Analysis of crystallographic slip and grain boundary sliding in a Ti-45Al-2Nb-2Mn (at%)-0.8 vol%TiB2 alloy by high temperature in situ mechanical testing

This work aims to contribute to a further understanding of the fundamentals of crystallographic slip and grain boundary sliding in the γ-TiAl Ti–45Al–2Nb–2Mn (at%)–0.8 vol%TiB2 intermetallic alloy, by means of in situ high-temperature tensile testing combined with electron backscatter diffraction (EBSD). Several microstructures, containing different fractions and sizes of lamellar colonies and equiaxed γ-grains, were fabricated by either centrifugal casting or powder metallurgy, followed by heat treatment at 1300 °C and furnace cooling. in situ tensile and tensile-creep experiments were performed in a scanning electron microscope (SEM) at temperatures ranging from 580 °C to 700 °C. EBSD was carried out in selected regions before and after straining. Our results suggest that, during constant strain rate tests, true twin γ/γ interfaces are the weakest barriers to dislocations and, thus, that the relevant length scale might be influenced by the distance between non-true twin boundaries. Under creep conditions both grain/colony boundary sliding (G/CBS) and crystallographic slip are observed to contribute to deformation. The incidence of boundary sliding is particularly high in γ grains of duplex microstructures. The slip activity during creep deformation in different microstructures was evaluated by trace analysis. Special emphasis was placed in distinguishing the compliance of different slip events with the Schmid law with respect to the applied stress.

Void formation and grain boundary sliding in aluminum-magnesium solid solution alloys

"Materials Central, Contract no. AF 33(616)-5926. Project no. 7351."

Microstructure and grain boundary microanalysis of X70 pipeline steel

Grain boundaries (GBs), particularly ferrite: ferrite GBs, of X70 pipeline steel were characterized using analytical electron microscopy (AEM) in order to understand its intergranular stress corrosion cracking (IGSCC) mechanism(s). The microstructure consisted of ferrite (alpha), carbides at ferrite GBs, some pearlite and some small precipitates inside the ferrite grains. The precipitates containing Ti, Nb, V and N were identified as complex carbo-nitrides and designated as (Ti, Nb, WC, N). The GB carbides occurred (1) as carbides along ferrite GBs, (2) at triple points, and (3) at triple points and extending along the three ferrite GBs. The GB carbides were Mn rich, were sometimes also Si rich, contained no micro-alloying elements (Ti, Nb, V) and also contained no N. It was not possible to measure the GB carbon concentration due to surface hydrocarbon contamination despite plasma cleaning and glove bag transfer from the plasma cleaner to the electron microscope. Furthermore, there may not be enough X-ray signal from the small amount of carbon at the GBs to enable measurement using AEM. However, the microstructure does indicate that carbon does segregate to alpha : alpha GBs during microstructure development. This is particularly significant in relation to the strong evidence in the literature linking the segregation of carbon at GBs to IGSCC. It was possible to measure all other elements of interest. There was no segregation at alpha : alpha GBs, in particular no S, P and N, and also no segregation of the micro-alloying elements, Ti, Nb and V. (C) 2003 Kluwer Academic Publishers.

Atom probe field ion microscope measurements of carbon segregation at an a:a grain boundary and service failures by intergranular stress corrosion cracking

This work reports on a critical measurement to understand the intergranular stress corrosion cracking (IGSCC) of pipeline steels: the atom probe field ion microscope (APFIM) measurement of the carbon concentration at a grain boundary (GB). The APFIM measurement was related to the microstructure and to IGSCC observations. The APFIM indicated that the GB carbon concentration of X70 was similar to 10 at% or less, which correlated with a high resistance to IGSCC for X70. (C) 2005 Elsevier Ltd. All rights reserved.

Dynamic recrystallization induced by plastic deformation at high strain rate in a Monel alloy

An investigation has been made into the plastic deformation behavior of a Monel alloy deformed at high strain rate of 10(5) s(-1) by split Hopkinson bar. The results reveal that there are some equiaxed grains with an average size of 150 nm in diameter in the center of the shear bands, suggesting that this microstructure characteristics be developed by dynamic recrystallization, arising from the deformation and the rapid temperature rise in the band. Analysis shows that the plastic strain rate and the mobile dislocation density play a key role in the new crystallized grain formation and growth. Based on grain boundary energy change and diffusion mechanism, the grain growth kinetics is developed for plastic deformation at a high strain rate.

A model for energy and morphology of crystalline grain boundaries with arbitrary geometric character

It has been well-established that interfaces in crystalline materials are key players in the mechanics of a variety of mesoscopic processes such as solidification, recrystallization, grain boundary migration, and severe plastic deformation. In particular, interfaces with complex morphologies have been observed to play a crucial role in many micromechanical phenomena such as grain boundary migration, stability, and twinning. Interfaces are a unique type of material defect in that they demonstrate a breadth of behavior and characteristics eluding simplified descriptions. Indeed, modeling the complex and diverse behavior of interfaces is still an active area of research, and to the author's knowledge there are as yet no predictive models for the energy and morphology of interfaces with arbitrary character. The aim of this thesis is to develop a novel model for interface energy and morphology that i) provides accurate results (especially regarding "energy cusp" locations) for interfaces with arbitrary character, ii) depends on a small set of material parameters, and iii) is fast enough to incorporate into large scale simulations.

In the first half of the work, a model for planar, immiscible grain boundary is formulated. By building on the assumption that anisotropic grain boundary energetics are dominated by geometry and crystallography, a construction on lattice density functions (referred to as "covariance") is introduced that provides a geometric measure of the order of an interface. Covariance forms the basis for a fully general model of the energy of a planar interface, and it is demonstrated by comparison with a wide selection of molecular dynamics energy data for FCC and BCC tilt and twist boundaries that the model accurately reproduces the energy landscape using only three material parameters. It is observed that the planar constraint on the model is, in some cases, over-restrictive; this motivates an extension of the model.

In the second half of the work, the theory of faceting in interfaces is developed and applied to the planar interface model for grain boundaries. Building on previous work in mathematics and materials science, an algorithm is formulated that returns the minimal possible energy attainable by relaxation and the corresponding relaxed morphology for a given planar energy model. It is shown that the relaxation significantly improves the energy results of the planar covariance model for FCC and BCC tilt and twist boundaries. The ability of the model to accurately predict faceting patterns is demonstrated by comparison to molecular dynamics energy data and experimental morphological observation for asymmetric tilt grain boundaries. It is also demonstrated that by varying the temperature in the planar covariance model, it is possible to reproduce a priori the experimentally observed effects of temperature on facet formation.

Finally, the range and scope of the covariance and relaxation models, having been demonstrated by means of extensive MD and experimental comparison, future applications and implementations of the model are explored.

Influence of grain boundaries on the vibrational properties of silver nanowires

Metal and semiconductor nanowires (NWs) have been widely employed as the building blocks of the nanoelectromechanical systems, which usually acted a resonant beam. Recent researches reported that nanowires are often polycrystalline, which contains grain boundaries (GBs) that transect the whole nanowire into a bamboo like structure. Based on the larger-scale molecular dynamics (MD) simulations, a comprehensive investigation of the influence from grain boundaries on the vibrational properties of doubly clamped Ag NWs is conducted. It is found that, the presence of grain boundary will result in significant energy dissipation during the resonance of polycrystalline NWs, which leads a great deterioration to the quality factor. Further investigation reveals that the energy dissipation is originated from the plastic deformation of polycrystalline NWs in the form of the nucleation of partial dislocations or the generation of micro stacking faults around the GBs and the micro stacking faults is found to keep almost intact during the whole vibration process. Moreover, it is observed that the closer of the grain boundary getting to the regions with the highest strain state, the more energy dissipation will be resulted from the plastic deformation. In addition, either the increase of the number of grain boundaries or the decrease of the distance between the grain boundary and the highest strain state region is observed to induce a lower first resonance frequency. This work sheds lights on the better understanding of the mechanical properties of polycrystalline NWs, which benefits the increasing utilities of NWs in diverse nano-electronic devices.

Analysis and prediction of the critical current density across [001]-tilt YBa2Cu3O7- grain boundaries of arbitrary misorientation angles

A qualitative analysis of the expected dilatation strain field in the vicinity of an array of grain-boundary (GB) dislocations is presented. The analysis provides a basis for the prediction of the critical current densities (jc) across low-angle YBa2Cu3O7- (YBCO) GBs as a function of their energy. The introduction of the GB energy allows the extension of the analysis to high-angle GBs using established models which predict the GB energy as a function of misorientation angle. The results are compared to published data for jc across [001]-tilt YBCO GBs for the full range of misorientations, showing a good fit. Since the GB energy is directly related to the GB structure, the analysis may allow a generalization of the scaling behavior of jc with the GB energy. © 1995 The American Physical Society.

Energetic and thermal properties of tilt grain boundaries in graphene/hexagonal boron nitride heterostructures

Graphene/hexagonal boron nitride (G/h-BN) heterostructure has attracted tremendous research efforts owing to its great potential for applications in nano-scale electronic devices. In such hybrid materials, tilt grain boundaries (GBs) between graphene and h-BN grains may have unique physical properties, which have not been well understood. Here we have conducted non-equilibrium molecular dynamics simulations to study the energetic and thermal properties of tilt GBs in G/h-BN heterostructures. The effect of misorientation angles of tilt GBs on both GB energy and interfacial thermal conductance are investigated.

Surface modifications in single crystal surfaces of YBa2Cu3O7-delta upon high energy ion irradiation

Atomic force microscopy investigations on swift heavy ion (200 MeV An) irradiated surfaces of a high T-c single crystal YBa2Cu3O7-delta are presented. Results obtained revealed an ion-induced erosion/sputtering clearly confirming our earlier observation on grain boundary dominated thin films. Apart from sputtering, notable effects were seen with many defect structures like dikes/hillocks surrounded by craters, dikes, holes, pearl like structures and ripple formation of sub-micron undulations, all in one crystal. Results are discussed in the light of co-operative phenomena of material re-distribution mechanism related to mass transfer and crater formations.

Grain Growth in ECAE Processed Pure Magnesium

Grain growth kinetics was studied for commercially pure magnesium subjected to equal channel angular extrusion (ECAE). The specimens were ECAE processed upto 4 passes at 523 K following all the three important routes, namely A, 13, and C. Texture and microstructures of the samples were studied using Electron Back Scattered Diffraction (EBSD) technique in a Field Emission Gun Scanning Electron Microscope (FEG-SEM). It was observed that the grain size significantly reduces after ECAE. ECAE process produces a slightly rotated B and C-2 fiber. Static annealing leads to normal grain growth with unimodal distribution of grains through out the temperature range. Average activation energy for grain growth in the temperature range studied is found to be less than the activation energy for lattice diffusion and grain boundary diffusion of magnesium. No significant change in texture during isochronal annealing for 1 hour i.e., the predominant deformation texture remains same.

Decay of photo-induced conductivity in Sb-doped SnO2 thin films, using monochromatic light of about bandgap energy

Doping tin dioxide (SnO2) with pentavalent Sb5+ ions leads to an enhancement in the electrical conductivity of this material, because Sb5+ substitutes Sn4+ in the matrix, promoting an electronic density increase in the conduction band, due to the donor-like nature of the doping atom. Results of computational simulation, based on the Density Functional Theory (DFT), of SnO2:4%Sb and SnO2:8%Sb show that the bandgap magnitude is strongly affected by the doping concentration, because the energy value found for 4 at%Sb and 8 at%Sb was 3.27 eV and 3.13 eV, respectively, whereas the well known value for undoped SnO2 is about 3.6 eV. Sb-doped SnO2 thin films were obtained by the sol-gel-dip-coating technique. The samples were submitted to excitation with below theoretical bandgap light (450 nm), as well as above bandgap light (266 nm) at low temperature, and a temperature-dependent increase in the conductivity is observed. Besides, an unusual temperature and time dependent decay when the illumination is removed is also observed, where the decay time is slower for higher temperatures. This decay is modeled by considering thermally activated cross section of trapping centers, and the hypothesis of grain boundary scattering as the dominant mechanism for electronic mobility. © 2012 Elsevier B.V. All rights reserved.

The grain-scale distribution and behaviour of melt and fluid in crystalline analogue systems

The production, segregation and migration of melt and aqueous fluids (henceforth called liquid) plays an important role for the transport of mass and energy within the mantle and the crust of the Earth. Many properties of large-scale liquid migration processes such as the permeability of a rock matrix or the initial segregation of newly formed liquid from the host-rock depends on the grain-scale distribution and behaviour of liquid. Although the general mechanisms of liquid distribution at the grain-scale are well understood, the influence of possibly important modifying processes such as static recrystallization, deformation, and chemical disequilibrium on the liquid distribution is not well constrained. For this thesis analogue experiments were used that allowed to investigate the interplay of these different mechanisms in-situ. In high-temperature environments where melts are produced, the grain-scale distribution in “equilibrium” is fully determined by the liquid fraction and the ratio between the solid-solid and the solid-liquid surface energy. The latter is commonly expressed as the dihedral or wetting angle between two grains and the liquid phase (Chapter 2). The interplay of this “equilibrium” liquid distribution with ongoing surface energy driven recrystallization is investigated in Chapter 4 and 5 with experiments using norcamphor plus ethanol liquid. Ethanol in contact with norcamphor forms a wetting angle of about 25°, which is similar to reported angles of rock-forming minerals in contact with silicate melt. The experiments in Chapter 4 show that previously reported disequilibrium features such as trapped liquid lenses, fully-wetted grain boundaries, and large liquid pockets can be explained by the interplay of the liquid with ongoing recrystallization. Closer inspection of dihedral angles in Chapter 5 reveals that the wetting angles are themselves modified by grain coarsening. Ongoing recrystallization constantly moves liquid-filled triple junctions, thereby altering the wetting angles dynamically as a function of the triple junction velocity. A polycrystalline aggregate will therefore always display a range of equilibrium and dynamic wetting angles at raised temperature, rather than a single wetting angle as previously thought. For the deformation experiments partially molten KNO3–LiNO3 experiments were used in addition to norcamphor–ethanol experiments (Chapter 6). Three deformation regimes were observed. At a high bulk liquid fraction >10 vol.% the aggregate deformed by compaction and granular flow. At a “moderate” liquid fraction, the aggregate deformed mainly by grain boundary sliding (GBS) that was localized into conjugate shear zones. At a low liquid fraction, the grains of the aggregate formed a supporting framework that deformed internally by crystal plastic deformation or diffusion creep. Liquid segregation was most efficient during framework deformation, while GBS lead to slow liquid segregation or even liquid dispersion in the deforming areas.

A New Technique for Firn Grain-Size Measurement Using SEM Image Analysis

Firn microstructure is accurately characterized using images obtained from scanning electron microscopy (SEM). Visibly etched grain boundaries within images are used to create a skeleton outline of the microstructure. A pixel-counting utility is applied to the outline to determine grain area. Firn grain sizes calculated using the technique described here are compared to those calculated using the techniques of Cow (1969) and Gay and Weiss (1999) on samples of the same material, and are found to be substantially smaller. The differences in grain size between the techniques are attributed to sampling deficiencies (e.g. the inclusion of pore filler in the grain area) in earlier methods. The new technique offers the advantages of greater accuracy and the ability to determine individual components of the microstructure (grain and pore), which have important applications in ice-core analyses. The new method is validated by calculating activation energies of grain boundary diffusion using predicted values based on the ratio of grain-size measurements between the new and existing techniques. The resulting activation energy falls within the range of values previously reported for firn/ice.