM 200 DS single crystal, and cellular gamma/gamma' - delta and NiCrAlY/Pt on lamellar gamma/gamma' - delta. Crack initiation survival rates were recorded for all alloys, with and without coatings. All uncoated alloys, except MM 509, exhibited significant oxidation weight loss in 75,000 to 15,000 cycles. MM 509 specimens had weight losses only slightly higher than coated specimens through 7,500 cycles. All coated specimens had low weight loss.

Synthesis of uniformly distributed single- and double-sided zinc oxide (ZnO) nanocombs

DOE Office of Scientific and Technical Information (OSTI.GOV)

Altintas Yildirim, Ozlem; Liu, Yuzi; Petford-Long, Amanda K.

Uniformly distributed single- and double-sided zinc oxide (ZnO) nanocomb structures have been prepared by a vapor-liquid-solid technique from a mixture of ZnO nanoparticles and graphene nanoplatelets. The ZnO seed nanoparticles were synthesized via a simple precipitation method. The structure of the ZnO nanocombs could easily be controlled by tuning the carrier-gas flow rate during growth. Higher flow rate resulted in the formation of uniformly-distributed single-sided comb structures with nanonail-shaped teeth, as a result of the self-catalysis effect of the catalytically active Zn-terminated polar (0001) surface. Lower gas flow rate was favorable for production of double-sided comb structures with the twomore » sets of teeth at an angle of similar to 110 degrees to each other along the comb ribbon, which was attributed to the formation of a bicrystal nanocomb ribbon. Lastly, the formation of such a double-sided structure with nanonail-shaped teeth has not previously been reported.« less

Synthesis of uniformly distributed single- and double-sided zinc oxide (ZnO) nanocombs

DOE PAGES

Altintas Yildirim, Ozlem; Liu, Yuzi; Petford-Long, Amanda K.

2015-08-21

Uniformly distributed single- and double-sided zinc oxide (ZnO) nanocomb structures have been prepared by a vapor-liquid-solid technique from a mixture of ZnO nanoparticles and graphene nanoplatelets. The ZnO seed nanoparticles were synthesized via a simple precipitation method. The structure of the ZnO nanocombs could easily be controlled by tuning the carrier-gas flow rate during growth. Higher flow rate resulted in the formation of uniformly-distributed single-sided comb structures with nanonail-shaped teeth, as a result of the self-catalysis effect of the catalytically active Zn-terminated polar (0001) surface. Lower gas flow rate was favorable for production of double-sided comb structures with the twomore » sets of teeth at an angle of similar to 110 degrees to each other along the comb ribbon, which was attributed to the formation of a bicrystal nanocomb ribbon. Lastly, the formation of such a double-sided structure with nanonail-shaped teeth has not previously been reported.« less

Fabrication of sapphire-based high performance step-edge HTS Josephson junctions and SQUIDs and their application to scanning SQUID microscopy

NASA Astrophysics Data System (ADS)

Ming, Bin

Josephson junctions are at the heart of any superconductor device applications. A SQUID (Superconducting Quantum Interference Device), which consists of two Josephson junctions, is by far the most important example. Unfortunately, in the case of high-Tc superconductors (HTS), the quest for a robust, flexible, and high performance junction technology is yet far from the end. Currently, the only proven method to make HTS junctions is the SrTiO3(STO)-based bicrystal technology. In this thesis we concentrate on the fabrication of YBCO step-edge junctions and SQUIDs on sapphire. The step-edge method provides complete control of device locations and facilitates sophisticated, high-density layout. We select CeO2 as the buffer layer, as the key step to make device quality YBCO thin films on sapphire. With an "overhang" shadow mask produced by a novel photolithography technique, a steep step edge was fabricated on the CeO2 buffer layer by Ar+ ion milling with optimized parameters for minimum ion beam divergence. The step angle was determined to be in excess of 80° by atomic force microscopy (AFM). Josephson junctions patterned from those step edges exhibited resistively shunted junction (RSJ) like current-voltage characteristics. IcR n values in the 200--500 mV range were measured at 77K. Shapiro steps were observed under microwave irradiation, reflecting the true Josephson nature of those junctions. The magnetic field dependence of the junction Ic indicates a uniform current distribution. These results suggest that all fabrication processes are well controlled and the step edge is relatively straight and free of microstructural defects. The SQUIDs made from the same process exhibit large voltage modulation in a varying magnetic field. At 77K, our sapphire-based step-edge SQUID has a low white noise level at 3muphi0/ Hz , as compared to typically >10muphi0/ Hz from the best bicrystal STO SQUIDS. Our effort at device fabrication is chiefly motivated by the scanning SQUID microscopy (SSM) application. A scanning SQUID microscope is a non-contact, non-destructive imaging tool that can resolve weak currents beneath the sample surface by detecting their magnetic fields. Our low-noise sapphire-based step-edge SQUIDs should be particularly suitable for such an application. An earlier effort to make SNS trench junctions using focused ion beam (FIB) is reviewed in a separate chapter. (Abstract shortened by UMI.)

Experimentally quantifying critical stresses associated with basal slip and twinning in magnesium using micro-pillars

DOE PAGES

Liu, Yue; Li, Nan; Mariyappan, Arul Kumar; ...

2017-06-07

Basal slip and {01more » $$\\bar{1}$$2} twinning are two major plastic deformation mechanisms in hexagonal closed-packed magnesium. Here in this paper, we quantify the critical stresses associated with basal slip and twinning in single-crystal and bi-crystal magnesium samples by performing in situ compression of micropillars with different diameters in a scanning electron microscope. The micropillars are designed to favor either slip or twinning under uniaxial compression. Compression tests imply a negligible size effect related to basal slip and twinning as pillar diameter is greater than 10 μm. The critical resolved shear stresses are deduced to be 29 MPa for twinning and 6 MPa for basal slip from a series of micropillar compression tests. Employing full-field elasto-visco-plastic simulations, we further interpret the experimental observations in terms of the local stress distribution associated with multiple twinning, twin nucleation, and twin growth. Our simulation results suggest that the twinning features being studied should not be close to the top surface of the micropillar because of local stress perturbations induced by the hard indenter.« less

Colloidal crystal grain boundary formation and motion

PubMed Central

Edwards, Tara D.; Yang, Yuguang; Beltran-Villegas, Daniel J.; Bevan, Michael A.

2014-01-01

The ability to assemble nano- and micro- sized colloidal components into highly ordered configurations is often cited as the basis for developing advanced materials. However, the dynamics of stochastic grain boundary formation and motion have not been quantified, which limits the ability to control and anneal polycrystallinity in colloidal based materials. Here we use optical microscopy, Brownian Dynamic simulations, and a new dynamic analysis to study grain boundary motion in quasi-2D colloidal bicrystals formed within inhomogeneous AC electric fields. We introduce “low-dimensional” models using reaction coordinates for condensation and global order that capture first passage times between critical configurations at each applied voltage. The resulting models reveal that equal sized domains at a maximum misorientation angle show relaxation dominated by friction limited grain boundary diffusion; and in contrast, asymmetrically sized domains with less misorientation display much faster grain boundary migration due to significant thermodynamic driving forces. By quantifying such dynamics vs. compression (voltage), kinetic bottlenecks associated with slow grain boundary relaxation are understood, which can be used to guide the temporal assembly of defect-free single domain colloidal crystals. PMID:25139760

Intergranular fracture in UO{sub 2}: derivation of traction-separation law from atomistic simulations

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Yongfeng; Millett, P.C.; Tonks, M.R.

2013-07-01

In this study, the intergranular fracture behavior of UO{sub 2} was studied by molecular dynamics simulations using the Basak potential. In addition, the constitutive traction-separation law was derived from atomistic data using the cohesive-zone model. In the simulations a bicrystal model with the (100) symmetric tilt Σ5 grain boundaries was utilized. Uniaxial tension along the grain boundary normal was applied to simulate Mode-I fracture. The fracture was observed to propagate along the grain boundary by micro-pore nucleation and coalescence, giving an overall intergranular fracture behavior. Phase transformations from the Fluorite to the Rutile and Scrutinyite phases were identified at themore » propagating crack tips. These new phases are metastable and they transformed back to the Fluorite phase at the wake of crack tips as the local stress concentration was relieved by complete cracking. Such transient behavior observed at atomistic scale was found to substantially increase the energy release rate for fracture. Insertion of Xe gas into the initial notch showed minor effect on the overall fracture behavior. (authors)« less

Intergranular fracture in UO2: derivation of traction-separation law from atomistic simulations

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yongfeng Zhang; Paul C Millett; Michael R Tonks

2013-10-01

In this study, the intergranular fracture behavior of UO2 was studied by molecular dynamics simulations using the Basak potential. In addition, the constitutive traction-separation law was derived from atomistic data using the cohesive-zone model. In the simulations a bicrystal model with the (100) symmetric tilt E5 grain boundaries was utilized. Uniaxial tension along the grain boundary normal was applied to simulate Mode-I fracture. The fracture was observed to propagate along the grain boundary by micro-pore nucleation and coalescence, giving an overall intergranular fracture behavior. Phase transformations from the Fluorite to the Rutile and Scrutinyite phases were identified at the propagatingmore » crack tips. These new phases are metastable and they transformed back to the Fluorite phase at the wake of crack tips as the local stress concentration was relieved by complete cracking. Such transient behavior observed at atomistic scale was found to substantially increase the energy release rate for fracture. Insertion of Xe gas into the initial notch showed minor effect on the overall fracture behavior.« less

Shear-coupled grain-boundary migration dependence on normal strain/stress

NASA Astrophysics Data System (ADS)

Combe, N.; Mompiou, F.; Legros, M.

2017-08-01

In specific conditions, grain-boundary (GB) migration occurs in polycrystalline materials as an alternative vector of plasticity compared to the usual dislocation activity. The shear-coupled GB migration, the expected most efficient GB based mechanism, couples the GB motion to an applied shear stress. Stresses on GB in polycrystalline materials seldom have, however, a unique pure shear component. This work investigates the influence of a normal strain on the shear coupled migration of a Σ 13 (320 )[001 ] GB in a copper bicrystal using atomistic simulations. We show that the yield shear stress inducing the GB migration strongly depends on the applied normal stress. Beyond, the application of a normal stress on this GB qualitatively modifies the GB migration: while the Σ 13 (320 )[001 ] GB shear couples following the 〈110 〉 migration mode without normal stress, we report the observation of the 〈010 〉 mode under a sufficiently high tensile normal stress. Using the nudge elastic band method, we uncover the atomistic mechanism of this 〈010 〉 migration mode and energetically characterize it.

Study of Etching Pits in a Large-grain Single Cell Bulk Niobium Cavity

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhao, Xin; Ciovati, Gianluigi; Reece, Charles E.

2009-11-01

Performance of SRF cavities are limited by non-linear localized effects. The variation of local material characters between "hot" and "cold" spots is thus of intense interest. Such locations were identified in a BCP-etched large-grain single-cell cavity and removed for examination by high resolution electron microscopy (SEM), electron-back scattering diffraction microscopy (EBSD), optical microscopy, and 3D profilometry. Pits with clearly discernable crystal facets were observed in both "hotspot" and "coldspot" specimens. The pits were found in-grain, at bi-crystal boundaries, and on tri-crystal junctions. They are interpreted as etch pits induced by surface crystal defects (e.g. dislocations). All "coldspots" examined had qualitativelymore » low density of etching pits or very shallow tri-crystal boundary junction. EBSD revealed crystal structure surrounding the pits via crystal phase orientation mapping, while 3D profilometry gave information on the depth and size of the pits. In addition, a survey of the samples by energy dispersive X-ray analysis (EDX) did not show any significant contamination of the samples surface.« less

A model for finite-deformation nonlinear thermomechanical response of single crystal copper under shock conditions

NASA Astrophysics Data System (ADS)

Luscher, Darby J.; Bronkhorst, Curt A.; Alleman, Coleman N.; Addessio, Francis L.

2013-09-01

A physically consistent framework for combining pressure-volume-temperature equations of state with crystal plasticity models is developed for the application of modeling the response of single and polycrystals under shock conditions. The particular model is developed for copper, thus the approach focuses on crystals of cubic symmetry although many of the concepts in the approach are applicable to crystals of lower symmetry. We employ a multiplicative decomposition of the deformation gradient into isochoric elastic, thermoelastic dilation, and plastic parts leading to a definition of isochoric elastic Green-Lagrange strain. This finite deformation kinematic decomposition enables a decomposition of Helmholtz free-energy into terms reflecting dilatational thermoelasticity, strain energy due to long-range isochoric elastic deformation of the lattice and a term reflecting energy stored in short range elastic lattice deformation due to evolving defect structures. A model for the single crystal response of copper is implemented consistent with the framework into a three-dimensional Lagrangian finite element code. Simulations exhibit favorable agreement with single and bicrystal experimental data for shock pressures ranging from 3 to 110 GPa.

Low-temperature mechanical properties of superconducting radio frequency cavity materials

DOE Office of Scientific and Technical Information (OSTI.GOV)

Byun, Thak Sang; Kim, Sang-Ho; Mammosser, John

2009-01-01

Low temperature mechanical behaviors have been investigated for the constituent materials of superconducting radio frequency cavities. Test materials consist of small grain Nb, single crystal Nb, large grain Nb (bicrystal), Ti45Nb-Nb weld joint (e-beam welded), and Ti-316L bimetal joint (explosion welded). The strength of all test metals displayed strong temperature dependence and the Ti-316L bimetal showed the highest strength and lowest ductility among the test materials. The fracture toughness of the small grain Nb metals decreased with decreasing test temperature and reached the lower shelf values (30 40 MPa m) at or above 173 K. The Ti45Nb base and Ti45Nb-Nbmore » weld metals showed much higher fracture toughness than the small grain Nb. An extrapolation and comparison with existing data showed that the fracture toughness of the small grain Nb metals at 4 K was expected to be similar to those at 173 K and 77 K. The results from optical photography at a low magnification and fractography by a scanning electron microscope were consistent with corresponding mechanical properties.« less

Three-dimensional interaction and movements of various dislocations in anisotropic bicrystals with semicoherent interfaces

NASA Astrophysics Data System (ADS)

Vattré, A.; Pan, E.

2018-07-01

Lattice dislocation interactions with semicoherent interfaces are investigated by means of anisotropic field solutions in metallic homo- and hetero-structures. The present framework is based on the mathematically elegant and computationally powerful Stroh formalism, combining further with the Fourier integral and series transforms, which cover different shapes and dimensions of various extrinsic and intrinsic dislocations. Two-dimensional equi-spaced arrays of straight lattice dislocations and finite arrangements of piled-up dislocations as well as any polygonal and elliptical dislocation loops in three dimensions are considered using a superposition scheme. Self, image and Peach-Koehler forces are derived to compute the equilibrium dislocation positions in pile-ups, including the internal structures and energetics of the interfacial dislocation networks. For illustration, the effects due to the elastic and misfit mismatches are discussed in the pure misfit Au/Cu and heterophase Cu/Nb systems, while discrepancies resulting from the approximation of isotropic elasticity are clearly exhibited. These numerical examples not only feature and enhance the existing works in anisotropic bimaterials, but also promote a novel opportunity of analyzing the equilibrium shapes of planar glide dislocation loops at nanoscale.

Investigating Deformation and Mesoscale Void Creation in HMX Based Composites using Tomography Based Grain Scale Finite Element Modeling

NASA Astrophysics Data System (ADS)

Walters, David J.; Luscher, Darby J.; Manner, Virginia; Yeager, John D.; Patterson, Brian M.

2017-06-01

The microstructure of plastic bonded explosives (PBXs) significantly affects their macroscale mechanical characteristics. Imaging and modeling of the mesoscale constituents allows for a detailed examination of the deformation of mechanically loaded PBXs. In this study, explosive composites, formulated with HMX crystals and various HTPB based polymer binders have been imaged using micro Computed Tomography (μCT). Cohesive parameters for simulation of the crystal/binder interface are determined by comparing numerical and experimental results of the delamination of a polymer bound bi-crystal system. Similarly, polycrystalline samples are discretized into a finite element mesh using the mesoscale geometry captured by in-situ μCT imaging. Experimentally, increasing the stiffness of the HTPB binder in the polycrystalline system resulted in a transition from ductile flow with little crystal/binder delamination to brittle behavior with increased void creation along the interfaces. Simulating the macroscale compression of these samples demonstrates the effects that the mesoscale geometry, cohesive properties, and binder stiffness have on the creation and distribution of interfacial voids. Understanding void nucleation is critical for modeling damage in these complex materials.

Electromigration-Induced Surface Drift and Slit Propagation in Polycrystalline Interconnects: Insights from Phase-Field Simulations

NASA Astrophysics Data System (ADS)

Mukherjee, Arnab; Ankit, Kumar; Selzer, Michael; Nestler, Britta

2018-04-01

We employ the phase-field method to assess electromigration (EM) damage in wide polycrystalline interconnects due to grain-boundary grooving. An interplay of surface and grain-boundary diffusion is shown to drastically influence the mode of progressive EM damage. Rapid atomic transport along the surface leads to shape-preserving surface drift reminiscent of Blech drift-velocity experiments. On the other hand, a comparatively faster grain-boundary transport localizes the damage, resulting in the proliferation of intergranular slits with a shape-preserving tip. At steady state, the two regimes exhibit exponents of 1 and 3 /2 , respectively, in Black's law. While surface drift obeys an inverse scaling with grain size, slits exhibit a direct relationship at small sizes, with the dependence becoming weaker at larger ones. Furthermore, we explain the influence of curvature- or EM-mediated healing fluxes running along the surface on groove replenishment. Insights derived from phase-field simulations of EM in bicrystals are extended to investigate the multiphysics of mixed-mode damage of a polycrystalline interconnect line that is characterized by a drift of small grain surfaces, slit propagation, and coarsening. The triple and quadruple junctions are identified as prominent sites of failure.

Atomic scale structure and chemistry of interfaces by Z-contrast imaging and electron energy loss spectroscopy in the stem

DOE Office of Scientific and Technical Information (OSTI.GOV)

McGibbon, M.M.; Browning, N.D.; Chisholm, M.F.

The macroscopic properties of many materials are controlled by the structure and chemistry at grain boundaries. A basic understanding of the structure-property relationship requires a technique which probes both composition and chemical bonding on an atomic scale. High-resolution Z-contrast imaging in the scanning transmission electron microscope (STEM) forms an incoherent image in which changes in atomic structure and composition across an interface can be interpreted directly without the need for preconceived atomic structure models. Since the Z-contrast image is formed by electrons scattered through high angles, parallel detection electron energy loss spectroscopy (PEELS) can be used simultaneously to provide complementarymore » chemical information on an atomic scale. The fine structure in the PEEL spectra can be used to investigate the local electronic structure and the nature of the bonding across the interface. In this paper we use the complimentary techniques of high resolution Z-contrast imaging and PEELS to investigate the atomic structure and chemistry of a 25{degree} symmetric tilt boundary in a bicrystal of the electroceramic SrTiO{sub 3}.« less

Effects of solutes on dislocation nucleation from grain boundaries

DOE PAGES

Borovikov, Valery; Mendelev, Mikhail I.; King, Alexander H.

2016-12-27

When grain sizes are reduced to the nanoscale, grain boundaries (GB) become the dominant sources of the dislocations that enable plastic deformation. Here, we present the first molecular dynamics (MD) study of the effect of substitutional solutes on the dislocation nucleation process from GBs during uniaxial tensile deformation. A simple bi-crystal geometry is utilized in which the nucleation and propagation of dislocations away from a GB is the only active mechanism of plastic deformation. Solutes with atomic radii both larger and smaller than the solvent atomic radius were considered. Although the segregation sites are different for the two cases, bothmore » produce increases in the stress required to nucleate a dislocation. MD simulations at room temperature revealed that this increase in the nucleation stress is associated with changes of the GB structure at the emission site caused by dislocation emission, leading to increases in the heats of segregation of the solute atoms, which cannot diffuse to lower-energy sites on the timescale of the nucleation event. These results contribute directly to understanding the strength of nanocrystalline materials, and suggest suitable directions for nanocrystalline alloy design leading toward structural applications.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yang, Hao; Lee, H. S.; Sarahan, M. C.

Grain boundaries (GBs) in complex oxides such as perovskites have been shown to readily accommodate nonstoichiometry changing the electrostatic potential at the boundary plane and effectively controlling material properties such as capacitance, magnetoresistance and superconductivity. Understanding and quantifying exactly how variations in atomic scale nonstoichiometry at the boundary plane extend to the practical mesoscale operating length of the system is therefore critical for improving the overall properties. Bicrystals of SrTiO 3 were fabricated to provide the model GB model structures that are analysed in this paper. We show that statistical analysis of aberration-corrected scanning transmission electron microscope images acquired frommore » a large area of GB is an effective routine to understanding the variation in boundary structure that occurs to accommodate nonstoichiometry. In the case of the SrTiO 3 22.6° Σ13 (510)/[100] GB analysed here, the symmetric atomic structures observed from a micron-long GB can be categorized as two different competing structural arrangements, with and without a rigid-body translation along the boundary plane. How this quantified experimental approach can provide direct insights into the GB energetics is further confirmed from the first principles density functional theory, and the effect of nonstoichiometry in determining the GB energies is quantified.« less

Molecular dynamics simulations of intergranular fracture in UO2 with nine empirical interatomic potentials

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yongfeng Zhang; Paul C Millett; Michael R Tonks

The intergranular fracture behavior of UO2 was studied using molecular dynamics simulations with a bicrystal model. The anisotropic fracture behavior due to the different grain boundary characters was investigated with the View the MathML source symmetrical tilt S5 and the View the MathML source symmetrical tilt S3 ({1 1 1} twin) grain boundaries. Nine interatomic potentials, seven rigid-ion plus two core–shell ones, were utilized to elucidate possible potential dependence. Initiating from a notch, crack propagation along grain boundaries was observed for most potentials. The S3 boundary was found to be more prone to fracture than the S5 one, indicated bymore » a lower energy release rate associated with the former. However, some potential dependence was identified on the existence of transient plastic deformation at crack tips, and the results were discussed regarding the relevant material properties including the excess energies of metastable phases and the critical energy release rate for intergranular fracture. In general, local plasticity at crack tips was observed in fracture simulations with potentials that predict low excess energies for metastable phases and high critical energy release rates for intergranular fracture.« less

Domain pinning near a single-grain boundary in tetragonal and rhombohedral lead zirconate titanate films

DOE PAGES

Marincel, Dan M.; Zhang, H. R.; Briston, J.; ...

2015-04-27

The interaction of grain boundaries with ferroelectric domain walls strongly influences the extrinsic contribution to piezoelectric activity in Pb(Zr,Ti)O 3 (PZT), ubiquitous in modern transducers and actuators. However, the fundamental understanding of these phenomena has been limited by complex mechanisms originating from the interplay of atomic-level domain wall pinning, collective domain wall dynamics, and emergent mesoscopic behavior. This contribution utilizes engineered grain boundaries created by depositing epitaxial PZT films with various Zr:Ti ratio onto 24º SrTiO 3 tilt bicrystals. The nonlinear piezoelectric response and surface domain structure across the boundary are investigated using piezoresponse force microscopy whilst cross section domainmore » structure is studied using transmission electron microscopy. The grain boundary reduces domain wall motion over a width of 800±70 nm for PZT 45:55 and 450±30 nm for PZT 52:48. Phase field modeling provides an understanding of the elastic and electric fields associated with the grain boundary and local domain configurations. In conclusion, this study demonstrates that complex mesoscopic behaviors can be explored to complement atomic-level pictures of the material system.« less

Combined measurement of surface, grain boundary and lattice diffusion coefficients on olivine bi-crystals

NASA Astrophysics Data System (ADS)

Marquardt, Katharina; Dohmen, Ralf; Wagner, Johannes

2014-05-01

Diffusion along interface and grain boundaries provides an efficient pathway and may control chemical transport in rocks as well as their mechanical strength. Besides the significant relevance of these diffusion processes for various geologic processes, experimental data are still very limited (e.g., Dohmen & Milke, 2010). Most of these data were measured using polycrystalline materials and the formalism of LeClaire (1951) to fit integrated concentration depth profiles. To correctly apply this formalism, certain boundary conditions of the diffusion problem need to be fulfilled, e.g., surface diffusion is ignored, and furthermore the lattice diffusion coefficient has to be known from other studies or is an additional fitting parameter, which produces some ambiguity in the derived grain boundary diffusion coefficients. We developed an experimental setup where we can measure the lattice and grain boundary diffusion coefficients simultaneously but independent and demonstrate the relevance of surface diffusion for typical grain boundary diffusion experiments. We performed Mg2SiO4 bicrystal diffusion experiments, where a single grain boundary is covered by a thin-film of pure Ni2SiO4 acting as diffusant source, produced by pulsed laser deposition. The investigated grain boundary is a 60° (011)/[100]. This specific grain boundary configuration was modeled using molecular dynamics for comparison with the experimental observations in the transmission electron microscope (TEM). Both, experiment and model are in good agreement regarding the misorientation, whereas there are still some disagreements regarding the strain fields along the grain boundary that are of outmost importance for the strengths of the material. The subsequent diffusion experiments were carried out in the temperature range between 800° and 1450° C. The inter diffusion profiles were measured using the TEMs energy dispersive x-ray spectrometer standardized using the Cliff-Lorimer equation and EMPA measurements. To evaluate the obtained diffusion profiles we adapted the isolated grain boundary model, first proposed by Fisher (1951) to match several observations: (i) Anisotropic diffusion in forsterite, (ii) fast diffusion along the grain boundary, (iii) fast diffusion on the surface of the sample. The latter process is needed to explain an additional flux of material from the surface into the grain boundary. Surface and grain boundary diffusion coefficients are on the order of 10000 times faster than diffusion in the lattice. Another observation was that in some regions the diffusion profiles in the lattice were greatly extended. TEM observations suggest here that surface defects (nano-cracks, ect.) have been present, which apparently enhanced the diffusion through the bulk lattice. Dohmen, R., & Milke, R. (2010). Diffusion in Polycrystalline Materials: Grain Boundaries, Mathematical Models, and Experimental Data. Reviews in Mineralogy and Geochemistry, 72(1), 921-970. Fisher, J. C. (1951). Calculations of Diffusion Penetration Curves for Surface and Grain Boundary Diffusion. Journal of Applied Physics, 22(1), 74-77. Le Claire, A. D. (1951). Grain boundary diffusion in metals. Philosophical Magazine A, 42(328), 468-474.

Paving the way to nanoionics: atomic origin of barriers for ionic transport through interfaces.

PubMed

Frechero, M A; Rocci, M; Sánchez-Santolino, G; Kumar, Amit; Salafranca, J; Schmidt, Rainer; Díaz-Guillén, M R; Durá, O J; Rivera-Calzada, A; Mishra, R; Jesse, Stephen; Pantelides, S T; Kalinin, Sergei V; Varela, M; Pennycook, S J; Santamaria, J; Leon, C

2015-12-17

The blocking of ion transport at interfaces strongly limits the performance of electrochemical nanodevices for energy applications. The barrier is believed to arise from space-charge regions generated by mobile ions by analogy to semiconductor junctions. Here we show that something different is at play by studying ion transport in a bicrystal of yttria (9% mol) stabilized zirconia (YSZ), an emblematic oxide ion conductor. Aberration-corrected scanning transmission electron microscopy (STEM) provides structure and composition at atomic resolution, with the sensitivity to directly reveal the oxygen ion profile. We find that Y segregates to the grain boundary at Zr sites, together with a depletion of oxygen that is confined to a small length scale of around 0.5 nm. Contrary to the main thesis of the space-charge model, there exists no evidence of a long-range O vacancy depletion layer. Combining ion transport measurements across a single grain boundary by nanoscale electrochemical strain microscopy (ESM), broadband dielectric spectroscopy measurements, and density functional calculations, we show that grain-boundary-induced electronic states act as acceptors, resulting in a negatively charged core. Besides the possible effect of the modified chemical bonding, this negative charge gives rise to an additional barrier for ion transport at the grain boundary.

Miniaturization of Micro-Solder Bumps and Effect of IMC on Stress Distribution

NASA Astrophysics Data System (ADS)

Choudhury, Soud Farhan; Ladani, Leila

2016-07-01

As the joints become smaller in more advanced packages and devices, intermetallic (IMCs) volume ratio increases, which significantly impacts the overall mechanical behavior of joints. The existence of only a few grains of Sn (Tin) and IMC materials results in anisotropic elastic and plastic behavior which is not detectable using conventional finite element (FE) simulation with average properties for polycrystalline material. In this study, crystal plasticity finite element (CPFE) simulation is used to model the whole joint including copper, Sn solder and Cu6Sn5 IMC material. Experimental lap-shear test results for solder joints from the literature were used to validate the models. A comparative analysis between traditional FE, CPFE and experiments was conducted. The CPFE model was able to correlate the experiments more closely compared to traditional FE analysis because of its ability to capture micro-mechanical anisotropic behavior. Further analysis was conducted to evaluate the effect of IMC thickness on stress distribution in micro-bumps using a systematic numerical experiment with IMC thickness ranging from 0% to 80%. The analysis was conducted on micro-bumps with single crystal Sn and bicrystal Sn. The overall stress distribution and shear deformation changes as the IMC thickness increases. The model with higher IMC thickness shows a stiffer shear response, and provides a higher shear yield strength.

Paving the way to nanoionics: Atomic origin of barriers for ionic transport through interfaces

DOE PAGES

Frechero, M. A.; Rocci, M.; Sanchez-Santolino, G.; ...

2015-12-17

The blocking of ion transport at interfaces strongly limits the performance of electrochemical nanodevices for energy applications. The barrier is believed to arise from space-charge regions generated by mobile ions by analogy to semiconductor junctions. Here we show that something different is at play by studying ion transport in a bicrystal of yttria (9% mol) stabilized zirconia (YSZ), an emblematic oxide ion conductor. Aberration-corrected scanning transmission electron microscopy (STEM) provides structure and composition at atomic resolution, with the sensitivity to directly reveal the oxygen ion profile. We find that Y segregates to the grain boundary at Zr sites, together withmore » a depletion of oxygen that is confined to a small length scale of around 0.5 nm. Contrary to the main thesis of the space-charge model, there exists no evidence of a long-range O vacancy depletion layer. Combining ion transport measurements across a single grain boundary by nanoscale electrochemical strain microscopy (ESM), broadband dielectric spectroscopy measurements, and density functional calculations, we show that grain-boundary-induced electronic states act as acceptors, resulting in a negatively charged core. In conclusion, besides the possible effect of the modified chemical bonding, this negative charge gives rise to an additional barrier for ion transport at the grain boundary.« less

Stress Distribution During Deformation of Polycrystalline Aluminum by Molecular-Dynamics and Finite-Element Modeling

NASA Technical Reports Server (NTRS)

Yamakov, V.; Saether, E.; Phillips, D.; Glaessgen, E. H.

2004-01-01

In this paper, a multiscale modelling strategy is used to study the effect of grain-boundary sliding on stress localization in a polycrystalline microstructure with an uneven distribution of grain size. The development of the molecular dynamics (MD) analysis used to interrogate idealized grain microstructures with various types of grain boundaries and the multiscale modelling strategies for modelling large systems of grains is discussed. Both molecular-dynamics and finite-element (FE) simulations for idealized polycrystalline models of identical geometry are presented with the purpose of demonstrating the effectiveness of the adapted finite-element method using cohesive zone models to reproduce grain-boundary sliding and its effect on the stress distribution in a polycrystalline metal. The yield properties of the grain-boundary interface, used in the FE simulations, are extracted from a MD simulation on a bicrystal. The models allow for the study of the load transfer between adjacent grains of very different size through grain-boundary sliding during deformation. A large-scale FE simulation of 100 grains of a typical microstructure is then presented to reveal that the stress distribution due to grain-boundary sliding during uniform tensile strain can lead to stress localization of two to three times the background stress, thus suggesting a significant effect on the failure properties of the metal.

Landau levels and SdH-oscillations of the quasi two-dimensional electron gas at grain boundaries and near heterojunctions

NASA Astrophysics Data System (ADS)

Paasch, G.; Gobsch, G.; Schulze, D.; Handschack, S.

1989-04-01

For the quasi two-dimensional (Q2D) electron gas important experimental information is obtained from magnetotransport measurements with a perpendicular magnetic field. The energy spectrum consists of series of Landau levels for each electric subband. There still exist several open questions if two or more electric Subbands are populated. Results are presented here for this situation. The usual procedure for interpreting Shubnikov-de Haas (SdH) measurements for the case of several populated subbands is analyzed (connection with the saw-tooth like Fermi energy as a function of the magnetic field). The transverse magnetoresistance is calculated for the Q2D electron gas in InSb-bicrystals and at InGaAs-InP heterojunctions. All details of the experimental curves can be explained including an anomalous behaviour of the quantum Hall effect (QHE) in the second system. Basic assumptions of the theory are the broadening of the Landau levels and in addition a background of localized states in the second case. The dependence of the electronic structure on the perpendicular magnetic field is discussed qualitatively. First results of magnetic field dependent self-consistent calculations for inversion layers are presented. It is shown for the first time that this magnetic field dependence causes qualitative changes of the Landau level spectrum.

Terahertz Josephson spectral analysis and its applications

NASA Astrophysics Data System (ADS)

Snezhko, A. V.; Gundareva, I. I.; Lyatti, M. V.; Volkov, O. Y.; Pavlovskiy, V. V.; Poppe, U.; Divin, Y. Y.

2017-04-01

Principles of Hilbert-transform spectral analysis (HTSA) are presented and advantages of the technique in the terahertz (THz) frequency range are discussed. THz HTSA requires Josephson junctions with high values of characteristic voltages I c R n and dynamics described by a simple resistively shunted junction (RSJ) model. To meet these requirements, [001]- and [100]-tilt YBa2Cu3O7-x bicrystal junctions with deviations from the RSJ model less than 1% have been developed. Demonstrators of Hilbert-transform spectrum analyzers with various cryogenic environments, including integration into Stirling coolers, are described. Spectrum analyzers have been characterized in the spectral range from 50 GHz to 3 THz. Inside a power dynamic range of five orders, an instrumental function of the analyzers has been found to have a Lorentz form around a single frequency of 1.48 THz with a spectral resolution as low as 0.9 GHz. Spectra of THz radiation from optically pumped gas lasers and semiconductor frequency multipliers have been studied with these spectrum analyzers and the regimes of these radiation sources were optimized for a single-frequency operation. Future applications of HTSA will be related with quick and precise spectral characterization of new radiation sources and identification of substances in the THz frequency range.

Gradient plasticity for thermo-mechanical processes in metals with length and time scales

NASA Astrophysics Data System (ADS)

Voyiadjis, George Z.; Faghihi, Danial

2013-03-01

A thermodynamically consistent framework is developed in order to characterize the mechanical and thermal behavior of metals in small volume and on the fast transient time. In this regard, an enhanced gradient plasticity theory is coupled with the application of a micromorphic approach to the temperature variable. A physically based yield function based on the concept of thermal activation energy and the dislocation interaction mechanisms including nonlinear hardening is taken into consideration in the derivation. The effect of the material microstructural interface between two materials is also incorporated in the formulation with both temperature and rate effects. In order to accurately address the strengthening and hardening mechanisms, the theory is developed based on the decomposition of the mechanical state variables into energetic and dissipative counterparts which endowed the constitutive equations to have both energetic and dissipative gradient length scales for the bulk material and the interface. Moreover, the microstructural interaction effect in the fast transient process is addressed by incorporating two time scales into the microscopic heat equation. The numerical example of thin film on elastic substrate or a single phase bicrystal under uniform tension is addressed here. The effects of individual counterparts of the framework on the thermal and mechanical responses are investigated. The model is also compared with experimental results.

Evidence for preferential flux flow at the grain boundaries of superconducting RF-quality niobium

NASA Astrophysics Data System (ADS)

Sung, Z.-H.; Lee, P. J.; Gurevich, A.; Larbalestier, D. C.

2018-04-01

The question of whether grain boundaries (GBs) in niobium can be responsible for lowered operating field (B RF) or quality factor (Q 0) in superconducting radio frequency (SRF) cavities is still controversial. Here, we show by direct DC transport across planar GBs isolated from a slice of very large-grain SRF-quality Nb that vortices can preferentially flow along the grain boundary when the external magnetic field lies in the GB plane. However, increasing the misalignment between the GB plane and the external magnetic field vector markedly reduces preferential flux flow along the GB. Importantly, we find that preferential GB flux flow is more prominent for a buffered chemical polished than for an electropolished bi-crystal. The voltage-current characteristics of GBs are similar to those seen in low angle grain boundaries of high temperature superconductors where there is clear evidence of suppression of the superconducting order parameter at the GB. While local weakening of superconductivity at GBs in cuprates and pnictides is intrinsic, deterioration of current transparency of GBs in Nb appears to be extrinsic, since the polishing method clearly affect the local GB degradation. The dependence of preferential GB flux flow on important cavity preparation and experimental variables, particularly the final chemical treatment and the angle between the magnetic field and the GB plane, suggests two more reasons why real cavity performance can be so variable.

Large grain CBMM Nb ingot slices: An ideal test bed for exploring the microstructure-electromagnetic property relationships relevant to SRF

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sung, Zu-Hawn, E-mail: ZSung@uss.com; Now at US-Steel, Pittsburgh, US; Lee, Peter J., E-mail: lee@asc.magnet.fsu.edu

2015-12-04

High purity (RRR > 200), large grain (> 5-10 cm) niobium ingot slices have been successfully used to fabricate radio frequency (RF) cavities for particle accelerators. They offer significantly reduced fabrication cost by eliminating processing steps and furthermore they provide the opportunity to study the influence of individual grain boundaries in SRF Nb. Here we summarize our measurements of grain boundary (GB) effects on the superconducting properties of large grain high purity niobium sheet manufactured by CBMM. We show by magneto-optical (MO) imaging that GBs allow premature flux penetration, but only when they are oriented close to the direction of themore » magnetic field. However, even low angle GBs produced by minor deformations commensurate with half-cell forming produce localized flux penetration. The transport properties of grain boundaries were investigated by direct transport across them and evidence for preferential vortex flow along the GBs of SRF Nb was observed for the first time. Using transmission electron microscopy (TEM) and micro crystallographic analysis with electron backscattered diffraction (EBSD), we were able to quantitatively characterize surface substructures that can lead to localized thermal breakdown of superconductivity. Important to these studies was the development of sample preparation techniques that made the cutout single, bi-crystal and tri-crystal Nb coupons as representative as possible of the surface properties of cavities manufactured by standard techniques.« less

A simple and inclusive method to determine the habit plane in transmission electron microscope based on accurate measurement of foil thickness

DOE Office of Scientific and Technical Information (OSTI.GOV)

Qiu, Dong, E-mail: d.qiu@uq.edu.au; Zhang, Mingxing

2014-08-15

A simple and inclusive method is proposed for accurate determination of the habit plane between bicrystals in transmission electron microscope. Whilst this method can be regarded as a variant of surface trace analysis, the major innovation lies in the improved accuracy and efficiency of foil thickness measurement, which involves a simple tilt of the thin foil about a permanent tilting axis of the specimen holder, rather than cumbersome tilt about the surface trace of the habit plane. Experimental study has been done to validate this proposed method in determining the habit plane between lamellar α{sub 2} plates and γ matrixmore » in a Ti–Al–Nb alloy. Both high accuracy (± 1°) and high precision (± 1°) have been achieved by using the new method. The source of the experimental errors as well as the applicability of this method is discussed. Some tips to minimise the experimental errors are also suggested. - Highlights: • An improved algorithm is formulated to measure the foil thickness. • Habit plane can be determined with a single tilt holder based on the new algorithm. • Better accuracy and precision within ± 1° are achievable using the proposed method. • The data for multi-facet determination can be collected simultaneously.« less

Large grain CBMM Nb ingot slices: An ideal test bed for exploring the microstructure-electromagnetic property relationships relevant to SRF

DOE PAGES

Sung, Zu -Hawn; Lee, Peter J.; Polyanskii, Anatolii; ...

2015-12-04

High purity (RRR > 200), large grain (> 5-10 cm) niobium ingot slices have been successfully used to fabricate radio frequency (RF) cavities for particle accelerators. In addition, they offer significantly reduced fabrication cost by eliminating processing steps and furthermore they provide the opportunity to study the influence of individual grain boundaries in SRF Nb. Here we summarize our measurements of grain boundary (GB) effects on the superconducting properties of large grain high purity niobium sheet manufactured by CBMM. We show by magneto-optical (MO) imaging that GBs allow premature flux penetration, but only when they are oriented close to themore » direction of the magnetic field. However, even low angle GBs produced by minor deformations commensurate with half-cell forming produce localized flux penetration. The transport properties of grain boundaries were investigated by direct transport across them and evidence for preferential vortex flow along the GBs of SRF Nb was observed for the first time. Using transmission electron microscopy (TEM) and micro crystallographic analysis with electron backscattered diffraction (EBSD), we were able to quantitatively characterize surface substructures that can lead to localized thermal breakdown of superconductivity. Important to these studies was the development of sample preparation techniques that made the cut-out single, bi-crystal and tri-crystal Nb coupons as representative as possible of the surface properties of cavities manufactured by standard techniques.« less

Faceting of {sigma}3 and {sigma}9 grain boundaries in Cu-Bi alloys

DOE Office of Scientific and Technical Information (OSTI.GOV)

Straumal, B.B.; Polyakov, S.A.; Max-Planck-Institut fuer Metallforschung and Institut fuer Metallkunde, Heisenbergstr. 3, 70569 Stuttgart

2005-01-10

The faceting of {sigma}3 and {sigma}9 tilt grain boundaries (GBs) has been studied in bicrystals of pure Cu and Cu-Bi alloys containing 2.5 x 10{sup -3}, 10 x 10{sup -3} and 16 x 10{sup -3} at.% Bi. The {sigma}3(1 0 0), {sigma}9(1 0 0), {sigma}9(-1 1 0), and {sigma}9(-1 2 0) facets and non-CSL {sigma}3 82 deg 9R facet were observed, where {sigma} is the inverse density of coincidence sites. The ratio between GB energy, {sigma}{sub GB}, and surface energy, {sigma}{sub sur}, was measured by atomic force microscopy using the GB thermal-groove method. The GB energy and thermal-groove deepening ratemore » increased slightly between 0 and 10 x 10{sup -3} at.% Bi for all facets studied. However, between 10 x 10{sup -3} and 16 x 10{sup -3} at.% Bi the GB energy increased dramatically [from a factor 2 for the {sigma}9(1 1 0) facet to 15 times larger for the {sigma}3(1 0 0) facet]. The thermal-groove deepening rate also increased by a factor of 10 in this concentration range. This change corresponds well with the GB solidus line (i.e., the formation of a stable layer of a liquid-like GB phase called GB prewetting) observed previously. Wulff diagrams were constructed using measured {sigma}{sub GB}/{sigma}{sub sur} values.« less

Evidence for preferential flux flow at the grain boundaries of superconducting RF-quality niobium

DOE PAGES

Sung, Z. -H.; Lee, P. J.; Gurevich, A.; ...

2018-02-19

Here, the question of whether grain boundaries (GBs) in niobium can be responsible for lowered operating field (B RF) or quality factor (Q 0) in superconducting radio-frequency (SRF) cavities is still controversial. Here, we show by direct DC transport across planar grain boundaries isolated from a slice of very large-grain SRF-quality Nb that vortices can preferentially flow along the grain boundary when the external magnetic field lies in the GB plane. However, increasing the misalignment between the GB plane and the external magnetic field vector markedly reduces preferential flux flow along GB. Importantly, we find that preferential GB flux flowmore » is more prominent for a buffered chemical polished than for an electropolished bi-crystal. The voltage-current characteristics of GBs are similar to those seen in low angle grain boundaries of high temperature superconductors where there is clear evidence of suppression of the superconducting order parameter at the GB. While local weakening of superconductivity at GBs in cuprates and pnictides is intrinsic, deterioration of current transparency of GBs in Nb appears to be extrinsic, since the polishing method clearly affect the local GB degradation. The dependence of preferential GB flux flow on important cavity preparation and experimental variables, particularly, the final chemical treatment and the angle between the magnetic field and the GB plane, suggests two more reasons why real cavity performance can be so variable.« less

Evidence for preferential flux flow at the grain boundaries of superconducting RF-quality niobium

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sung, Z. -H.; Lee, P. J.; Gurevich, A.

Here, the question of whether grain boundaries (GBs) in niobium can be responsible for lowered operating field (B RF) or quality factor (Q 0) in superconducting radio-frequency (SRF) cavities is still controversial. Here, we show by direct DC transport across planar grain boundaries isolated from a slice of very large-grain SRF-quality Nb that vortices can preferentially flow along the grain boundary when the external magnetic field lies in the GB plane. However, increasing the misalignment between the GB plane and the external magnetic field vector markedly reduces preferential flux flow along GB. Importantly, we find that preferential GB flux flowmore » is more prominent for a buffered chemical polished than for an electropolished bi-crystal. The voltage-current characteristics of GBs are similar to those seen in low angle grain boundaries of high temperature superconductors where there is clear evidence of suppression of the superconducting order parameter at the GB. While local weakening of superconductivity at GBs in cuprates and pnictides is intrinsic, deterioration of current transparency of GBs in Nb appears to be extrinsic, since the polishing method clearly affect the local GB degradation. The dependence of preferential GB flux flow on important cavity preparation and experimental variables, particularly, the final chemical treatment and the angle between the magnetic field and the GB plane, suggests two more reasons why real cavity performance can be so variable.« less

Characterization of etch pits found on a large-grain bulk niobium superconducting radio-frequency resonant cavity

DOE PAGES

Zhao, Xin; Ciovati, G.; Bieler, T. R.

2010-12-15

The performance of superconducting radio-frequency (SRF) resonant cavities made of bulk niobium is limited by nonlinear localized effects. Surface analysis of regions of higher power dissipation is thus of intense interest. Such areas (referred to as “hotspots”) were identified in a large-grain single-cell cavity that had been buffered-chemical polished and dissected for examination by high resolution electron microscopy, electron backscattered diffraction microscopy (EBSD), and optical microscopy. Pits with clearly discernible crystal facets were observed in both “hotspot” and “coldspot” specimens. The pits were found in-grain, at bicrystal boundaries, and on tricrystal junctions. They are interpreted as etch pits induced bymore » crystal defects (e.g. dislocations). All coldspots examined had a qualitatively lower density of etch pits or relatively smooth tricrystal boundary junctions. EBSD mapping revealed the crystal orientation surrounding the pits. Locations with high pit density are correlated with higher mean values of the local average misorientation angle distributions, indicating a higher geometrically necessary dislocation content. In addition, a survey of the samples by energy dispersive x-ray analysis did not show any significant contamination of the samples’ surface. In conclusion, the local magnetic field enhancement produced by the sharp-edge features observed on the samples is not sufficient to explain the observed degradation of the cavity quality factor, which starts at peak surface magnetic field as low as 20 mT.« less

A phase field dislocation dynamics model for a bicrystal interface system: An investigation into dislocation slip transmission across cube-on-cube interfaces

DOE PAGES

Zeng, Y.; Hunter, A.; Beyerlein, I. J.; ...

2015-09-14

In this study, we present a phase field dislocation dynamics formulation designed to treat a system comprised of two materials differing in moduli and lattice parameters that meet at a common interface. We apply the model to calculate the critical stress τ crit required to transmit a perfect dislocation across the bimaterial interface with a cube-on-cube orientation relationship. The calculation of τ crit accounts for the effects of: 1) the lattice mismatch (misfit or coherency stresses), 2) the elastic moduli mismatch (Koehler forces or image stresses), and 3) the formation of the residual dislocation in the interface. Our results showmore » that the value of τ crit associated with the transmission of a dislocation from material 1 to material 2 is not the same as that from material 2 to material 1. Dislocation transmission from the material with the lower shear modulus and larger lattice parameter tends to be easier than the reverse and this apparent asymmetry in τ crit generally increases with increases in either lattice or moduli mismatch or both. In efforts to clarify the roles of lattice and moduli mismatch, we construct an analytical model for τcrit based on the formation energy of the residual dislocation. We show that path dependence in this energetic barrier can explain the asymmetry seen in the calculated τ crit values.« less

Grain boundary grooving induced by the anisotropic surface drift diffusion driven by the capillary and electromigration forces: Simulations

NASA Astrophysics Data System (ADS)

Akyildiz, Oncu; Omer Ogurtani, Tarik

2011-08-01

The morphological evolution kinetics of a bicrystal thin film induced by anisotropic surface drift diffusion and driven by the applied electrostatic field is investigated via self consistent dynamical computer simulations. The physico-mathematical model, which is based upon the irreversible thermodynamic treatment of surfaces and interfaces with singularities [T. O. Ogurtani, J. Chem. Phys. 124, 144706 (2006)], provided us with auto-control on the otherwise free-motion of the triple junction at the intersection of the grooving surface and the grain boundary, without having any a priori assumption on the equilibrium dihedral angles. The destruction of the symmetry of the freshly formed grain boundary grooves under the anisotropic surface diffusion driven by the concurrent action of the capillarity and electromigration is observed. After prolonged exposure times the applied electric field above the well defined threshold level modifies Mullins' familiar stationary state time law as, t¯1/4, and causes the premature termination of the groove penetration because of the current crowding at the tips of counteracting grain boundary-grooves initiated on both sides of the test modulus. That finding indicates that the electromigration plays the same role as a healing agent [T. O. Ogurtani, J. Appl. Phys. 106, 053503 (2009)] in arresting the thermal grooving, thereby avoiding the premature interconnect failure as in the case of surface roughening and crack initiation caused by compressive stress gradients. The role of the electromigration and wetting parameter on the ridge/slit formations are thoroughly investigated in this study and the prerequisite conditions are also identified.

The Material Point Method and Simulation of Wave Propagation in Heterogeneous Media

NASA Astrophysics Data System (ADS)

Bardenhagen, S. G.; Greening, D. R.; Roessig, K. M.

2004-07-01

The mechanical response of polycrystalline materials, particularly under shock loading, is of significant interest in a variety of munitions and industrial applications. Homogeneous continuum models have been developed to describe material response, including Equation of State, strength, and reactive burn models. These models provide good estimates of bulk material response. However, there is little connection to underlying physics and, consequently, they cannot be applied far from their calibrated regime with confidence. Both explosives and metals have important structure at the (energetic or single crystal) grain scale. The anisotropic properties of the individual grains and the presence of interfaces result in the localization of energy during deformation. In explosives energy localization can lead to initiation under weak shock loading, and in metals to material ejecta under strong shock loading. To develop accurate, quantitative and predictive models it is imperative to develop a sound physical understanding of the grain-scale material response. Numerical simulations are performed to gain insight into grain-scale material response. The Generalized Interpolation Material Point Method family of numerical algorithms, selected for their robust treatment of large deformation problems and convenient framework for implementing material interface models, are reviewed. A three-dimensional simulation of wave propagation through a granular material indicates the scale and complexity of a representative grain-scale computation. Verification and validation calculations on model bimaterial systems indicate the minimum numerical algorithm complexity required for accurate simulation of wave propagation across material interfaces and demonstrate the importance of interfacial decohesion. Preliminary results are presented which predict energy localization at the grain boundary in a metallic bicrystal.

Atomistically derived cohesive zone model of intergranular fracture in polycrystalline graphene

DOE Office of Scientific and Technical Information (OSTI.GOV)

Guin, Laurent; Department of Mechanical Engineering, Columbia University, New York, New York 10027; Raphanel, Jean L.

2016-06-28

Pristine single crystal graphene is the strongest known two-dimensional material, and its nonlinear anisotropic mechanical properties are well understood from the atomic length scale up to a continuum description. However, experiments indicate that grain boundaries in the polycrystalline form reduce the mechanical behavior of polycrystalline graphene. Herein, we perform atomistic-scale molecular dynamics simulations of the deformation and fracture of graphene grain boundaries and express the results as continuum cohesive zone models (CZMs) that embed notions of the grain boundary ultimate strength and fracture toughness. To facilitate energy balance, we employ a new methodology that simulates a quasi-static controlled crack propagationmore » which renders the kinetic energy contribution to the total energy negligible. We verify good agreement between Griffith's critical energy release rate and the work of separation of the CZM, and we note that the energy of crack edges and fracture toughness differs by about 35%, which is attributed to the phenomenon of bond trapping. This justifies the implementation of the CZM within the context of the finite element method (FEM). To enhance computational efficiency in the FEM implementation, we discuss the use of scaled traction-separation laws (TSLs) for larger element sizes. As a final result, we have established that the failure characteristics of pristine graphene and high tilt angle bicrystals differ by less than 10%. This result suggests that one could use a unique or a few typical TSLs as a good approximation for the CZMs associated with the mechanical simulations of the polycrystalline graphene.« less

Modeling collective behavior of dislocations in crystalline materials

NASA Astrophysics Data System (ADS)

Varadhan, Satya N.

Elastic interaction of dislocations leads to collective behavior and determines plastic response at the mesoscale. Notable characteristics of mesoscale plasticity include the formation of dislocation patterns, propagative instability phenomena due to strain aging such as the Luders and Portevin-Le Chatelier effects, and size-dependence of low stress. This work presents a unified approach to modeling collective behavior based on mesoscale field dislocation mechanics and crystal plasticity, using constitutive models with physical basis. Successful application is made to: compression of a bicrystal, where "smaller is stronger"---the flow stress increases as the specimen size is reduced; torsional creep of ice single crystals, where the plastic strain rate increases with time under constant applied torque; strain aging in a single crystal alloy, where the transition from homogeneous deformation to intermittent bands to continuous band is captured as the applied deformation rate is increased. A part of this work deals with the kinematics of dislocation density evolution. An explicit Galerkin/least-squares formulation is introduced for the quasilinear evolution equation, which leads to a symmetric and well-conditioned system of equations with constant coefficients, making it attractive for large-scale problems. It is shown that the evolution equation simplifies to the Hamilton-Jacobi equations governing geometric optics and level set methods in the following physical contexts: annihilation of dislocations, expansion of a polygonal dislocation loop and operation of a Frank-Read source. The weak solutions to these equations are not unique, and the numerical method is able to capture solutions corresponding to shock as well as expansion fans.

Surface film effects on drop tube undercooling studies

NASA Technical Reports Server (NTRS)

Ethridge, E. C.; Kaukler, W. F.

1986-01-01

The effects of various gaseous atmospheric constituents on drop-tube solidified samples of elemental metals were examined from a microstructural standpoint. All specimens were prepared from the purest available elements, so effects of impurities should not account for the observed effects. The drop-tube gas has a definite effect on the sample microstructure. Most dramatically, the sample cooling rate is effected. Some samples receive sufficient cooling to solidify in free fall while others do not, splating at the end of the drop tube in the sample catcher. Gases are selectively absorbed into the sample. Upon solidification gas can become less soluble and as a result forms voids within the sample. The general oxidation/reduction characteristics of the gas also affect sample microstructures. In general, under the more favorable experimental conditions including reducing atmospheric conditions and superheatings, examination of sample microstructures indicates that nucleation has been suppressed. This is indicated by underlying uniform dendrite spacings throughout the sample and with a single dendrite orientation through most of the sample. The samples were annealed yielding a few large grains and single or bi-crystal samples were commonly formed. This was especially true of samples that were inadvertently greatly superheated. This is in contrast with results from a previous study in which surface oxides were stable and contained numerous sites of nucleation. The number of nucleation events depends upon the surface state of the specimen as determined by the atmosphere and is consistent with theoretical expectations based upon the thermodynamic stability of surface oxide films. Oxide-free specimens are characterized by shiny surfaces, with no observable features under the scanning electron microscope at 5000X.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Regan, S.P.

This volume of the LLE Review, covering the period October--December 1998, includes two articles addressing issues applicable to direct-drive ICF on the National Ignition Facility (NIF): laser-plasma interactions and laser-irradiation uniformity. Additional highlights of the research presented in this issue are: (1) P.B. Radha and S. Skupsky present a novel charged-particle diagnostic that performs simultaneous {rho}R measurements of the fuel, shell, and ablator regions of a compressed ICF target, consisting of an inner DT fuel region, a plastic (CH) shell, and an ablator (CD), by measuring the knock-on deuteron spectrum. (2) F. Dahmani, S. Burns, J. Lambropoulos, S. Papernov, andmore » A. Schmid report results from stress-inhibited laser-driven crack propagation and stress-delayed damage-initiation experiments in fused silica at 351 nm. Research is underway presently to determine the ramifications of these findings for large-aperture systems, such as OMEGA. (3) V. Goncharov presents an analytic theory of the ablative Richtmyer-Meshkov instability, which shows that the main stabilizing mechanism of the ablation-front perturbations is the dynamic overpressure of the blowoff plasma with respect to the target material. The perturbation evolution during the shock transit time is studied to determine the initial conditions for the Rayleigh-Taylor phase of the instability and to analyze the level of laser imprint on ICF direct-drive targets. (4) J.M. Larkin, W.R. Donaldson, T.H. Foster, and R.S. Knox examine the triplet state of rose bengal, a dye used in photodynamic therapy, that is produced by 1,064-nm excitation of T{sub 1}. (5) R. Adam, M. Currie, R. Sobolewski, O. Harnack, and M. Darula report measurements of the picosecond photoresponse of a current-biased YBCO microbridge coupled to a bicrystal YBCO Josephson junction.« less

Laser Crystallization of Silicon Thin Films for Three-Dimensional Integrated Circuits

NASA Astrophysics Data System (ADS)

Ganot, Gabriel S.

Advanced sequential lateral solidification (SLS), as presented in this thesis, is a novel implementation of the previously-developed directional-SLS method, and is specifically aimed at addressing the microstructural non-uniformity issue that can be encountered in the directional solidification processing of continuous Si films. Films crystallized via the directional-SLS method, for instance, can contain physically distinct regions with varying densities of planar defects and/or crystallographic orientations. As a result, transistors fabricated within such films can potentially exhibit relatively poor device uniformity. To address this issue, we employ advanced SLS whereby Si films are prepatterned into closely-spaced, long, narrow stripes that are then crystallized via directional-SLS in the long-axis-direction of the stripe length. By doing so, one can create microstructurally distinct regions within each stripe, which are then placed within the active channel region of a device. It is shown that when the stripes are sufficiently narrow (less than 2 µm), a bi-crystal microstructure is observed. This is explained based on the change in the interface morphology as a consequence of enhanced heat flow at the edges of the stripe. It is suggested that this bi-crystal formation is beneficial to the approach, as it increases the effective number of stripes within the active channel region. One issue of fundamental and technological significance that is nearly always encountered in laser crystallization is the formation of structural defects, in general, and in particular, twins. Due to the importance of reducing the density of these defects in order to increase the performance of transistors, this thesis investigates the formation mechanism of twins in rapidly laterally solidified Si thin films. These defects have been characterized and examined in the past, but a physically consistent explanation has not yet been provided. To address this situation, we have carried out experiments using a particular version of SLS, namely dot-SLS. This specific technique is chosen because we identify that it is endowed with a fortuitous combination of experimental factors that enable the systematic examination of twinning in laterally grown Si thin films. Based on extensive microstructural analysis of dot-SLS-crystallized regions, we propose that it is the energetics associated with forming a new atomic layer (during growth) in either a twinned or non-twinned configuration heterogeneously at the oxide/film interface that dictate the formation (or absence) of twins. The second method presented in this thesis is that of advanced MPS. The basic MPS approach was originally conceived as a way to generate Si films for solar cells as it is capable of producing large, intragrain-defect-free regions that are predominantly (100) surface-textured. However, the location of the grain boundaries of these equiaxed grains is essentially random, and hence, transistors placed within the interior of the grains would exhibit differing performance compared to those that are place across the grain boundaries. To address this, advanced MPS is introduced and demonstrated as a means to manipulate solidification by seeding from {100} surface-oriented regions and to induce limited directional growth. This is accomplished using a continuous-wave laser with a Gaussian-shaped beam profile wherein a central, completely molten region is surrounded by a "mixed-phase-region'' undergoing MPS. The technique creates quasi-directional material that consists of large, elongated, parallel, {100} surface-oriented grains. This material is an improvement over previously generated directionally solidified materials, and can allow one to build devices without high angle grain boundaries that are within, and oriented perpendicular to, the active channel. The resulting microstructure is explained in terms of the non-uniform energy density distribution generated by the Gaussian-shaped laser beam, and the corresponding shape and growth of the solid/liquid interface. Based on the observations and considerations from these results, we propose and demonstrate a related scheme whereby a flash-lamp annealing system is utilized in order to induce the advanced MPS condition. This method can potentially time-efficiently crystallize, and create in the process, well-defined regions that are microstructurally suitable for the fabrication of 3D-ICs. (Abstract shortened by UMI.).

Effect of natural homointerfaces on the magnetic properties of pseudomorphic La0.7Sr0.3MnO3 thin film: Phase separation vs split domain structure

NASA Astrophysics Data System (ADS)

Congiu, Francesco; Sanna, Carla; Maritato, Luigi; Orgiani, Pasquale; Geddo Lehmann, Alessandra

2016-12-01

We studied the effect of naturally formed homointerfaces on the magnetic and electric transport behavior of a heavily twinned, 40 nm thick, pseudomorphic epitaxial film of La0.7Sr0.3MnO3 deposited by molecular beam epitaxy on ferroelastic LaAlO3(001) substrate. As proved by high resolution X-ray diffraction analysis, the lamellar twin structure of the substrate is imprinted in La0.7Sr0.3MnO3. In spite of the pronounced thermomagnetic irreversibility in the DC low field magnetization, spin-glass-like character, possibly related to the structural complexity, was ruled out, on the base of AC susceptibility results. The magnetic characterization indicates anisotropic ferromagnetism, with a saturation magnetization Ms = 3.2 μB/Mn, slightly reduced with respect to the fully polarized value of 3.7 μB/Mn. The low field DC magnetization vs temperature is non bulklike, with a two step increase in the field cooled MFC(T) branch and a two peak structure in the zero field cooled MZFC(T) one. Correspondingly, two peaks are present in the resistivity vs temperature ρ(T) curve. With reference to the behavior of epitaxial manganites deposited on bicrystal substrates, results are discussed in terms of a two phase model, in which each couple of adjacent ferromagnetic twin cores, with bulklike TC = 370 K, is separated by a twin boundary with lower Curie point TC = 150 K, acting as barrier for spin polarized transport. The two phase scenario is compared with the alternative one based on a single ferromagnetic phase with the peculiar ferromagnetic domains structure inherent to twinned manganites films, reported to be split into interconnected and spatially separated regions with in-plane and out-of-plane magnetization, coinciding with twin cores and twin boundaries respectively.

Evolution of displacement cascades in Fe-Cr structures with different [001] tilt grain boundaries

NASA Astrophysics Data System (ADS)

Abu-Shams, M.; Haider, W.; Shabib, I.

2017-06-01

Reduced-activation ferritic/martensitic steels of Cr concentration between 2.25 and 12 wt% are candidate structural materials for next-generation nuclear reactors. In this study, molecular dynamics (MD) simulation is used to generate the displacement cascades in Fe-Cr structures with different Cr concentrations by using different primary knock-on atom (PKA) energies between 2 and 10 keV. A concentration-dependent model potential has been used to describe the interactions between Fe and Cr. Single crystals (SCs) of three different coordinate bases (e.g. [310], [510], and [530]) and bi-crystal (BC) structures with three different [001] tilt grain boundaries (GBs) (e.g. Σ5, Σ13, and Σ17) have been simulated. The Wigner-Seitz cell criterion has been used to identify the produced Frenkel pairs. The results show a marked difference between collisions observed in SCs and those in BC structures. The numbers of vacancies and interstitials are found to be significantly higher in BC structures than those found in SCs. The number of point defects exhibits a power relationship with the PKA energies; however, the Cr concentration does not seem to have any influence on the number of survived point defects. In BC models, a large fraction of the total survived point defects (between 59% and 93%) tends accumulate at the GBs, which seem to trap the generated point defects. The BC structure with Σ17 GB is found to trap more defects than Σ5 and Σ13 GBs. The defect trapping is found to be dictated by the crystallographic parameters of the GBs. For all studied GBs, self-interstitial atoms (SIAs) are easily trapped within the GB region than vacancies. An analysis of defect composition reveals an enrichment of Cr in SIAs, and in BC cases, more than half of the Cr-SIAs are found to be located within the GB region.

Low-temperature silicon thin films for large-area electronics: Device fabrication using soft lithography and laser-crystallization by sequential lateral solidification

NASA Astrophysics Data System (ADS)

Jin, Hyun-Chul

This work demonstrates possible routes for fabricating large-area electronic devices on glass or plastic substrates using low-temperature materials deposition and soft lithographic device patterning. Hydrogenated amorphous silicon (a-Si:H) and polycrystalline silicon (poly-Si) have been extensively studied as the semiconducting material for flat panel displays and solar cells. On glass substrates, we have deposited a-Si:H films at a temperature lower than 125°C, and we have used pulsed excimer laser crystallization in the sequential lateral solidification (SLS) regime to fabricate poly-Si films. We use micromolding in capillaries (MIMIC), a form of soft lithography involving micrometer-scale polymer molding, as a means to fabricate amorphous silicon thin-film transistors (TFTs), and photoconductive sensor arrays on both planar and curved substrates. The use of non-planar substrates has captured considerable attention in the field because it would open up new applications and new designs. Field-effect transistors made by SLS poly-Si show excellent mobility and on/off current ratio; however, the microstructure of the material had never been well documented. We determined the microtexture using electron backscattering diffraction (EBSD): the first crystallites formed in the a-Si layer are random; along the direction of the solidification, a strong <100> in-plane orientation quickly develops due to competitive growth and occlusion. The misorientation angle between neighboring grains is also analyzed. A large fraction of the boundaries within the material are low-angle and coincidence site lattice (CSL) types. We discuss the implications of the findings on the defect generation mechanism and on the electrical properties of the films. We have analyzed the electrical properties of SLS poly-Si films on oxidized Si wafer using the pseudo-MOSFET geometry; the majority carrier mobility is extracted from the transconductance. However, the data are non-ideal due to large contact resistance and current spreading. We discuss the future use of these electrical characterization techniques to analyze the properties of individual grain boundaries in thin film Si bicrystals formed by SLS.

Defects in electro-optically active polymer solids

NASA Technical Reports Server (NTRS)

Martin, David C.

1993-01-01

There is considerable current interest in the application of organic and polymeric materials for electronic and photonic devices. The rapid, non-linear optical (NLO) response of these materials makes them attractive candidates for waveguides, interferometers, and frequency doublers. In order to realize the full potential of these systems, it is necessary to develop processing schemes which can fabricate these molecules into ordered arrangements. There is enormous potential for introducing well-defined, local variations in microstructure to control the photonic properties of organic materials by rational 'defect engineering.' This effort may eventually become as technologically important as the manipulation of the electronic structure of solid-state silicon based devices is at present. The success of this endeavor will require complimentary efforts in the synthesis, processing, and characterization of new materials. Detailed information about local microstructure will be necessary to understand the influence of symmetry breaking of the solid phases near point, line, and planar defects. In metallic and inorganic polycrystalline materials, defects play an important role in modifying macroscopic properties. To understand the influence of particular defects on the properties of materials, it has proven useful to isolate the defect by creating bicrystals between two-component single crystals. In this way the geometry of a grain boundary defect and its effect on macroscopic properties can be determined unambiguously. In crystalline polymers it would be valuable to establish a similar depth of understanding about the relationship between defect structure and macroscopic properties. Conventionally processed crystalline polymers have small crystallites (10-20 nm), which implies a large defect density in the solid state. Although this means that defects may play an important or even dominant role in crystalline or liquid crystalline polymer systems, it also makes it difficult to isolate the effect of a particular boundary on a macroscopically observed property. However, the development of solid-state and thin-film polymerization mechanisms have facilitated the synthesis of highly organized and ordered polymers. These systems provide a unique opportunity to isolate and investigate in detail the structure of covalently bonded solids near defects and the effect of these defects on the properties of the material. The study of defects in solid polymers has been the subject of a recent review (Martin, 1993).

PREFACE: EUCAS '09: The 9th European Conference on Applied Superconductivity (Dresden, Germany, 13-17 September 2009) EUCAS '09: The 9th European Conference on Applied Superconductivity (Dresden, Germany, 13-17 September 2009)

NASA Astrophysics Data System (ADS)

Holzapfel, Bernhard; Schultz, Ludwig; Schlörb, Heike

2010-03-01

During the 9th European Conference on Applied Superconductivity, 6 plenary, 22 invited, 206 oral and 429 poster contributions were presented on recent developments in the field of applied superconductivity. This issue of Superconductor Science and Technology contains plenary, invited and a selection of contributed oral papers of the four main EUCAS areas: materials, wires and tapes, large scale applications and electronics. The remaining contributed papers that were selected for the conference proceedings will be published in the Journal of Physics: Conference Series. The Dresden EUCAS conference, with 712 participants from 43 countries, continued the tradition of preceding EUCAS conferences of combining basic superconductivity research contributions with the discussion of recent material advances and new developments in large scale and electronic applications. In Dresden, contributions on the recently discovered Fe-based superconductors were presented for the first time during a EUCAS conference and their potential for applications was intensively discussed. Among all the high level papers of this issue we particularly want to highlight the plenary contribution of Praveen Chaudhari on grain boundaries in cuprate superconductors. In his paper Praveen discusses the Jc limitation in HTSC tapes and tunnelling spectroscopy in LSCO thin film bicrystals. Just a few weeks ago we received the sad news that Praveen had passed away on 13 January 2010. Already fighting with his serious illness, Praveen spent all his efforts last fall finishing his plenary talk and paper. This paper will remind us always of his contributions to basic and applied aspects of superconductivity in general and especially his important work on HTSC grain boundaries. Finally we want to acknowledge the help of the International Advisory and National Committees in setting up the scientific program and we would especially like to express our gratitude to all the members of the Local Organization Committee. Their enthusiastic and well organized work made this Dresden EUCAS conference a memorable event for all participants.

Bottom-up multiferroic nanostructures

NASA Astrophysics Data System (ADS)

Ren, Shenqiang

Multiferroic and especially magnetoelectric (ME) nanocomposites have received extensive attention due to their potential applications in spintronics, information storage and logic devices. The extrinsic ME coupling in composites is strain mediated via the interface between the piezoelectric and magnetostrictive components. However, the design and synthesis of controlled nanostructures with engineering enhanced coupling remain a significant challenge. The purpose of this thesis is to create nanostructures with very large interface densities and unique connectivities of the two phases in a controlled manner. Using inorganic solid state phase transformations and organic block copolymer self assembly methodologies, we present novel self assembly "bottom-up" techniques as a general protocol for the nanofabrication of multifunctional devices. First, Lead-Zirconium-Titanate/Nickel-Ferrite (PZT/NFO) vertical multilamellar nanostructures have been produced by crystallizing and decomposing a gel in a magnetic field below the Curie temperature of NFO. The ensuing microstructure is nanoscopically periodic and anisotropic. The wavelength of the PZT/NFO alternation, 25 nm, agrees within a factor of two with the theoretically estimated value. The macroscopic ferromagnetic and magnetoelectric responses correspond qualitatively and semi-quantitatively to the features of the nanostructure. The maximum of the field dependent magnetoelectric susceptibility equals 1.8 V/cm Oe. Second, a magnetoelectric composite with controlled nanostructures is synthesized using co-assembly of two inorganic precursors with a block copolymer. This solution processed material consists of hexagonally arranged ferromagnetic cobalt ferrite (CFO) nano-cylinders within a matrix of ferroelectric Lead-Zirconium-Titanate (PZT). The initial magnetic permeability of the self-assembled CFO/PZT nanocomposite changes by a factor of 5 through the application of 2.5 V. This work may have significant impact on the development of novel memory or logic devices through self assembly techniques. It also demonstrates a universal two-phase hard template application. Last, solid-state self assembly had been used recently to form pseudoperiodic chessboard-like nanoscale morphologies in a series of chemically homogeneous complex oxide systems. We improved on this approach by synthesizing a spontaneously phase separated nanolamellar BaTiO3-CoFe2O4 bi-crystal. The superlattice is magnetoelectric with a frequency dependent coupling. The BaTiO3 component is a ferroelectric relaxor with a Vogel-Fulcher temperature of 311 K. Since the material can be produced by standard ceramic processing methods, the discovery represents great potential for magnetoelectric devices.

Surface polishing of niobium for superconducting radio frequency (SRF) cavity applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhao, Liang

2014-08-01

Niobium cavities are important components in modern particle accelerators based on superconducting radio frequency (SRF) technology. The interior of SRF cavities are cleaned and polished in order to produce high accelerating field and low power dissipation on the cavity wall. Current polishing methods, buffered chemical polishing (BCP) and electro-polishing (EP), have their advantages and limitations. We seek to improve current methods and explore laser polishing (LP) as a greener alternative of chemical methods. The topography and removal rate of BCP at different conditions (duration, temperature, sample orientation, flow rate) was studied with optical microscopy, scanning electron microscopy (SEM), and electronmore » backscatter diffraction (EBSD). Differential etching on different crystal orientations is the main contributor to fine grain niobium BCP topography, with gas evolution playing a secondary role. The surface of single crystal and bi-crystal niobium is smooth even after heavy BCP. The topography of fine grain niobium depends on total removal. The removal rate increases with temperature and surface acid flow rate within the rage of 0~20 °C, with chemical reaction being the possible dominate rate control mechanism. Surface flow helps to regulate temperature and avoid gas accumulation on the surface. The effect of surface flow rate on niobium EP was studied with optical microscopy, atomic force microscopy (AFM), and power spectral density (PSD) analysis. Within the range of 0~3.7 cm/s, no significant difference was found on the removal rate and the macro roughness. Possible improvement on the micro roughness with increased surface flow rate was observed. The effect of fluence and pulse accumulation on niobium topography during LP was studied with optical microscopy, SEM, AFM, and PSD analysis. Polishing on micro scale was achieved within fluence range of 0.57~0.90 J/cm2, with pulse accumulation adjusted accordingly. Larger area treatment was proved possible by overlapping laser tracks at proper ratio. Comparison of topography and PSD indicates that LP smooths the surface in a way similar to EP. The optimized LP parameters were applied to different types of niobium surfaces representing different stages in cavity fabrication. LP reduces the sharpness on rough surfaces effectively, while doing no harm to smooth surfaces. Secondary ion mass spectrometer (SIMS) analysis showed that LP reduces the oxide layer slightly and no contamination occurred from LP. EBSD showed no significant change on crystal structure after LP.« less

Discovering the Role of Grain Boundary Complexions in Materials

DOE Office of Scientific and Technical Information (OSTI.GOV)

Harmer, Martin P.

Grain boundaries are inherently an area of disorder in polycrystalline materials which define the transport and various other material properties. The relationship between the interfacial chemistry, structure and the material properties is not well understood. Among the various taxonomies for grain boundaries, Grain Boundary Complexion is a relatively new conceptual scheme that relates the structure and kinetic properties of grain boundaries. In this classification scheme, grain boundaries are considered to be distinct three dimensional (the thickness being considerably smaller as compared to the other two dimensions but nonetheless discernible) equilibrium thermodynamic phases abutted between two crystalline phases. The stability andmore » structure of these interfacial phases are dictated by various thermodynamic variables such as temperature, stress (pressure), interfacial chemistry (chemical potential) and most importantly by the energies of the adjoining crystal surfaces. These phases are only stable within the constraint of the adjoining grains. Although these interfacial phases are not stable in bulk form, they can transform from one complexion to another as a function of various thermodynamic variables analogous to the behavior of bulk phases. Examples of different complexions have been reported in various publications. However, a systematic investigation exploring the existence of grain boundary complexions in material systems other than alumina remains to be done. Although the role of interfacial chemistry on grain boundary complexions in alumina has been addressed, a clear understanding of the underlying thermodynamics governing complexion formation is lacking. Finally, the effects of grain boundary complexions in bulk material properties are widely unknown. Factors above urge a thorough exploration of grain boundary complexions in a range of different materials systems The purpose of the current program is to verify the existence of grain boundary complexion in a range of materials systems, and to characterize their structures, range of stability and selected physical properties. First, an Au-based bilayer interfacial phase was discovered at a bicrystal boundary in the Si-Au system. This bilayer transitioned abruptly to an intrinsic (“clean”) grain boundary phase, suggesting first-order phase behavior. This study represents the discovery of grain boundary complexions in a completely new system, i.e., a semiconductor-metal system, giving further support to the expectation that grain boundary complexions are a general phenomenon not limited to any particular class of materials. The TiO 2-CuO system exhibited four grain boundary interfacial phases: a monolayer, disordered bilayer, disordered trilayer, and non-wetting nanoscale amorphous drop (which likely resulted from dewetting of a nanoscale IGF). SiO 2 contamination was discovered in the TiO 2-CuO samples, and we hypothesize that this impurity may have caused an “order-disorder” transition to occur. In other words, we expect that pure TiO 2-CuO may have a higher tendency to exhibit ordered bilayer and trilayer complexions, which may also exhibit a well-defined order-disorder transition temperature. In this effort we have also identified unique complexion transitions in yttria and strontium titanate.« less

Effects of Stress Concentrations on the Attenuation by Diffusionally-assisted Grain Boundary Sliding

NASA Astrophysics Data System (ADS)

Lee, L.; Morris, S.; Zohdi, T.

2009-12-01

We report the numerical results from the Raj-Ashby model for diffusionally-assisted grain boundary sliding with finite slope grain interface. The model is a bicrystal consisting of two Hookean elastic layers of finite thickness, separated by a prescribed spatially periodic interface y = f(x). We assume infinitesimal plane deformation. Within the grains, the displacement field u(x,y,t) satisfies the equations of elastostatic equilibrium. At y = f(x), the shear stress σns and normal stress σnn are assumed continuous. Time-derivatives enter the model only through the constitutive equation prescribing the discontinuity in ∂u / ∂t across the grain boundary; the tangential and the normal components of the jump are related to the shear and the normal components of stress respectively by the equations η' [∂us /∂t] = l σns and [∂un /∂t] + (v l D / k T)(∂2σnn / ∂s2) = 0. Here, η', l, v, D, k and T denote respectively the slip (boundary) viscosity, grain boundary thickness, molecular volume, grain boundary diffusivity, Boltzmann constant, and absolute temperature. The equations define two timescales: tv=η' λ / μ l and tD = k T λ3 / v l D μ, where λ and μ are respectively the interface wavelength, and the elastic rigidity of the grains. Consistent with the small-slope (i.e. ɛ = max|df / dx| << 1) analysis by Morris & Jackson (2009), our numerical results of a sawtooth interface show that the mechanical loss L varies as ω-1 at low frequencies (i.e. ω td << 1), whereas at large frequencies (i.e. ω td >> 1), the mechanical loss L decreases slowly with frequency ω. In addition, we also find that the mechanical loss L decreases more rapidly with frequency ω as the interface slope ɛ is increased. For a slope ɛ = 1, which corresponds to a sawtooth sliding plane found in a regular array of hexagonal polycrystals, the mechanical loss spectrum L ˜ ω-1/3, similar to the scaling found experimentally (Jackson et al. 2002), and observed seismically (Shito et al., 2004). We show that this behaviour is an outcome of stress concentrations arising at sharp corners. At low frequencies, the dissipation rate does not depend on frequency ω. Because the time available for dissipation varies inversely with ω, the mechanical loss per cycle L varies as ω-1. At high frequency, the loss decreases more slowly with ω; although the time available for dissipation still varies as ω-1., stress concentrations at triple junction now cause the dissipation-rate to be an increasing function of ω. As a result, the mechanical loss now varies as ω-(2/3)(1 + p). When ɛ = 1, a local analysis by Picu & Gupta (1996) show that p = -0.55 and so, our argument predicts L ˜ ω- 0.3 , close to our numerical results. Thus, the loss spectrum at high frequencies is controlled by the form of stress singularity arising at sharp corners along the grain interface.

Realizing Controllable Quantum States

NASA Astrophysics Data System (ADS)

Takayanagi, Hideaki; Nitta, Junsaku

1. Entanglement in solid states. Orbital entanglement and violation of bell inequalities in mesoscopic conductors / M. Büttiker, P. Samuelsson and E. V. Sukhoruk. Teleportation of electron spins with normal and superconducting dots / O. Sauret, D. Feinberg and T. Martin. Entangled state analysis for one-dimensional quantum spin system: singularity at critical point / A. Kawaguchi and K. Shimizu. Detecting crossed Andreev reflection by cross-current correlations / G. Bignon et al. Current correlations and transmission probabilities for a Y-shaped diffusive conductor / S. K. Yip -- 2. Mesoscopic electronics. Quantum bistability, structural transformation, and spontaneous persistent currents in mesoscopic Aharonov-Bohm loops / I. O. Kulik. Many-body effects on tunneling of electrons in magnetic-field-induced quasi one-dimensional systems in quantum wells / T. Kubo and Y. Tokura. Electron transport in 2DEG narrow channel under gradient magnetic field / M. Hara et al. Transport properties of a quantum wire with a side-coupled quantum dot / M. Yamaguchi et al. Photoconductivity- and magneto-transport studies of single InAs quantum wires / A. Wirthmann et al. Thermoelectric transports in charge-density-wave systems / H. Yoshimoto and S. Kurihara -- 3. Mesoscopic superconductivity. Parity-restricted persistent currents in SNS nanorings / A. D. Zaikin and S. V. Sharov. Large energy dependence of current noise in superconductingh/normal metal junctions / F. Pistolesi and M. Houzet. Generation of photon number states and their superpositions using a superconducting qubit in a microcavity / Yu-Xi Liu, L. F. Wei and F. Nori. Andreev interferometry for pumped currents / F. Taddei, M. Governale and R. Fazio. Suppression of Cooper-pair breaking against high magnetic fields in carbon nanotubes / J. Haruyama et al. Impact of the transport supercurrent on the Josephson effect / S. N. Shevchenko. Josephson current through spin-polarized Luttinger liquid / N. Yokoshi and S. Kurihara -- 4. Mesoscopic superconductivity with unconventional superconductor or ferromagnet. Ultraefficient microrefrigerators realized with ferromagnet-superconductor junctions / F. Giazotto et al. Anomalous charge transport in triplet superconductor junctions by the synergy effect of the proximity effect and the mid gap Andreev resonant states / Y. Tanaka and S. Kashiwaya. Paramagnetic and glass states in superconductive YBa[symbol]Cu[symbol]O[symbol] ceramics of sub-micron scale grains / H. Deguchi et al. Quantum properties of single-domain triplet superconductors / A. M. Gulian and K. S. Wood. A numerical study of Josephson current in p wave superconducting junctions / Y. Asano et al. Tilted bi-crystal sapphire substrates improve properties of grain boundary YBa[symbol]Cu[symbol]O[symbol] junctions and extend their Josephson response to THZ frequencies / E. Stepantsov et al. Circuit theory analysis of AB-plane tunnel junctions of unconventional superconductor Bi[symbol]Sr[symbol]Ca[symbol]Cu[symbol]O[symbol] / I. Shigeta et al. Transport properties of normal metal/anisotropic superconductor junctions in the eutectic system Sr[symbol]RuO[symbol]Ru / M. Kawamura et al. Macroscopic quantum tunneling in d-wave superconductor Josephson / S. Kawabata et al. Quasiparticle states of high-T[symbol] oxides observed by a Zeeman magnetic field response / S. Kashiwaya et al. Experimentally realizable devices for controlling the motion of magnetic flux quanta in anisotropic superconductors: vortex lenses, vortex diodes and vortex pumps / S. Savel'ev and F. Nori. Stability of vortex-antivortex "molecules" in mesoscopic superconducting triangles / V. R. Misko et al. Superconducting network with magnetic decoration - Hofstadter butterfly in spatially modulated magnetic field / Y. Iye et al. Observation of paramagnetic supercurrent in mesoscopic superconducting rings and disks using multiple-small-tunnel-junction method / A. Kanda et al. Guidance of vortices in high-T[stmbol] superconducting thin films with special arrangements of antidots / R. Wöerdenweber, P. Dymashevski and V. R. Misko. Quantum tunneling of relativistic fluxons / K. Konno et al. -- 6. Quantum information processing in solid states. Qubit decoherence by low-frequency noise / K. Rabenstein, V. A. Sverdlov and D. V. Averin. A critique of two-level approximation / K. Savran and T. Hakioǧlu. Josephson arrays as quantum channels / A. Romito, C. Bruder and R. Fazio. Fighting decoherence in a Josephson qubit circuit / E. Collin et al. Fast switching current detection at low critical currents / J. Walter, S. Corlevi and D. Haviland. Asymmetric flux bias for coupled qubits to observe entangled states / Y. Shimazu. Interaction of Josephson qubits with strong QED cavity modes: dynamical entanglement transfer and navigation / G. Falci et al. Controlling decoherence of transported quantum spin information in semiconductor spintronics / B. Nikolic and S. Souma. Decoherence due to telegraph and 1/f noise in Josephson qubits / E. Paladino et al. Detection of entanglement in NMR quantum information processing / R. Rahimi, K. Takeda and M. Kitagawa. Multiphoton absorption and SQUID switching current behaviors in superconducting flux-qubit experiments / H. Takayanagi et al. -- 7. Quantum information theory. Quantum query complexities / K. Iwama. A construction for non-stabilizer Clifford codes / M. Hagiwara and H. Imai. Quantum pushdown automata that can deterministically solve a certain problem / Y. Murakami et al. Trading classical for quantum computation using indirection / R. van Meter. Intractability of the initial arrangement of input data on qubits / Y. Kawano et al. Reversibility of modular squaring / N. Kunihiro, Y. Takahashi and Y. Kawano. Study of proximity effect at D-wave superconductors in quasiclassical methods / Y. Tanuma, Y. Tanaka and S. Kashiwaya -- 8. Spintronics in band electrons. Triplet superconductors: exploitable basis for scalable quantum computing / K. S. Wood et al. Spin excitations in low-dimensional electron gases studied by far-infrared photoconductivity spectroscopy / C.-M. Hu. Control of photogenerated carriers and spins using surface acoustic waves / P. V. Santos, J. A. H. Stotz and R. Hey. PbTe nanostructures for spin filtering and detecting / G. Grabecki. G-factor control in an Ids-inserted InGaAs/InAlAs heterostructure / J. Nitta et al. Spin hall effect in p-type semiconductors / S. Murakami. Spin diffusion in mesoscopic superconducting A1 wires / Y.-S. Shin. H.-J. Lee and H.-W. Lee. Magnetization processes revealed by in-plane DC magnetoresistance measurements on manganite bicrystal thin film devices / R. Gunnarsson. M. Hanson and T. Claeson. Giant magnetoconductance at interface between a two-dimensional hole system and a magnetic semiconductor (Ga, Mn)As / Y. Hashimoto, S. Katsumoto and Y. Iye. Diffusion modes of the transport in diluted magnetic semiconductors / I. Kanazawa. Effect of an invasive voltage probe on the spin polarized current / J. Ohe and T. Ohtsuki -- 9. Spintronics in quantum dots. Tunable exchange interaction and Kondo screening in quantum dot devices / H. Tamura et al. Kondo effect in quantum dots in presence of itinerant-electron magnetism / J. Martinek et al. Optical band edge of II-VI and III-V based diluted magnetic semiconductors / M. Takahashi. Spin-polarized transport properties through double quantum dots / Y. Tanaka and N. Kawakami. RKKY interaction between two quantum dots embedded in an Aharonov-Bohm ring / Y. Utsumi et al. Fabrication and characterization of quantum dot single electron spin resonance devices / T. Kodera et al. Kondo effect in quantum dots with two orbitals and spin 1/2 - crossover from SU (4) to SU (2) symmetry / M. Eto. Detecting spin polarization of electrons in quantum dot edge channels by photoluminescence / S. Nomura. Manipulation of exchange interaction in a double quantum dot / M. Stopa, S. Tarucha and T. Hatano. Electron-density dependence of photoluminescence from Be-[symbol]-doped GaAs quantum wells with a back gate / M. Yamaguchi et al. Direct observation of [symbol]Si nuclear-spin decoherence process / S. Sasaki and S. Watanabe.

PREFACE: Superconductivity in ultrathin films and nanoscale systems Superconductivity in ultrathin films and nanoscale systems

NASA Astrophysics Data System (ADS)

Bianconi, Antonio; Bose, Sangita; Garcia-Garcia, Antonio Miguel

2012-12-01

The recent technological developments in the synthesis and characterization of high-quality nanostructures and developments in the theoretical techniques needed to model these materials, have motivated this focus section of Superconductor Science and Technology. Another motivation is the compelling evidence that all new superconducting materials, such as iron pnictides and chalcogenides, diborides (doped MgB2) and fullerides (alkali-doped C60 compounds), are heterostrucures at the atomic limit, such as the cuprates made of stacks of nanoscale superconducting layers intercalated by different atomic layers with nanoscale periodicity. Recently a great amount of interest has been shown in the role of lattice nano-architecture in controlling the fine details of Fermi surface topology. The experimental and theoretical study of superconductivity in the nanoscale started in the early 1960s, shortly after the discovery of the BCS theory. Thereafter there has been rapid progress both in experiments and the theoretical understanding of nanoscale superconductors. Experimentally, thin films, granular films, nanowires, nanotubes and single nanoparticles have all been explored. New quantum effects appear in the nanoscale related to multi-component condensates. Advances in the understanding of shape resonances or Fano resonances close to 2.5 Lifshitz transitions near a band edge in nanowires, 2D films and superlattices [1, 2] of these nanosized modules, provide the possibility of manipulating new quantum electronic states. Parity effects and shell effects in single, isolated nanoparticles have been reported by several groups. Theoretically, newer techniques based on solving Richardson's equation (an exact theory incorporating finite size effects to the BCS theory) numerically by path integral methods or solving the entire Bogoliubov-de Gennes equation in these limits have been attempted, which has improved our understanding of the mechanism of superconductivity in these confined systems. In addition, the role of thermodynamic fluctuations on superconducting properties has been extensively studied in the context of nanoparticles and nanowires both experimentally and theoretically. In the past decade, a lot of work has been initiated in the area of interface superconductivity where different techniques have been demonstrated to tune Tc. Although the progress in this field has deepened our understanding of nanoscale superconductors, there are several open and key questions which need to be addressed. Some of these are: (1) can superconductivity be enhanced and Tc increased in nanostructures with respect to the bulk limit and if so, how can it be controlled? (2) What are the theoretical and experimental limits for the enhancement and control of superconductivity? (3) Can the phenomena identified in conventional nanostructures shed light on phenomena in high Tc superconductors and vice versa? (4) How will the new fundamental physics of superconductivity at the nanoscale promote advances in nanotechnology applications and vice versa? The papers in this focus section reflect the advances made in this field, in particular in nanowires and nanofilms, but also attempt to answer some of the key open questions outlined above. The theoretical papers explore unconventional quantum phenomena such as the role of confinement in the dynamics of single Cooper pairs in isolated grains [1] and Fano resonances in superconducting gaps in multi-condensate superconductors near a 2.5 Lifshitz transition [2]. Here a new emerging class of quantum phenomena of fundamental physics appear at the Bose-BCS crossover in multi-condensate superconductors [2]. Nanosize effects can now be manipulated by controlling defects in layered oxides [3]. A new approach is provided by controlling the self-organization of oxygen interstitials in layered copper oxides that show an intrinsic nanoscale phase separation [4]. In this case a non-trivial distribution of superconducting nanograins appears to enhance the critical temperature [4]. This is a hot topic as in the past year many works have clarified the nanoscale phase separation in electron-doped chalcogenides, showing the key role of a complex texture of nanograins and opening new avenues for the fundamental understanding of quantum phenomena in networks of superconducting nanograins. The advances in nanotechnology allow the exploration of the possible existence of superconductivity in single carbon nanotubes [5]. The technological applications presented by Gomez [6] and Lehtinen [7] show the fundamental physics of superconductivity at the nanoscale to promote new advances in quantum devices. We hope that this combination will make these focus papers in Superconductor Science and Technology interesting and promote cross-fertilization among the different sub-branches of the field which all share the same goal of addressing the key questions on nanoscale superconductors. References [1]Croitoru M D, Vagov A, Shanenko A A and Axt V M 2012 The Cooper problem in nanoscale: enhancement of the coupling due to confinement Supercond. Sci. Technol. 25 124001 [2]Perali A, Innocenti A, Valletta A and Bianconi A 2012 Anomalous isotope effect near a 2.5 Lifshitz transition in a multi-band multi-condensate superconductor made of a superlattice of stripes Supercond. Sci. Technol. 25 124002 [3]Zeng S W, Huang Z, Wang X, Lü W M, Liu Z Q, Zhang B M, Dhar S, Venkatesan T and Ariando 2012 The influence of La substitution and oxygen reduction in ambipolar La-doped YBa2Cu3Oy thin films Supercond. Sci. Technol. 25 124003 [4]Poccia N, Bianconi A, Campi G, Fratini M and Ricci A 2012 Size evolution of the oxygen interstitial nanowires in La2CuO4+y by thermal treatments and x-ray continuous illumination Supercond. Sci. Technol. 25 124004 [5]Yang Y, Fedorov G, Zhang J, Tselev A, Shafranjuk S and Barbara P 2012 The search for superconductivity at van Hove singularities in carbon nanotubes Supercond. Sci. Technol. 25 124005 [6]Gomez A, Gonzalez E M and Vicent J L 2012 Superconducting vortex dynamics on arrays with bicrystal-like structures: matching and rectifier effects Supercond. Sci. Technol. 25 124006 [7]Lehtinen J S and Arutyunov K Yu 2012 The quantum phase slip phenomenon in superconducting nanowires with a low-Ohmic environment Supercond. Sci. Technol. 25 124007

Preface

NASA Astrophysics Data System (ADS)

Gorse, D.; Boutard, J.-L.

2002-09-01

The Symposium on “Structural materials for Hybrid systems: A challenge in metallurgy" was held during the “Journées d'Automne 2001" of the “Société Française de Métallurgie et de Matériaux", Paris from October 29 through 31, 2001. The editors of this volume, D. Gorse and J.-L. Boutard, would like to acknowledge GDR GEDEON, CEA - Direction de l'énergie Nucléaire, CNRS - Département des Sciences Chimiques, et Centre d'études de Chimie Métallurgique for sponsoring this symposium. This symposium was divided into three sessions dealing with i) thermodynamics, intergranular penetration and liquid metal embrittlement, ii) irradiation effects in structural materials and iii) compatibility of structural materials with lead alloys in relation with R& D studies for MEGAPIE. The intent of this symposium was to provide a forum for discussing the most recent results obtained in the frame of the materials research program of the “Groupement De Recherche (GDR) GEDEON". Special emphasis was given to all factors susceptible to affect the durability of structural materials for spallation targets, like irradiation effects under proton and neutron mixed spectrum, Liquid Metal Corrosion (LMC) and Embrittlement (LME). The material research program of GEDEON is a joint CEA-CNRS venture. In 1997, the GDR GEDEON gave opportunity to metallurgists and nuclear physicists of both organizations to collaborate for validating the concept of Pb-Bi spallation targets as a key component for Accelerator-Driven Systems (ADS). Historically, since 1995, GDR GEDEON has promoted ADS, also called Hybrid System, as an option for waste management. The starting point of the material program was the 1st GEDEON Workshop on “Materials For Hybrid Systems" held in Paris in 1997, where reference materials of the 9-12 Cr martensitic steels series were selected: EM10 (9Cr-1Mo) and the modified 9Cr-1Mo, T91 (9Cr-1Mo-V-Nb). However, besides their specific concern for ADS, our studies are also of interest for the next generation of LM spallation targets in EU, U.S.A. and Japan. These proceedings contain manuscripts from 90% of the presented papers. The organizers would like to thank all their Colleagues who presented papers, contributed with manuscripts and attended the sessions at the symposium. For sake of clarity, this volume is divided into five sections: 1) general R& D for spallation targets, 2) irradiation effects in liquid metal spallation targets, 3) oxygen control: thermodynamics and monitoring, 4) resistance to liquid metal corrosion and embrittlement of structural materials for spallation targets and 5) basic studies of intergranular penetration and liquid metal embrittlement. Section 1 begins with a description of the spallation neutron source facility SINQ and of ongoing R& D programs at PSI (Switzerland), including MEGAPIE, the joint initiative by six European research institutions and JAERI (Japan), DOE (USA) and KAERI (Korea) to design, build, operate and assess the performance of a liquid lead-bismuth spallation target for 1MW of beam power (G. Bauer et al.). The materials aspects related to the MEGAPIE target and to the LiSoR (Liquid Solid Reactions under irradiation) experiment are reviewed by T. Auger et al. The advantages and drawbacks of solid tungsten spallation targets, compared to liquid Pb-Bi eutectic spallation targets are examined by R. Enderlé et al., presenting the CEA point of view. Section 2 is dedicated to irradiation effects in Liquid Metal (LM) spallation targets structure, a crucial problem for the feasibility of ADS. P. Jung is pointing out the specificity of the irradiation conditions in LM targets by comparison with fast neutron fission and fusion reactors, and the metallurgical consequences like irradiation and helium-induced embrittlement. The author emphasizes the importance of spallation residues whose deleterious effects on in-service properties of target container and window are largely unknown. Until recently, say 1997, only predictions of spallation residues production were available. This motivated the GEDEON workshop on “Nuclear Data for materials studies in the frame of hybrid systems" held in 1999 in Vichy (France). The paper presented by C. Villagrasa et al. highlights the progress achieved during the past five years, promoted by GDR GEDEON. The reverse kinematics experiments performed during that period allowed to obtaining reliable values for production cross sections of residual nuclei produced by spallation reactions. The authors also mention improvements on the computation codes. The case of the target window, thin target simply made of iron from the nuclear physics point of view, is thoroughly investigated. The authors also treat the production of residues in heavy metals, like lead. The experimental data reported below results from the cooperation of CEA, CNRS and Forschungszentrum Jülich within the program SPIRE of the 5th European Framework Program. From the metallurgists point of view, O. Danylova et al. reported an interesting attempt to simulate by doping production of three spallation residues, namely phosphorus, sulfur and titanium, certainly detrimental regarding the mechanical properties (fracture toughness...) of the 9% Cr martensitic steels pre-selected for the target window and container. The authors describe the inherent difficulties encountered for obtaining the microstructure and modified steel composition expected under irradiation. In all cases, production of hydrogen and helium is expected very high, ~90 000 appm/year for hydrogen and ~5000 appm/year for helium, corresponding to a damage level of ~100 dpa/year in the target window. These estimated values are just mentioned to show the importance of the metallurgical problem to be faced. These data motivated studies of helium implantation effects by J. Henry et al. in two 9Cr-1Mo (EM10) and modified 9Cr-1Mo-V-Nb (T91) pre-selected martensitic steels. Homogeneous implantation of 5000 appm He in T91 and EM10 thin foils followed by TEM examination and tensile testing revealed an important hardening and embrittlement at 250 °C. At 500 °C both materials exhibit far less hardening and retain significant ductility. In the latter case, those findings were correlated with the appearance of helium bubbles detected in Transmission Electron Microscopy (TEM) examination. At 250 °C, no He bubble is detected by TEM. Conversely, Small Angle Neutron Scattering (SANS) allows to identify a high density of objects ~1-2 nm, most probably tiny He bubbles. The low temperature He embrittlement is most probably due to the conjunction of grain hardening and decrease of the cohesive energy of prior austenitic grain boundaries due to He segregation. Besides hydrogen and helium, significant quantities of other spallation residues will be also accumulated in the target window during one year of operation. About 1000 appm of calcium form after one year of irradiation with 1 GeV protons. This exemplary insoluble spallation residue could also contribute to embrittle the window. G. Amiri et al. studied the implantation of both calcium and sulfur (up to 1-2 at% corresponding to a 20 dpa damage level) at 500 °C, assumed to be the highest temperature of the target window in service conditions. P. Pareige et al. detected the formation of Ca nanoclusters using the 3D atomic probe. Neither calcium sulfides nor carbides were detectable whatever the temperature (300 °C or 500 °C) and damage levels. E. Cadel, P. Pareige and M.O. Ruault showed how powerful is the 3D atom probe to characterize both chemical and structural evolution of irradiated steel specimens, at a nanometric scale allowing for interpretation of radiation damages “from first principles". Section 3 is dedicated to oxygen control, including thermodynamic aspects and monitoring. The GDR GEDEON material program promoted the development of oxygen sensors in liquid metals. V. Ghetta et al. studied carefully the possibilities, limitations of existing sensors and proposed new developments allowing to interpret e.m.f measurements at temperatures well below 450 °C. Intercomparisons between oxygen sensors, using various static facilities (BIP, JACOMEX and COLIMESTA) were carried out by J.-L. Courouau et al. This study is now going on including our EU partners in the closely related TECLA program granted by the 5th framework program. C. Lesueur et al. developed original methods for measuring wettability, permitting to determine the stability of native oxides (on Al, Fe, Ni and also T91 steel) in contact with molten lead. A. Maitre et al. presented a preliminary thermodynamic study of the quinary Bi-Fe-Hg-O-Pb system, beginning with the Bi-Hg-Pb system. No solid ternary phase was found in Pb-Bi eutectic in the temperature range expected for the spallation target. Then the authors focused on the possible formation of oxygenated compounds of low melting point either at the T91 steel/Pb or at the T91 steel/Pb-Bi eutectic interface. Section 4 concerns the resistance to LMC and LME of structural materials pre-selected for the spallation target of ADS, with special emphasis on the liquid Pb-Bi eutectic target concept. The compatibility of 9% Cr martensitic steels (like EM10 or T91...) with liquid Pb and Pb-Bi eutectic was examined. Qualification of the T91 steel/LBE system is required to build the liquid Pb-Bi target in PSI in 2005 and for further applications. A comparative study of the long-term corrosion behaviour of various martensitic and austenitic steels in forced circulation loop was carried out by F. Balbaud-Celerier et al. allowing to vary the temperature and oxygen content in LBE covering the range 10-8wt% -10-6wt.% . This work results from a fruitful collaboration with IPPE (Obninsk, Russia). The two following papers of Section 4 deal with the tensile behaviour of T91 steel in contact with lead and its alloys. The most severe metallurgical (J.-B. Vogt et al.) and environmental (J.-L. Pastol et al.) conditions are considered in order to estimate the risk of LME for the target window in service. J.-B. Vogt et al. observed a transgranular (TG) brittle fracture after hardening heat treatment of T91 steel after tensile testing of notched specimens at 350 °C in oxygen-saturated lead. Note that cases of TG-LME are rather scarcely observed. On the other hand, J.-L. Pastol et al. obtained an embrittling effect on notched specimens by optimizing the environmental parameters (in LBE at 350 °C under He-4% H2 cover gas...) and tensile testing conditions. F. Gamaoun et al. showed that a few days exposure of T91 steel in lead under either reducing or oxidizing conditions gives rise to a significant porosity in the steel. This could justify the increased stress relaxation kinetics of specimens submitted to 4-point bending tests under the same conditions. Besides the R& D research related to the spallation target for ADS, a non-negligible part of the GEDEON material research program was dedicated to intergranular penetration and LME. Some exemplary LME studies are reported in Section 5 of this volume, illustrating various aspects of this very old, tricky and exotic problem in metallurgy. One can find in this volume studies involving various Solid Metal/Liquid Metal (SM/LM) couples, going from high purity metal couples (Ni/Pb, Ni/Bi...) to industrial metallic alloys put in contact with liquid metals or alloys of varying purity. LME is a multi scale phenomenon that cannot be explained on the sole basis of either thermodynamics, metallurgical or kinetics criteria. In this section, the role of the stress-strain state is emphasized. The importance of the microstructure of the grains boundaries (facetting...) on LM penetration is also pointed out. This aspect of the problem can now be dealt with thanks to Atomic Force Microscopy (AFM), High Resolution Transmission Electron Microscopy (HRTEM), Electron Energy Loss Spectroscopy (EELS) and Auger Electron Spectroscopy (AES) techniques. Crack propagation kinetics can now be followed at ESRF (Grenoble) using synchrotron radiation imaging techniques. It is now possible to follow the propagation, structure and chemistry of the embrittling phase in the crack, at microscopic and at nanometric scale. It is also possible, in principle, to take into account the role of defects in grain-boundaries (GB) on the penetration of the embrittling species and conversely to investigate the role of the defects produced by wetting on the GB microstructure. We do hope that these techniques open a new and attractive field of research to improve the understanding of LME. The HRTEM study carried out by A. Charai et al. enlightens the importance of crystallography on wetting. Two exemplary couples are thoroughly investigated: the Mo/Ni couple giving rise to an interfacial nanometer thick interface for one type of Mo bicrystal wetted by nickel and the Ni/Pb couple pointing out the role of the GB plane on wetting. Y. Brechet et al. investigated not only the microstructure effects on “LM" penetration into cracks (cracks kinetics and morphologies), but also the plasticity effects ahead of the crack tip, studying a variant of the mythic Al/Ga couple, say the 7010 Aluminum alloy in contact with Gallium, allowing for modifications of the precipitation state at the GBs by applying various heat treatments. Y. Brechet et al. conclude in favour of a step by step penetration process, quasi at atomic scale and give an estimate of crack propagation velocity, of the order of a few micrometers per second, in good agreement with experimental observations. The author stresses the importance of defects in the GBs (precipitates...) at different scales which can explain discrepancies between the experimental crack velocity and the one calculated using a continuum elastic model. The paper presented by W. Ludwig et al. concentrates on two synchrotron radiation imaging techniques (X-ray micro-radiography and micro-fluorescence) available at ESRF (Grenoble) in order to characterize the penetration kinetics of embrittling species in the crack. Beside the Al/Ga couple, it is shown that those techniques are suitable to follow intergranular propagation of cracks in the Ni/Bi system, even when the embrittling layer becomes nanometric. Structuration of liquid Al in contact with Cu(100) and Cu(111) surfaces of a bulk Cu crystal was studied by P. Geysermans et al. using Molecular Dynamics simulations. The authors showed an epitaxial relationship, whatever the density of the solid and contacting liquid phases. This feature is of importance to understand the structure of the wetting layers in GBs. J. Bernardini et al. emphasize the role of macroscopic defects like facets in GBs on “LM" penetration and propose a model allowing to describe the real shape of the cracks they observed with Ni annealed in contact with pure lead, inconsistent with Mullins grooving theory. Cu/Bi, Cu/LBE (Lead-Bismuth Eutectic) and Ni/LBE systems were studied by K. Wolski et al. using AES semi-quantitative analysis of fractured specimens under vacuum within an Auger Electron spectrometer, enlightening the embrittling role of the nanometer-thick wetting layer in the crack tip area. In summary, during the past five years close cooperation between researchers within the material research program of GEDEON co-sponsored by the 5th EU Framework program allowed to make significant progress. Research dedicated to radiation damage in structural materials for ADS and spallation targets was very active and a number of impressive results were obtained. The low temperature He embrittlement is certainly a matter of concern. The controlling mechanisms and their dependence with temperature, He and dpa production rate has to be clarified. Likewise, compatibility studies of structural materials with lead and lead alloys, particularly LBE, gave rise to a number of remarkable results. One can mention here specifically the progress made with oxygen sensors. Significant is also the renewal of interest for LME during the past five years. Promising results on LME and intergranular penetration are already obtained and should be obtained in this attractive field of research. Of course, a great deal of work remains to be done in order to validate the concept of Pb-Bi spallation target for ADS. Especially, the effect of spallation elements production in structural materials and in LBE has to be assessed as well as LMC and LME under irradiation.