First observation of a wetting phase transition in low-angle grain boundaries

The wetting phase transition at low-angle intercrystallite grain boundaries has been experimentally observed. In contrast to the high-angle grain boundaries with the misorientation angels θ > 15°, the low-angle grain boundaries (θ < 15°) are not continuous two-dimensional defects, but constitute a discrete wall (network) of lattice dislocations (edge and/or helical). The theory predicts that, depending on θ, either a continuous layer of the liquid phase or a wall (network) of microscopic liquid tubes on wetted dislocation nuclei is formed at completely wetted low-angle grain boundaries. It has been shown that the continuous liquid layers at low-angle grain boundaries in the Cu-Ag alloys appear at the temperature T _wminL = 970°C, which is 180°C higher than the onset temperature T _wmin = 790°C and 50°C lower than the finish temperature of the wetting phase transition at high-angle grain boundaries, T _wmax = 1020°C.     

Coupled motion of [10−10] tilt boundaries in magnesium bicrystals

Magnesium bicrystals were grown with symmetric and asymmetric tilt boundaries about the [10–10] axis using the vertical Bridgman technique. Isothermal constant load tensile tests were conducted on these bicrystals in the temperature range 300–500°C and relative displacements of the two grains were measured to obtain an appreciation for grain boundary motion characteristics. Coupled grain boundary motion was noted in almost all cases with the degree of tangential motion versus migration changing with tilt misorientation, temperature and applied stress. Specifically, within the family of symmetric bicrystals evaluated, a minimum in grain boundary displacement in the specimen plane was observed at a tilt misorientation of 20°. In specific stress/temperature regimes, rigid body sliding was observed for the particular case of a 35° asymmetric tilt misorientation. The ease of basal and prism slip in magnesium at the temperatures considered and the consequential impingement of intragranular dislocations on the bicrystal boundary and their decomposition and motion along the boundary are thought to play an important role in the observed coupled motion of these tilt boundaries.     

MOLECULAR DYNAMICS SIMULATION ON LOW ANGLE GRAIN BOUNDARIES

Molecular dynamics simulation has been performed to investigate the microstructure and properties of low angle grain boundaries, employing the embedded atom method(EAM) type interatomic potential for Ni-Al alloy. The energies of the low angle grain boundaries with different dislocation densities were calculated, and the results indicate that the low angle grain boundary energy varies as a function of misorientation angle. The simulation was found in good agreement with the calculation on the basis of the dislocation theories in the low angle scale. The low angle grain boundary energy goes up with the increase of misorientation angle and tends to go down after reaching a maximum. An energy cusp exists when the misorientation angle increases further, but in this scale the dislocation theories are invalid for energy calculation due to the strong interaction of the dislocations at the boundaries. The simulation results also indicate that the microstructure of low angle grain boundaries can still be described as dislocations when the misorientation angle is larger than 10°.     

Spin-dependent electron transport in manganite bicrystal junctions

Magnetic bicrystal films and junctions of magnetic La_0.67Sr_0.33MnO₃ (LSMO) and La_0.67Ca_0.33MnO₃ (LCMO) films epitaxially grown on NdGaO₃ substrates with the (110) planes of their two parts misoriented (tilted) at angles of 12°, 22°, 28°, and 38° are investigated. For comparison, bicrystal boundaries with a 90° misorientation of the axes of the NdGaO₃ (110) planes were fabricated. The directions of the axes and the magnetic anisotropy constants of the films on both sides of the boundary are determined by two independent techniques of magnetic resonance spectroscopy. The magnetic misorientation of the axes in the substrate plane has been found to be much smaller than the crystallographic misorientation for tilted bicrystal boundaries, while the crystallographic and magnetic misorientation angles coincide for boundaries with rotation of the axes. An increase in the magnetoresistance and characteristic resistance of bicrystal junctions with increasing misorientation angle was observed experimentally. The magnetoresistance of bicrystal junctions has been calculated by taking into account the uniaxial anisotropy, which has allowed the contributions from the tunneling and anisotropic magnetoresistances to be separated. The largest tunneling magnetoresistance was observed on LCMO bicrystal junctions, in which the characteristic resistance of the boundary is higher than that in LSMO boundaries.     

Asymmetric tilt grain boundary structure and energy in copper and aluminium

Atomistic simulations were employed to investigate the structure and energy of asymmetric tilt grain boundaries in Cu and Al. In this work, we examine the Σ5 and Σ13 systems with a boundary plane rotated about the ? 100 ? misorientation axis, and the Σ9 and Σ11 systems rotated about the ? 110 ? misorientation axis. Asymmetric tilt grain boundary energies are calculated as a function of inclination angle and compared with an energy relationship based on faceting into the two symmetric tilt grain boundaries in each system. We find that asymmetric tilt boundaries with low index normals do not necessarily have lower energies than boundaries with similar inclination angles, contrary to previous studies. Further analysis of grain boundary structures provides insight into the asymmetric tilt grain boundary energy. The Σ5 and Σ13 systems in the ? 100 ? system agree with the aforementioned energy relationship; structures confirm that these asymmetric boundaries facet into the symmetric tilt boundaries. The Σ9 and Σ11 systems in the ? 110 ? system deviate from the idealized energy relationship. As the boundary inclination angle increases towards the Σ9 (221) and Σ11 (332) symmetric tilt boundaries, the minimum energy asymmetric boundary structures contain low index {111} and {110} planes bounding the interface region.     

Structure and morphology of nanosized lead inclusions in aluminum grain boundaries

Grain boundary lead inclusions formed by ion implantation of mazed bicrystal aluminum films have been investigated by transmission electron microscopy. The vapor-grown bicrystal films contained mainly 90°(110) tilt boundaries with fixed misorientation but variable inclination, as well as some growth twins with 70.5°(110) symmetrical tilt boundaries and a few small-angle boundaries. It was found that the shape, size and orientation of the inclusions in the grain boundaries depend on the orientation of the aluminum grain boundary plane. Inclusions at 90°(110) tilt boundaries were invariably sharply faceted toward one aluminum grain and more rounded toward the other grain. The faceted side was a section of the cuboctahedral equilibrium shape of bulk lead inclusions in parallel topotaxy with the aluminum matrix. The rounded side, where the aluminum grain was rotated by 90° with respect to the lead lattice, approximated a spherical cap. At specific low-energy segments of the grain boundary where a (100) plane in grain 1 meets an (011) plane in grain 2, only two of several possible shapes were observed. One of these was preferred in as-implanted samples while both types were found after melting and re-solidification of the lend inclusions. The observations are discussed in terms of a modified Wulff construction.     

Grain boundary diffusion of Cu in TiN film by X-ray photoelectron spectroscopy

In this study, the grain boundary diffusion of Cu through a TiN layer with columnar structure was investigated by X-ray photoelectron spectroscopy (XPS). It was observed that Cu atoms diffuse from the Cu layer to the surface along the grain boundaries in the TiN layer at elevated temperature. In order to estimate the grain boundary diffusion constants, we used the surface accumulation method. The diffusivity of Cu through TiN layer with columnar structure from 400 °C to 650 °C is D_b≈6×10⁻¹¹exp(−0.29/(k_BT )) cm²/s. Received: 18 May 1999 / Accepted: 8 September 1999 / Published online: 23 February 2000     

Cut-off deviation for CSL boundaries in recrystallized face-centered cubic materials

Abstract

Brandon’s criterion is frequently used to quantify distribution of coincident site lattice (CSL) boundaries in studies related to grain boundary character distribution. This criterion is based on theoretical considerations and is meant to define a range within which special boundaries may exist. Experiments have repeatedly shown that this range includes boundaries which do not show special properties. A broad aim of this study is to explore if there exists a cut-off in deviation which includes only boundaries with special properties. While most other criteria in literature are based on theoretical dependence of secondary dislocation spacing, in this work we find the cut-off deviation through experimental data of recrystallised microstructures from in situ as well as ex-situ heating experiments. Deviation from structure was considered in terms of both, deviation of misorientation axis-angle as well as deviation of the boundary plane from the symmetric tilt orientation. Our results indicate that the deviation in terms of misorientation angle is more important than boundary plane deviation. We also show that the limiting deviation for various orders of twin boundaries (Σ3ⁿ) in a recrystallized microstructure is a constant and approximately 1° which is significantly lower than that defined by Brandon’s criterion. We show that this constant cut-off deviation for various Σ3ⁿ CSL boundaries can also be obtained by assuming that the secondary dislocations are spaced proportional to displacement shift complete lattice vector. Similar analysis was also carried out for non-Σ3ⁿ boundaries but due to limited statistics, no cut-off value could be deduced for these boundaries.     

Grain boundaries in the refined solidification structure of undercooled Ni75Pd25

When a single-phase alloy solidifies in a low-undercooling range or above a critical undercooling, grain-refined structures are obtained. Taking Ni₇₅Pd₂₅ alloy as an example, the microscopic orientation of the refined grains was investigated by electron backscattered diffraction technology. It is revealed that the refined grains at low undercooling are completely randomly distributed. In the refined structure at high undercooling, certain grain boundaries with misorientation angles less than 5° can be observed, while most of the grain boundaries have large misorientation angles. The inverse pole figure indicates that the refined grains at high undercooling have a textured crystallographic orientation. The fact that twins exist in the refined structure at high undercooling and the dendritic substructure arms exhibit no misorientation supports such an argument that the grain refinement at high undercooling results from the recrystallization of the solidification dendrites.     

Refined Prediction and Observation of Dislocation Structures in Low Σ Symmetric Grain Boundaries

The grain boundary dislocation structures of three Fe–4at.% Si bicrystals with an additional misorientation of the order of 2° were studied by transmission electron microscopy (TEM), one S5 [001] (310) and two S9 [110] (1 [`1]\overline 1 4). It was found that in the S5 case two Burgers vectors of the structure are not simple basic complete displacement shift lattice (DSC) vectors and are larger than any one of them. This enabled formation of the preferred grain boundary dislocation (GBD) structure with a hexagonal net composed of three screw dislocations and an independent set of parallel edge dislocations. In the S9 case the GBD structure comprises three apparently independent sets of parallel dislocations. The Burgers vectors of two sets could be established as basic DSC vectors in screw and edge orientation, respectively, with respect to the GB plane. For the third set formed by separated groups of four dislocations no corresponding basic DSC vector exists. This case needs further investigation. The previously published table of predicted GBD structures for symmetrical coincidence boundaries up to S11 was refined according to the new results.     

Heteroepitaxy of GexSi1 ? x (x ～ 0.4–0.5) films on Si(001) substrates misoriented to (111): Formation of short edge misfit dislocations alone in the misorientation direction

Relaxation of mechanical misfit stresses in Ge _x Si_{1 − x} (x ∼ 0.4–0.5) epitaxial films grown by molecular epitaxy on Si substrates misoriented from the exact orientation (001) by an angle of 6° has been studied. Possible cases of induced nucleation and interaction of 60° misfit dislocations (MDs) propagating in the misorientation direction with the formation of short edge MD segments are considered. Such configurations are classified and their various forms experimentally detected by TEM are presented. It is shown that short edge MDs are formed by two different mechanisms: (A) correlated or induced nucleation of a complementary 60° dislocation half-loop followed by the formation of an edge dislocation segment; and (B) the formation of a 90° MD segment upon intersection of the already existing complementary 60° MDs gliding in oppositely inclined {111} planes. The nonequivalency of the interaction of 60° MDs propagating in opposite directions along the substrate misorientation is shown.     

Atomistic simulations of interactions between the 1 / 2⟨111⟩ edge dislocation and symmetric tilt grain boundaries in tungsten

The strength of polycrystals is largely controlled by the interaction between lattice dislocations and grain boundaries. The atomistic details of these interactions are difficult to discern even by advanced high-resolution microscopy methods. In this paper we present results of atomistic simulations of interactions between an edge dislocation and three symmetric tilt grain boundaries in body-centred cubic tungsten. Our simulations reveal that the outcome of the dislocation–grain-boundary interaction depends sensitively on the grain boundary structure, the geometry of the slip systems in neighbouring grains, and the precise location of the interaction within the grain boundary. A detailed analysis of the evolution of the grain boundary structures and local stress fields during dislocation absorption and transmission is provided.     

Thermodynamic and Kinetic Properties of Grain-Boundary Ridges on Tilt $$[11\bar 20]$$ Grain Boundaries in Zinc

Thermodynamic and kinetic properties characteristic of grain-boundary ridges on tilt \([11\bar 20]\) grain boundaries in zinc are studied experimentally. Temperatures are determined for faceting–defaceting and roughening phase transitions in grain-boundary ridges for tilt \([11\bar 20]\) grain boundaries with 35°, 57°, and 85° angles of misorientation. Mobilities and enthalpies of activation are obtained for grain-boundary ridges on the same boundaries. Parameters of inhibition are also calculated for grain-boundary ridges, according to the observed shapes of grain-boundary loops.     

非对称倾侧亚晶界的晶体相场法研究

采用晶体相场法研究非对称倾侧亚晶界结构及其在应力作用下的微观运动机制.分别从温度、倾斜度角以及应力施加方向等方面对其结构及迁移过程进行分析和讨论.结果表明,非对称倾侧亚晶界由符号相同的一排刃型位错等距排列,部分出现由两个相互垂直排列的刃型位错构成的位错组;在应力作用下,非对称倾侧亚晶界迁移的微观机制包括位错的滑移和攀移、位错组分解、单个位错与位错组反应、单个位错分解以及位错湮灭;温度降低和倾斜度增大都会阻碍亚晶界的迁移过程;应力方向改变导致位错运动方向改变,从而改变晶界迁移形式.     

Irradiation induced changes in small angle grain boundaries in mosaic Cu thin films

We studied the effect of irradiation on small angle grain boundaries in mosaic structured Cu thin films. The films showed a decrease in mosaic spread via a narrowing of the full width at half maximum in XRD rocking curves and a smaller minimum yield of RBS channeling after irradiation. These data indicate the irradiation decreased the misorientation angles between mosaic blocks separated by small angle grain boundaries. Mechanisms involving interactions between grain boundary dislocations and irradiation induced defects are discussed.     

Symmetrical high-T c superconducting bicrystal Josephson junctions: Dependence of the electrical properties on the misorientation angle

The electrical properties of junctions at symmetrical bicrystal boundaries in high-T _c superconducting films are studied as functions of the misorientation angle in the range 8°–45°. The junctions are prepared by growing YBa₂Cu₃O₇ (YBCO) epitaxial films on Y-ZrO₂ (YSZ) bicrystal substrates. The proportional relationship between the characteristic voltages and the normal conductivities of junctions is derived from the dependences of the critical current and the normal resistance on the misorientation angle. The results are interpreted within the model of a superconductor-dielectric with defect levels in the band gap of the superconductor. The deviations from the proportional relationship are explained by the junction inhomogeneity. The thickness of the effective dielectric layer in the bicrystal junction and the Bohr radius of electrons on the defects are estimated.     

Formation of misfit edge dislocations in Ge x Si1 ? x films ( x ～ 0.4–0.5) grown on tilted Si(001) → (111) substrates

The dislocation structure of Ge _x Si_{1 − x} films (x ∼ 0.4–0.5) grown by molecular epitaxy on Si(001) substrates tilted by 6° about the 〈011〉 axis was studied. It is shown that, in the tilt direction, edge misfit dislocations (MDs) arise only in the form of short segments lying on the intersections of 60° MDs. As a result, the total length of edge MDs along the substrate tilt direction is smaller than that along the tilt axis. The deviation of the substrate surface from the singular plane made it possible to detect a dislocation configuration that consists of a short segment of an edge MD and two diverging 60° MDs propagating from it in the tilt direction. The formation of the segment is assumed to begin with simultaneous nucleation of complementary dislocation half-loops that form a short edge MD on the interface and then propagate on one side as two diverging 60° MD lines. Original Russian Text ? Yu.B. Bolkhovityanov, A.K. Gutakovskii, A.S. Deryabin, L.V. Sokolov, 2008, published in Fizika Tverdogo Tela, 2008, Vol. 50, No. 10, pp. 1783–1787.     

An extended read model for grain boundaries in GaAs

The space charging properties of grain boundaries in GaAs are discussed using an extended Read dislocation model. Model calculations for medium to high angle grain boundaries show: (1) the core-site occupational probability for a dislocation at the grain boundary is at least an order of magnitude lower than would be expected on the basis of simple Read theory; (2) due to the strong core-core interaction of the dislocations, the depletion width W decreases with an increase in tilt angle θ: and (3) W is approximately independent of θ in highly doped (N_D ? 10₁₇/cm³) material. Comparisons between model predictions and experimentally determined depletion widths of grain boundaries in GaAs are presented.     

Nucleation of dynamic recrystallization and variant selection in copper bicrystals

Orientation-controlled copper bicrystals containing [001] symmetrical tilt boundaries aligned parallel to the loading axis were deformed in tension at 923?K and a strain rate of 4.2?×?10^?4?s^?1. The nucleation of dynamic recrystallization (DRX) was investigated along the grain boundary. For this purpose, both optical and orientation imaging microscopy methods were used. After grain-boundary migration (GBM) and bulging, nuclei appeared behind the most deeply indented grain boundary regions. The critical strain for nucleation was about one-quarter to one-half of the peak strain and depended on the misorientation angle. All the nuclei were twin-related (Σ3) to the matrices. Furthermore, all the primary twin traces were parallel to those of the inactive slip planes of the parent single crystals. Crystallographic analysis revealed the important role of the direction of GBM on twinning-plane variant selection. The characteristics of grain boundary nucleation depended sensitively on grain boundary character and on grain boundary mobility. The observed DRX nucleation mechanism is discussed in relation to the occurrence of GBM and twinning.     

双晶铝晶界弛豫的转变温度

测量了夹角分别为60°和153.4°的[110]对称倾侧铝双晶晶界的扭转滞弹性蠕变曲线,指出了晶界的弛豫强度在低于温度T₀时变为零,此温度(T₀)约等于该金属的熔点温度(T_m)的二分之一,这说明晶界的内部结构在这个温度的附近发生了显著的变化。 关键词：