The study presents the results of the influence of high-energy ball-milling time on the structure of the new β-type Ti–Ta–Nb–Zr alloys for biomedical applications. Initial elemental powders were mechanically alloyed in a planetary high-energy ball mill at different milling times (from 10 to 90 h). Observation of the powder morphology after various stages of milling leads to the conclusion that with the increase of the milling time the size of the powder particles as well as the degree of aggregation change. Clear tendency of crystalline size reduction at every stage of the grinding process is clearly observed. The X-ray diffraction results confirmed the formation of β phase during high-energy ball milling of the precursor mixture of Ti, Ta, Nb, and Zr. The Rietveld refinement method has shown that both the production method and the atomic radii of the elements used in the mechanical synthesis have influence on the structure. Furthermore, it was found that a broadening of the diffraction peaks with increase of the milling time results from an increase in the crystallites dispersion and an enlargement in the lattice distortion. The results indicate that this technique is a powerful and high productive process for preparing new β-titanium alloys with nanocrystalline structure and appropriate morphology.

The microstructure evolution (crystallite size and microstrain) as well as the residual stress of Cu thin films of various thicknesses (250 nm, 500 nm, and 1 μm) on passivated Si substrates during isochronal annealing was investigated by in situ X-ray diffraction measurements in the temperature range between 25 °C and 250 °C. Before annealing, the thermoelastic behavior was investigated excluding the occurrence of thermally activated relaxation processes occurring above ambient temperature by in situ stress measurements below ambient temperature. On this basis, above ambient temperature, effects of stress relaxation and emerging secondary stresses (due to grain growth and annihilation of crystal defects, giving rise to a considerable tensile stress contribution development) could be identified for all three layers in the temperature regime between ambient temperature and 250 °C. Grain growth in the nanocrystalline thin films started at much lower temperatures as compared to coarse-grained materials. The results were discussed in terms of the effects of different driving forces and grain-boundary mobilities acting in nanocrystalline materials.

In the present work, we are investigating the electronic transport mechanism for antimony-doped tin oxide (ATO) ultrathin films produced by a colloidal deposition process (CDP) of nanocrystals synthesized via a solvothermal route in organic medium. The ATO ultrathin films were prepared from nanoparticles containing 9 mol% of Sb and the observed electrical resistivity at room temperature was 1.55, 1.10 × 10−1, and 1.83 × 10−3 Ω cm, respectively, for the 40, 45, and 71 nm films. X-ray diffraction, transmission electron microscopy, scanning electron microscopy, and atomic force microscopy were carried out to investigate the films and electrical resistivity measurements taken in the four-probe mode with temperature ranging from −260 to 27 °C (13–300 K ± 0.1 K). Results show a good data fitting on Mott's two-dimensional (2D) noninteracting variable range hopping for the 45 nm thin film, which is not further observed for the ATO ultrathin films obtained from CDP.

This paper shows that pair-distribution function (PDF) analyses can be carried out on organic and organometallic compounds from powder electron diffraction data. Different experimental setups are demonstrated, including selected area electron diffraction and nanodiffraction in transmission electron microscopy or nanodiffraction in scanning transmission electron microscopy modes. The methods were demonstrated on organometallic complexes (chlorinated and unchlorinated copper phthalocyanine) and on purely organic compounds (quinacridone). The PDF curves from powder electron diffraction data, called ePDF, are in good agreement with PDF curves determined from X-ray powder data demonstrating that the problems of obtaining kinematical scattering data and avoiding beam damage of the sample are possible to resolve.

To evaluate the influence of strain rate on mechanical behavior of nanocrystalline (NC) materials, a phase mixture constitutive model composed of ordered grain interior phase and plastically softer grain boundary dislocation pile up zone phase was built. Because of dissimilar properties and mismatch between the two phases, dislocation density evolution controlling mechanism based on statistically stored dislocations and geometrically necessary dislocations was analyzed and extended to NC regime to consider their disparate effects. Based on the composite model, a new stress–strain constitutive relation for strain rate-dependent behaviors was firstly established based on dislocation density evolution and strain gradient theory. The calculated data were then compared with corresponding experimental curves and strong strain rate-dependent behaviors were exhibited, which indicated that the predictions kept in good agreement with experiments. Further discussions were presented for calculations of strain rate sensitivity and activation volume for NC Ni through the proposed model.

We report on the analysis of virtual powder-diffraction patterns from serial femtosecond crystallography (SFX) data collected at an X-ray free-electron laser. Different approaches to binning and normalizing these patterns are discussed with respect to the microstructural characteristics which each highlights. Analysis of SFX data from a powder of Pr0.5Ca0.5MnO3 in this way finds evidence of other trace phases in its microstructure which was not detectable in a standard powder-diffraction measurement. Furthermore, a comparison between two virtual powder pattern integration strategies is shown to yield different diffraction peak broadening, indicating sensitivity to different types of microstrain. This paper is a first step in developing new data analysis methods for microstructure characterization from serial crystallography data.

A new physical model of plastic deformation in nanocrystalline (NC) materials with finest grains (whose grain size is 2–4 nm) is suggested and theoretically described. The model represents the effect of the finest grains located at triple junctions on the fracture toughness of NC materials in the case that there are multiple dislocations pile-up at grain boundaries (GBs). The maximum number n of the pile-up dislocations is determined by both the capacity of dislocations emitting associated with the crack propagation and the capacity of dislocations pile-up due to the existence of the finest grains. The calculation indicates that the parameter n increases with increment of the grain size and decreases with the finest grain size increasing. The results theoretically reveal that the triple junctions with finest grains can significantly improve the fracture toughness of NC materials compared with the normal triple junctions in wide ranges of their structural parameters.

A theoretical model of nanovoid nucleation at triple junctions in nanocrystalline materials is developed in this article. The sliding of grain boundaries (GBs) meeting at triple junctions, which can be attributed to the gliding of GB dislocations (GBDs), provides the driving force for nanovoid nucleation. The GB sliding is accommodated by the emission of partial dislocations from GBs as well as GB diffusion. The corresponding energy characteristics of the pile-ups of GBDs, the emission of partial dislocations from the GBs, and GB diffusion are calculated, respectively. Furthermore, an energy balance method to calculate the nucleation of nanovoid at triple junctions is studied. The analysis demonstrates that the nucleation of the triple junction nanovoid depends mainly on the applied stress, the GB length (length of the pile-up), the GB structures, and the GB sliding accommodations.

The employment of the Debye function to model line profiles in the powder diffraction pattern from small crystallites is briefly reviewed. It is also demonstrated that for the case of very small spherical particles, it is necessary to average patterns from multiple constructions of the particle to have complete agreement with reciprocal space models. In doing so it is demonstrated that the technique of Debye function analysis is best suited for systems with only a few possible atomic arrangements.

As the presence of Sc2O3 and CeO2 is known to largely enhance the ionic conductivity in the temperature range of 600–800°C, compared with the conventional yttria-stabilized ZrO2, Sc2O3&CeO2-stabilized ZrO2 provide its applicability as electrolytes in solid oxide fuel cells. The current study introduces the methodology to synthesize Sc2O3&CeO2-stabilized ZrO2 powders by using co-precipitation technique or high-temperature hydrothermal reaction, and further describes the structural characterization of the zirconia powders synthesized by the above-mentioned two methods. The co-precipitation technique was found to allow obtaining powders of cubic phase, whereas high-temperature hydrothermal synthesis results in the presence of a monoclinic phase as well. The scanning transmission electron microscope observations also confirm that the size of the synthesized ZrO2 powders in this study is found to be much smaller than that of commercially available powders.

The method of high-energy total elastic X-ray scattering to determine the atomic structure of nanocrystalline, highly disordered, and amorphous materials is presented. The current state of the technique, its potential, and limitations are discussed with two successful studies on the pressure induced phase transition in mackinawite (FeS) and the high-pressure behavior of liquid gallium.

The diffraction pattern of nanocrystalline Ce0.9Zr0.1O2 was analyzed by whole powder pattern modeling, a recently proposed method for the study of line broadening. The main result in this typical case of study—the crystalline domain size distribution—matches closely the corresponding information obtained by transmission electron microscopy. Further information on nature and content of lattice defects is also discussed.

From 1967 to 2000 Daniel Louër of the Department of Crystal Chemistry, University of Rennes, and J. Ian Langford of the Department of Physics, University of Birmingham, collaborated in studying structural imperfections by means of high-resolution X-ray powder diffractometry. They contributed to the theory and practice of line profile analysis and investigated the microstructure of a variety of nanocrystalline materials. Although many of the projects undertaken were part of the research programme at Rennes to investigate the mechanisms of solid-state reactions, the work is relevant in other fields of materials science.

A general expression is proposed for the peak profile produced by a system of simple-shape crystalline domains (sphere, cube, tetrahedron, octahedron) whose size is dispersed according to a gamma distribution. The analytical expression obtained is particularly suited to “on the fly” pattern simulation or profile fitting for nanocrystalline materials. An advantage of using the proposed profile expression is that it always corresponds to a physically meaningful, though a priori fixed, size distribution, whereas the traditionally employed Voigtian profiles can produce unphysical negative size distributions for certain combinations of profile parameters. The peak profile depends on the distribution mean and variance instead of the more common empirical parameters of peak width and shape.

Four sol-gel TiO2 powders have been prepared from titanium tetraisopropoxide. The calcined powders are then characterized by X-ray diffraction. Cell parameters are extracted using two Rietveld refinement programs (FULLPROF and MAUD) leading to close values and indicating a contraction of the a (or b) cell parameter and an expansion of the c cell parameter of the anatase phase with temperature. Crystallite size and microstrain are highly dependent not only on the sol synthesis but also on the diffraction line profile analysis (LPA) models (i.e., Williamson-Hall, Thomson-Cox-Hastings, Dehlez et al., and log-normal size distribution) employed. Discrepancies are then observed for the phase transformation critical size, the activation energy of grain growth, and the microstrain stored potential energy according to the LPA approach used to calculate the microstructural parameters.

To analyze nanocrystalline structures quantitatively in 3D, a novel method is presented based on electron diffraction. It allows determination of the average size and morphology of the coherently scattering domains (CSD) in a straightforward way without the need to prepare multiple sections. The method is applicable to all kinds of bulk nanocrystalline materials. As an example, the average size of the CSD in nanocrystalline FeAl made by severe plastic deformation is determined in 3D. Assuming ellipsoidal CSD, it is deduced that the CSD have a width of 19 ± 2 nm, a length of 18 ± 1 nm, and a height of 10 ± 1 nm.

Focused ion-beam milling has been applied to prepare needle-shaped atom probe tomography specimens from mechanically alloyed powders without the use of embedding media. The lift-out technique known from transmission electron microscopy specimen preparation was modified to cut micron-sized square cross-sectional blanks out of single powder particles. A sequence of rectangular cuts and annular milling showed the highest efficiency for sharpening the blanks to tips. First atom probe results on a Fe95Cu5 powder mechanically alloyed in a high-energy planetary ball mill for 20 h have been obtained. Concentration profiles taken from this powder sample showed that the Cu distribution is inhomogeneous on a nanoscale and that the mechanical alloying process has not been completed yet. In addition, small clusters of oxygen, stemming from the ball milling process, have been detected. Annular milling with 30 keV Ga ions and beam currents ≥50 pA was found to cause the formation of an amorphous surface layer, whereas no structural changes could be observed for beam currents ≤10 pA.