The material characterization toolbox has recently experienced a number of parallel revolutionary advances, foreshadowing a time in the near future when material scientists can quantify material structure evolution across spatial and temporal space simultaneously. This will provide insight to reaction dynamics in four-dimensions, spanning multiple orders of magnitude in both temporal and spatial space. This study presents the authors’ viewpoint on the material characterization field, reviewing its recent past, evaluating its present capabilities, and proposing directions for its future development. Electron microscopy; atom probe tomography; x-ray, neutron and electron tomography; serial sectioning tomography; and diffraction-based analysis methods are reviewed, and opportunities for their future development are highlighted. Advances in surface probe microscopy have been reviewed recently and, therefore, are not included [D.A. Bonnell et al.: Rev. Modern Phys. in Review]. In this study particular attention is paid to studies that have pioneered the synergetic use of multiple techniques to provide complementary views of a single structure or process; several of these studies represent the state-of-the-art in characterization and suggest a trajectory for the continued development of the field. Based on this review, a set of grand challenges for characterization science is identified, including suggestions for instrumentation advances, scientific problems in microstructure analysis, and complex structure evolution problems involving material damage. The future of microstructural characterization is proposed to be one not only where individual techniques are pushed to their limits, but where the community devises strategies of technique synergy to address complex multiscale problems in materials science and engineering.

Strain-induced selective growth was investigated in a 1.5% temper-rolled Fe∼1%Si alloy using the electron backscatter diffraction (EBSD) technique. The EBSD technique was used to quantify the presence of orientation spreads within grains and to show that this particular case of selective growth can be directly related to differences in stored energy as reflected in the geometrically necessary dislocation content. The differences in stored energy were sufficient to give rise to selective growth as evidenced by bi-modal grain sizes.

The orientation distribution of crystalline grains in calcium phosphate coatings produced by pulsed laser deposition was investigated using an X-ray pole-figure diffractometer. Increased laser energy density of a KrF excimer laser in the 4–7 J/cm2 range leads to the formation of hydroxyapatite grains with the c-axis preferentially aligned perpendicularly to the substrates. This preferred orientation is most pronounced when the plume direction of incidence is normal to the substrate. This crystallographic texture of hydroxyapatite grains in the coatings is associated with the highly directional and energetic nature of the ablation plume. Anisotropic stresses, transport of hydroxyl groups, and dehydroxylation effects during deposition all seem to play important roles in texture development. Studies of cell adsorption using human Mesenchymal stem cells reveal that hydroxyapatite coatings with strong texture and random orientation show different cell adsorption behavior, which is consistent with the notion that protein attach differently on different faces of hydroxyapatite crystals. Cells seeded on textured coatings exhibit better spreading and adhesion compared to those placed on randomly oriented coatings.

Extended abstract of a paper presented at Microscopy and Microanalysis 2005 in Honolulu, Hawaii, USA, July 31--August 4, 2005

The presence of impurities in aluminum alloys is of great interest with respect to microstructural properties, specifically, the effect of solute on texture and anisotropy. This paper presents new evidence of the pronounced effect of solute drag based on in-situ annealing and Electron Backscatter Diffraction experiments of Zr-rich Al alloys subject to prior strain. A compensation effect was found for grain boundary mobility maxima for specific boundary types. Trends in activation energy as a function of boundary type support the observations of a compensation effect with respect to temperature. Evidence for irregular motion of boundaries from in-situ observations is discussed in reference to new theoretical results that suggest that boundaries migrating in the presence of solutes should move sporadically provided that the length scale at which observations are made is small enough. A study of both boundary motion and solute segregation to specific boundary types using Scanning Transmission Electron Microscopy and in-situ TEM is presented.

This paper investigates the effect of solute in Al alloys on grain boundary character and mobility based on experiments in which individual boundaries migrate under a stored energy driving pressure acquired from prior plastic strain; among those studied are Zr, Fe and Si. A compensation effect is noted for both alloys studied with respect to both temperature and solute content. As supported by the literature, boundaries exhibit a maximum mobility for a 38-39°<111> misorientation in initial annealing experiments; this mobility maximum is asymmetric with a sharp cutoff below 38-39° but a more gradual decrease at misorientations beyond 40°. The presence of a minimum at 38-39° is found at both higher temperatures and higher solute concentrations. A shift in texture dependency with solute and temperature is also observed. This transition from a local mobility maximum to a minimum is discussed within the context of recent developments in solute drag theory.

The grain boundary plane distributions in MgO, SrTiO3, MgAl2O4, and Al are compared at lattice misorientations with a coincident site density of greater than or equal to 1/9. In most situations, the most frequently adopted grain boundary orientation is a habit plane of low index and low surface energy that depends on the particular material. Cases where the most common boundary orientation is a plane of high planar coincident site density instead of a characteristic habit plane are rare. In fact, in most cases, the distributions of grain boundary planes at misorientations with high lattice coincidence are not substantially different from the distributions at other, more general misorientations. The results indicate that a model for grain boundary energy and structure based on grain surface relationships is more appropriate than the widely accepted models based on lattice orientation relationships.

Relative grain boundary energy as a function of misorientation angle has been measured in cube-oriented, i.e., <100> fiber-textured, 120 [.proportional]m-thick Al foil using orientation imaging microscopy and a statistical multiscale method. The energies of low-angle boundaries increase with misorientation angle, in good agreement with the Read-Shockley model. The relative energies of high-angle boundaries exhibit little variation with misorientation. Examination of the grain structure of <111> fiber-textured, 100 nm-thick Al films annealed at 400°C for 0.5-10 h shows 5 and 6 sided grains to be the most frequent, and the fraction of four-sided grains to be significant. The mean number of sides is slightly lower than the expected value of 6 for two- dimensional structures. Of lognormal, gamma and Rayleigh distributions, gamma gives the best fit to the grain size data in the films; however, the difference between gamma and lognormal is small. Grain growth is not self-similar and stagnates after one hour of annealing. The evolution of the grain size distribution with time indicates that the growth stagnation in the films is neither consistent with boundary pinning by grooving nor with conventional treatments of solute drag. Surface, elastic-strain and plastic-strain energy driving forces do not play a significant role in the grain growth and the subsequent stagnation since the films are strongly textured even in the as- deposited state. The steady-state distributions of reduced grain area for two-dimensional, Monte Carlo and partial differential equation based simulations show excellent agreement with each other, even when anisotropic boundary energies are used. However, comparison with experimental distributions reveals a significantly higher population of small grains in the experiments.

We report on tensile tests performed on thin sheet samples of tantalum that have a nearcolumnar structure. By annealing sheet of approximately 1 mm thickness at high temperatures, a columnar structure is generated with grain boundaries nearly perpendicular to the flat surfaces. The purpose of the experiments is to investigate the mechanical behavior in terms of crystal plasticity in a geometry that is readily amenable to both experimental characterization and computer simulation. Automated electron backscatter diffraction (EBSD) has been used to obtain orientation maps both before and after deformation. For the small strains used in this study (<10%), the grains deform rather uniformly with little evidence of cell formation. Analysis of the lattice rotations shows considerable scatter in the rotation axis and demonstrates significant disagreement with polycrystal plasticity calculations.

Annealing of dilute binary Cu(Ti), Cu(In), Cu(Al), Cu(Sn), Cu(Mg), Cu(Nb), Cu(B), Cu(Co) and Cu(Ag) alloy films resulted in the strongest <111> fiber texture for Cu(Ti) and the lowest resistivity for Cu(Ag). The behavior of the alloy films was compared and contrasted with that for a pure evaporated Cu film. Electron beam evaporated films with compositions in the range of 2.0-4.2 at% and thicknesses in the range of 420-560 nm were annealed at 400°C for 5 hours. Two different approaches were used to derive volume fractions of texture components, namely fiber plots and orientation distributions. It is argued that for polytextured films such as the copper alloys studied here, orientation distributions derived from pole figures provide the most reliable basis for quantitative characterization.

It is known that by controlling microstructural development, desirable properties of materials can be achieved. The main objective of our research is to understand and control interface dominated material properties, and finally, to verify experimental results with computer simulations. We have previously showed a strong similarity between small-scale grain growth experiments and anisotropic three-dimensional simulations obtained from the Electron Backscattered Diffraction (EBSD) measurements [1]. Using the same technique, we obtained 5170-grain data from an Aluminum-film (120μm thick) with a columnar grain structure. Experimentally obtained starting microstructure and grain boundary properties are input for the three-dimensional grain growth simulation. In the computational model, minimization of the interface energy is the driving force for the grain boundary motion. The computed evolved microstructure is compared with the final experimental microstructure, after annealing at 550°C.

Annealing Cu and dilute Cu(Ti), Cu(Sn) and Cu(Al) alloy films resulted in the strengthening of film texture, with the strongest <111> fiber texture being found for Cu(Ti). Annealing also resulted in a decrease of electrical resistivity and the growth of grains, with the largest grain size and lowest resistivity being seen for pure Cu itself. Among the alloy films, the lowest resistivity was found for Cu(Ti) and the largest grain size for Cu(Al). Electron beam evaporated films with compositions in the range of 2.0-3.0 at% and thicknesses in the range of 420-540 nm were annealed at 400°C for 5 hours. Four point probe resistance measurement, xray diffraction and transmission electron microscopy were used to follow the changes in film resistivity, texture and grain size.

Complete control of the texture of a film during growth requires the ability to determine the in-plane and out-of-plane texture simultaneously. We present both computer simulation and experimental evidence for the simultaneous establishment of out-of-plane and in-plane texture during ion beam assisted deposition of aluminum. Channeling along 〈110〉 directions (60° from the normal) creates a {220} out-of-plane orientation rather than the thermodynamically preferred {111} orientation. The ion beam also aligned 〈220〉 directions within the plane of the film. Measured x-ray pole figures confirmed the presence of a strong out-of-plane texture and the presence of two main, twin-related, in-plane texture components. We theoretically demonstrated that it is impossible to completely control both the in-plane and out-of-plane texture with a single ion beam in high-symmetry crystals and two ion beams must be employed to ensure complete texture control.

The simulation of curvature driven growth in grain boundary systems is becoming an important tool in understanding the behavior of microstructure evolution and there is much distinguished work in this subject. Here we address the mesoscale simulation of large systems of grain boundaries subject to the Mullins equation of curvature driven growth with the Herring force balance equation imposed at triple junctions. We discuss several novel features of our approach which we anticipate will render it a flexible, scalable, and robust tool to aid in microstructural prediction. What is the result of the simulation? We discuss what such a simulation is capable of predicting, taking as a prototype the histogram of relative area population as it changes through the simulation. We do not use this data to seek the best distribution, like Hillert, Rayleigh, or lognormal. Instead we treat the set of distributions as the solution of an inverse problem for a time varying function and determine the equation they satisfy. This results in a coarse graining of the complex simulation to simpler system governed by a Fokker-Planck Equation. Even so, fundamental questions concerning the predictability of simulations of large metastable systems arise from these considerations.

Grain boundary and crystallographic orientation information of an Al-foil with a columnar grain structure is characterized by Electron Backscattered Diffraction (EBSD) technique. The starting microstructure and grain boundary properties are implemented as an input for the three- dimensional grain growth simulation. In the computational model, minimization of the interface energy is the driving force for the grain boundary motion. The computed evolved microstructure is compared with the final experimental microstructure, after annealing at 550 °C. Good agreement is observed between the experimentally obtained microstructure and the simulated microstructure. The constitutive description of the grain boundary properties was based on a 1- parameter characterization of the variation in mobility with misorientation angle.

Measurement of the geometry of triple junctions between grain boundaries in polycrystalline materials is used to generate large sets of dihedral angles from which maps of the grain boundary energy are extracted. A preliminary analysis has been performed for samples of magnesia and aluminum based on a three-parameter description of grain boundaries. An extended form of orientation imaging microscopy (OIM) was used to measure both triple junction geometry via image analysis in the SEM and local grain orientation via electron back scatter diffraction. Serial sectioning with registry of both in-plane images and successive sections characterizes triple junction tangents from which true dihedral angles are calculated. If there is local equilibrium at each triple junction, we may apply Herring's relation. By limiting grain boundary character to a (three parameter) specification of misorientation for the preliminary analysis, we can neglect the torque terms and apply the sine law to the three boundaries. This provides two independent relations per triple junction between grain boundary energies and dihedral angles. By discretizing the misorientation and employing multiscale statistical analysis on large data sets, (relative) grain boundary energy as a function of boundary character can be extracted from triple junction geometry. The results are discussed with respect to current understanding of grain boundary structure based on their crystallography. The results suggest that a three parameter characterization of grain boundaries (lattice disorientation) is not an adequate description of boundary character. A full analysis including torque terms and a five parameter boundary description is under development.

We have calculated the mechanical properties of brittle composites with spring-network (SN) model. The composites that we studied involve the transformation toughening effects and the accompanying micro-cracking. Our simulation results are consistent with experiments of MoSi2 toughened with ZrO2. By monitoring the stress changes due to the transformation and micro-cracking we are able to separate, for the first time, the contributions from these two competing effects. We also found that the fracture toughness of the composite increases as the modulus, interfacial cohesion of particle increases.

The properties of thin films prepared by coevaporation of Y, Cu and Ba.F2, followed by post anneals in O2/H2O, are described. In particular, we emphasize what is known about. the relationship between the processing variables and the physical and chemical structure of the resulting films.