The crystal structure of single crystals of kaolinite from Keokuk, Iowa, was refined using data measured at the microfocus X-ray beamline at the ESRF, Grenoble, France (λ = 0.6883, T = room temperature). The volume of the crystals was 8 and 0.8 μm3, respectively. Unit-cell parameters are: a = 5.154(9) Å, b = 8.942(4) Å, c = 7.401(10) Å, α = 91.69(9)°, β = 104.61(5)°, γ = 89.82(4)°. Space group Cl is consistent with the observed data. All non-hydrogen atoms were independently refined with anisotropic displacement parameters. The positions and isotropic displacement parameters for the three interlayer H atoms were refined also. The position of the intralayer H was found by difference-Fourier methods, although refinement was not possible. Difference-Fourier maps suggested large anisotropic displacement vectors of this intralayer H, however, no evidence for a second maximum was found. The diffraction patterns show diffuse scattering in streaks parallel to [001]* through hkl reflections with hk ≠ 0, which is caused by stacking faults. No twinning was observed for either of the two crystals.

We report an approach to expand the effective number of pixels available to small, two-dimensional electron detectors. To do so, we acquire subsections of a diffraction pattern that are then accurately stitched together in post-processing. Using an electron microscopy pixel array detector (EMPAD) that has only 128 × 128 pixels, we show that the field of view can be expanded while achieving high reciprocal-space sampling. Further, we highlight the need to properly account for the detector position (rotation) and the non-orthonormal diffraction shift axes to achieve an accurate reconstruction. Applying the method, we provide examples of spot and convergent beam diffraction patterns acquired with a pixelated detector.

The program FAULTS has been used to simulate the X-ray powder diffraction (XRD), neutron powder diffraction (NPD), and electron diffraction (ED) patterns of several structural models for LiNi1/3Mn1/3Co1/3O2, including different types of ordering of the transition metal (TM) cations in the TM slabs, different amounts of Li+/NiII+ cation mixing and different amounts of stacking faults. The results demonstrate the relevance of the structural information provided by NPD and ED data as compared with XRD to characterize the microstructure of NMC (LiNi1−y-zMnyCozO2) compounds.

X-ray reflectometry is a powerful tool for investigating rough surface and interface structures. Presently, X-ray reflectivity is based on Parratt formalism, accounting for the effect of roughness by the theory of Nevot–Croce. However, the calculated results showed a strange phenomenon in that the amplitude of the oscillation because of interference effects increases in the case of a specific roughness of the surface. We propose that the strange results originated from the currently used equation because of a serious error in which the Fresnel transmission coefficient in the reflectivity equation is increased at a rough interface, and the increase in the transmission coefficient completely overpowers any decrease in the value of the reflection coefficient because of lack of consideration in diffuse scattering. In the present study, we present a new improved formalism that corrects this error, and thereby derives an accurate analysis of X-ray reflectivity from a multilayer surface, taking into account the effect of roughness-induced diffuse scattering.

Recently, a new experimental setup for quick X-ray reflectivity (q-XRR) measurements was proposed, which is based on simultaneous recording of an X-ray reflectivity curve over all angles of interest. This new setup for q-XRR allows measurements to be done within seconds, thus permitting studies of the time evolution of chemical, thermal, and mechanical changes at the surfaces and interfaces of different materials. Since the q-XRR measurement setup utilizes an extended X-ray source and detector, it is important to develop models and to account for the following two effects: (i) diffuse scattering associated with different points of the source and (ii) sample curvature. Models accounting for both effects are presented, and their influences on interpretation of the q-XRR measurement results are discussed.

The ordered structures in different doping levels (x = 0.1, 0.15, 0.2, 0.25, 0.3) of yttrium doped ceria (YDC, Ce(1−x)YxO2−δ) electrolytes were investigated by electron diffraction, high-resolution transmission electron microscopy (TEM), scanning TEM, and electron energy loss spectroscopy. Oxygen vacancy ordering was experimentally confirmed within the ordered structures. With increasing the doping level, the concentration of trivalent Ce cations was increased in YDC samples and such trivalent Ce cations were supposed to mainly exist in the ordered structures. Based on our electron microscopic observation and microanalysis, a crystal model for the ordered structures is proposed.

Energy-filtered electron diffraction and three-dimensional reciprocal lattice mapping was used to study the nature of diffuse scattering in magnetite above the Verwey transition temperature. Characteristic Huang scattering associated with a single molecular polaron is observed at room temperature. As the temperature is lowered, the experiment shows narrowing of diffuse scattering in the 〈001〉 directions and additional ringlike diffuse scattering at q ∼ 0.8, which suggests the presence of one-dimensional structures above the Verwey transition. Experimental measurements of temperature-dependent correlation lengths and diffuse scattering intensity indicate an increase in the number and length of the one-dimensional structure as the temperature is cooled toward the transition. This study demonstrates the electron sensitivity to atomic displacement and the quality of electron diffraction data for studying phase transition in complex materials.