Cu-paddle-wheel-based Cu3(BTC)2 (nicknamed Cu-BTC, where BTC ≡ benzene 1,3,5-tricarboxylate) is a metal organic framework (MOF) compound that adopts a zeolite-like topology. We have determined the pore-size distribution using the Gelb and Gubbins technique, the microstructure using small-angle neutron scattering and (ultra) small-angle X-ray scattering (USAXS\SAXS) techniques, and X-ray powder diffraction reference patterns for both dehydrated d-Cu-BTC [Cu3(C9H3O6)2] and hydrated h-Cu-BTC [Cu3(C9H3O6)2(H2O)6.96] using the Rietveld refinement technique. Both samples were confirmed to be cubic Fm$\bar 3$m (no. 225), with lattice parameters of a = 26.279 19(3) Å, V = 18 148.31(6) Å3 for d-Cu-BTC, and a = 26.3103(11) Å, and V = 18 213(2) Å3 for h-Cu-BTC. The structure of d-Cu-BTC contains three main pores of which the diameters are approximately, in decreasing order, 12.6, 10.6, and 5.0 Å. The free volume for d-Cu-BTC is approximately (71.85 ± 0.05)% of the total volume and is reduced to approximately (61.33 ± 0.03)% for the h-Cu-BTC structure. The d-Cu-BTC phase undergoes microstructural changes when exposed to moisture in air. The reference X-ray powder patterns for these two materials have been determined for inclusion in the Powder Diffraction File.

HighScore with the Plus option (HighScore Plus) is the commercial powder diffraction analysis software from PANalytical. It has been in constant development over the last 13 years and has evolved into a very complete and mature product. In this paper, we present a brief overview of the suite focusing on the latest additions and its user-friendliness. The introduction briefly touches some basic ideas behind HighScore and the Plus option.

The evolution of the 003 reflection of the layered Li(Ni,Co,Mn)O2 (CGR) and Li(Ni,Co,Al)O2 (NCR) cathodes in commercial 18650 lithium-ion batteries during charge/discharge were determined using in situ neutron powder diffraction. The 003 reflection is chosen as it is the stacking axis of the layered structure and shows the largest change during charge/discharge. The comparison between these two cathodes shows that the NCR cathode exhibits an unusual contraction near the charged state and during the potentiostatic step, where the potentiostatic step is recommended by the manufacturer. This feature is not shown to the same degree by the CGR cathode. The behavior is likely related to the compositions of these cathodes, the amount of Li/Ni site mixing and the presence of Al or Mn.

The possibilities of modelling the diffraction profiles from bimodal microstructure in computer program MSTRUCT are demonstrated on two examples. A special “Double Component” profile effect can be utilized for such problems. At first it was applied to an analysis of a mixture of two nanocrystalline anatase powders with different crystallite sizes and the relative ratio of both components was determined from X-ray diffraction data. In the second case study, diffraction peaks from a pure polycrystalline copper sample treated by equal channel angular pressing were fitted using a two-phase model of large recrystallized defect-free grains and ultrafine crystallites with high dislocation density. The method is shown to be suitable for determination of the relative fraction of the microstructural components as well as other parameters (e.g. dislocation density).

Ongoing software developments for creating three-dimensional (3D) printed crystallographic models seamlessly from Crystallographic Information Framework (CIF) data (*.cif files) are reported. Color versus monochrome printing is briefly discussed. Recommendations are made on the basis of our preliminary printing efforts. A brief outlook on new materials for 3D printing is given.

Synchrotron X-ray diffraction images are increasingly used to characterize not only structural and microstructural features of polycrystalline materials, but also crystal preferred orientation distributions. Diffraction data can be analyzed quantitatively and efficiently with the Rietveld method and here the detailed procedure is reported from the experiment to the calibration of the two-dimensional detector and full analysis of the sample. In particular, we emphasize the advantage of doing the calibration inside the Rietveld least-squares fitting instead of a preliminary graphical calibration. Then the procedure is described to quantify crystal preferred orientations with the Rietveld method implemented in software “Materials Analysis Using Diffraction”. The process is illustrated for a US “nickel” coin, a 75 at.% copper 25 at.% nickel alloy with face-centered cubic structure and a strong cube texture.

A first attempt to differentiate goethite- and hematite-based natural materials, used for several purposes during the Late Palaeolithic in the Lessini Mountains (Italy), is here proposed. All raw materials were collected from known geological sites within a distance of about 20 km from archaeological excavations (Tagliente and Fumane caves) where ochre fragments were found. X-ray powder diffraction allowed the mineralogical composition of samples collected from carbonate and volcanic geological host and parent rocks to be inferred; in addition, a preliminary distinction based on the different mineral assemblages, on the presence of distinctive mineral phases and on the degree of crystallinity of some compounds such as hematite, became possible. The acquired data thus represent a sort of preliminary inventory for provenance studies on archaeological samples originating in the same region, for which ancillary micro-analytical and geochemical techniques are planned.

Synchrotron X-ray diffraction images are increasingly used to characterize crystallographic preferred orientation distributions (texture) of fine-grained polyphase materials. Diffraction images can be analyzed quantitatively with the Rietveld method as implemented in the software package Materials Analysis Using Diffraction. Here we describe the analysis procedure for diffraction images collected with high energy X-rays for a complex, multiphase shale, and for those collected in situ in diamond anvil cells at high pressure and anisotropic stress.

The crystal structure of one isotropic [(1) Brazil] and three birefringent spessartine samples [(2) California, (3) Tanzania, and (4) Colorado] were refined using the Rietveld method, cubic space group $Ia\overline 3 d$, and monochromatic synchrotron high-resolution powder X-ray diffraction (HRPXRD) data. The results of electron-microprobe analysis (EMPA) indicate homogeneous compositions, in terms of end-members, as follows: (1) Sps54Alm43, (2) Sps90Alm8, (3) Sps64Prp27Grs3, and (4) Sps73Alm19. Their crystal structures were modeled well as indicated by the Rietveld refinement statistics where the reduced χ2 and overall R (F2) values for each sample are: (1) 1.395 and 0.0329, (2) 1.082 and 0.0354, (3) 1.025 and 0.0347, and (4) 1.016 and 0.0413. Two cubic phases occur in samples 2–4, and a single cubic phase occurs in sample-1. The dominant cubic phase-1 with locality, weight fraction (%), unit-cell parameter (Å), distances (Å), and site occupancy factors (sofs) are as follows: (1) Brazil: 100%, a = 11.581 54 (1), average <Mn–O> = 2.3156, Al–O = 1.8949 (3), Si–O = 1.6376 (3) Å, Mn(sof) = 0.961(1), Al(sof) = 0.945(1), and Si(sof) = 0.936(1); (2) California: 96.67(7)%, a = 11.613 32(1), average <Mn–O> = 2.3249, Al–O = 1.8956 (4), Si–O = 1.6416 (4) Å, Mn(sof) = 0.951(1), Al(sof) = 0.946(1), and Si(sof) = 0.927(1); (3) Tanzania: 69.46(6)%, a = 11.598 45(1), average <Mn–O> = 2.3199, Al–O = 1.8964 (5), Si–O = 1.6398 (5) Å, Mn(sof) = 0.808(1), Al(sof) = 0.942(1), and Si(sof) = 0.922(1); and (4) Colorado: 98.58(6)%, a = 11.606 89(1), average <Mn–O> = 2.3204, Al-O = 1.8948 (6), Si–O = 1.6450 (6) Å, Mn(sof) = 0.949(1), Al(sof) = 0.967(2), and Si(sof) = 0.913(2). The two-phase intergrowth causes strain that arises from mismatch of the structural parameters and gives rise to strain-induced birefringence.

The crystal structure of a morimotoite garnet, ideally Ca3(Ti4+Fe2+)Si3O12, from the Ice River alkaline complex, British Columbia, Canada was refined by the Rietveld method, space group $Ia\overline 3 d$, and monochromatic synchrotron high-resolution powder X-ray diffraction (HRPXRD) data. Electron-microprobe analysis indicates a homogeneous sample with a formula {Ca2.91Mg0.05Mn2+0.03}Σ3[Ti1.09Fe3+0.46Fe2+0.37Mg0.08]Σ2(Si2.36Fe3+0.51Al0.14)Σ3O12. The HRPXRD data show a two-phase intergrowth. The reduced χ2 and overall R(F2) Rietveld refinement values are 1.572 and 0.0544, respectively. The weight percentage, unit-cell parameter (Å), distances (Å), and site occupancy factors (sofs) for phase-1 are as follows: 76.5(1)%, a = 12.156 98(1) Å, average <Ca–O> = 2.4383, Ti–O = 2.011(1), Si–O = 1.693(1) Å, Ca(sof) = 0.943(2), Ti(sof) = 0.966(2), and Si(sof) = 1.095(3). The corresponding values for phase-2 are 23.5(1)%, a = 12.160 67(2) Å, average <Ca–O> = 2.452, Ti–O = 1.988(3), Si–O = 1.704(3) Å, Ca(sof) = 1.063(7), Ti(sof) = 1.187(7), and Si(sof) = 1.220(8). The two phases cause strain that arises from structural mismatch and gives rise to low optical anisotropy. Because the two phases are structurally quite similar, a refinement using a single-phase model with anisotropic displacement parameters shows no unusual displacement ellipsoid for the O atom that requires a “split O-atom position”, as was done in previous studies.