Knowledge of the surface composition of planetary bodies comes from a number of sources; such as landers, remote sensing and meteorites. However, the bulk mapping of the composition of planetary surfaces has been undertaken by analysis of reflected sunlight and these data—principally collected in the near-infra-red (IR) region—are notoriously broad and ambiguous. Hence, if laboratory spectra could be tied to physical properties measurements, such as diffraction, this would substantially aid our understanding of processes occurring in these extra-terrestrial environments. This contribution presents the capability of collecting near-IR data at the same time as neutron and synchrotron X-ray diffraction in a range of conditions (low temperature, vacuum, and humidity variations) and highlights two examples where this capability could enhance our understanding of planetary surfaces.

The grazing incidence diffraction (GID) method in side inclination mode, described by Ma et al. in 2002, of polycrystalline thin-film residual stress was revisited and explained using simple geometric relations. To overcome the issue of decreasing peak intensity of this method, which is induced by the decreasing incident angle because of the Eulerian cradle Chi-tilt, an improvement of Omega (ω)–Phi (φ) compensation was devised and applied to a NiFe thin-film sample. The geometry of this improved ω–φ compensated GID method in side inclination mode is detailed in this paper. This improvement guarantees a constant incident angle on the sample surface and a fixed sample illumination volume during measurement. The measured data were analysed using parametric refinement in DIFFRAC.TOPAS v6 software in Launch Mode, and details of the input file (.INP) are explained in this paper. The tensile stress of the NiFe thin-film sample was measured to be 1181 ± 85 MPa using this improved method.

Elemental, chemical, and structural analysis of polycrystalline materials at the micron scale is frequently carried out using microfocused synchrotron X-ray beams, sometimes on multiple instruments. The Maia pixelated energy-dispersive X-ray area detector enables the simultaneous collection of X-ray fluorescence (XRF) and diffraction because of the relatively large solid angle and number of pixels when compared with other systems. The large solid angle also permits extraction of surface topography because of changes in self-absorption. This work demonstrates the capability of the Maia detector for simultaneous measurement of XRF and diffraction for mapping the short- and long-range order across the grain structure in a Ni polycrystalline foil.

Characterization of semi and noncrystalline materials, monitoring structural phase transitions in situ, and obtaining structural information together with spatial distribution of the investigated material are only a few applications that hugely benefitted from the combination of high-energy X-rays and modern algorithms for data processing. This work examines the possibility of advancing these applications by shortening the data acquisition and improving the data quality by using the new high-energy PILATUS3 CdTe detector.

In pursuit of design and characterisation of Cu adsorbing in thin films, we present data from a large variety of Cu-K edge X-ray Absorption Near Edge Spectroscopy (XANES) spectra obtained from organic and inorganic standards. Additionally, we have explored the impact of beam damage inducing redox alterations. Polymer nanoparticles were tested against films to produce higher concentration samples while maintaining high surface area to bulk effects. Spectra from nanoparticles were highly comparable to thin films of ~8 nm thickness, implying comparable contributions by surface effects on copper association. Finally, we observed no impact on Cu XANES spectra from vitrification with dimethyl sulfoxide to produce amorphous frozen, hydrated samples. The spectra should act as a valuable resource in assisting the design of experiments and identification of copper associations.

A robust analysis script was developed in MATLAB for cross-correlative quantification of internalised gold nanoparticle (AuNP) uptake in a large number of individual cells with the corresponding number of DNA double-strand breaks (DSBs) in the same cells. The correlation of inorganic NP content with a biological marker at the single-cell level will aid in the elucidation of mechanisms of NP radiosensitisation. PC-3 cells were co-cultured with AuNPs and irradiated using an iridium-192 source. AuNP uptake was measured using synchrotron X-ray fluorescence (XRF) and DSBs imaged via confocal microscopy. MATLAB 2016a was used to develop a script to cross-correlate the two imaging modalities and quantify both DSBs and internalised AuNP content in the same cell. Various user-defined options written into the script give a high degree of versatility, which can account for a large number of variables in experimental parameters and data acquisition. The analysis procedure is flexible and robust, which gives consistent consideration to the wide spectrum of potential input image/data sets. Quantitative correlative microscopy was achieved with a custom MATLAB script used to correlate γH2AX foci (a marker of DNA DSBs) from confocal microscopy with AuNP content acquired using synchrotron XRF at the single-cell level. The script can be extended to a broad range of multi-modality imaging spectroscopies.

The crystal structure and thermal expansion of the perovskite samarium cobalt oxide (SmCoO3) have been determined over the temperature range 295–1245 K by Rietveld analysis of X-ray powder diffraction data. Polycrystalline samples were prepared by a sol–gel synthesis route followed by high-temperature calcination in air. SmCoO3 is orthorhombic (Pnma) at all temperatures and is isostructural with GdFeO3. The structure was refined as a distortion mode of a parent $ Pm{\bar 3}m $ structure. The thermal expansion was found to be non-linear and anisotropic, with maximum average linear thermal expansion coefficients of 34.0(3) × 10−6, 24.05(17) × 10−6, and 24.10(18) × 10−6 K−1 along the a-, b-, and c-axes, respectively, between 814 and 875 K.

Graphite has been widely used as a negative electrode material in lithium-ion batteries, and recently it has attracted attention for its use in potassium-ion batteries. In this study, the first in situ X-ray diffraction characterisation of a K/graphite electrochemical cell is performed. Various graphite intercalation compounds are found, including the stage three KC36 and stage one KC8 compounds, along with the disappearance of the graphite during the potassiation process. These results show new insights on the non-equilibrium states of potassium-ion intercalation into graphite in K/graphite electrochemical cells.

Analysis of in situ neutron powder diffraction data collected for the porous framework material Zn(hba) during gas adsorption reveals a two-stage response of the host lattice to increasing CO2 guest concentration, suggesting progressive occupation of multiple CO2 adsorption sites with different binding strengths. The response of the lattice to moderate CH4 guest concentrations is virtually indistinguishable from the response to CO2, demonstrating that the influence of host–guest interactions on the Zn(hba) framework is defined more strongly by the concentration than by the identity of the guests.

The electrochemical behaviour of a number of Pb-based anode alloys, under simulated electrowinning conditions, in a 1.6 M H2SO4 electrolyte at 45 °C was studied. Namely, the evolution of PbO2 and PbSO4 surface layers was investigated by quantitative in situ synchrotron X-ray diffraction (S-XRD) and subsequent Rietveld-based quantitative phase analysis (QPA). In the context of seeking new anode alloys, this research shows that the industry standard Pb-0.08Ca-1.52Sn (wt%) anode, when exposed to a galvanostatic current and intermittent power interruptions, exhibited poor electrochemical performance relative to select custom Pb-based binary alloys; Pb–0.73Mg, Pb–5.05Ag, Pb–0.07Rh, and Pb–1.4Zn (wt%). The in situ S-XRD measurements and subsequent QPA indicated that this was linked to a lower proportion of β-PbO2, relative to PbSO4, on the Pb-0.08Ca-1.52Sn alloy at all stages of the electrochemical cycling. The best performing alloy, in terms of minimisation of overpotential during normal electrowinning operation and minimising the deleterious effects of repeated power interruptions – both of which are significant factors in energy consumption – was determined to be Pb–0.07Rh.

A series of phase transformations of a novel fluoroaluminosilicate glass forming a range of fluorapatite glass-ceramics on sintering are reported. The sintering process induces formation of fluorapatite, mullite, and anorthite phases within the amorphous silicate matrices of the glass-ceramics. The fluoroaluminosilicate glass, SiO2–Al2O3–P2O5–CaO–CaF2, is prepared from waste materials, such as rice husk ash, pacific oyster shells, and disposable aluminium cans. The thermally induced crystallographic and microstructure evolution of the fluoroaluminosilicate glass towards the fluorapatite glass-ceramics, with applications in dental and bone restoration, are investigated by powder X-ray diffraction and small-angle neutron-scattering techniques.

The decrease in quality of Australian iron ore, coupled with the demand for more efficient energy use, means that closer monitoring and optimisation of process conditions for iron ore sinter production is required. Here, the suitability of using partial least-squares regression analysis of powder X-ray diffraction data, collected for iron ore sinter samples, for the prediction of iron ore sinter strength has been further assessed. In addition, a preliminary assessment of the effect of 2θ range on the quality of prediction has been made. For the purposes of process control, the level of correlation between predicted strength and actual sinter strength would inform an operator whether or not the process was operating within the acceptable limits, or whether there was a potential problem requiring further investigation or rapid intervention. Reducing the 2θ range was found to reduce the level of correlation between predicted and actual strength, to a point where the particular analysis may no longer be suitable for process control.

Slags sourced from a derelict zinc–lead–copper–silver–tungsten mine were examined for their bulk elemental composition and mineralogy. pH, oxidation–reduction potential, and the leachability of selected elements (sulphur, calcium, iron, copper, zinc, and lead) were assessed during a 130-day deionised water extraction conducted under oxic conditions. Slags were rich in silicon, iron, copper, zinc, and lead, hosted within minerals including quartz (SiO2), goethite [FeO(OH)], augite [Ca(Mg,AI,Fe)Si2O6], and lead (Pb0). Leachates from the slags increased in analyte concentration throughout the 130-day experiment, with iron, copper, zinc, and lead attaining >5 mg l−1 in some samples. These findings indicate that this pyrometallurgical waste should not be considered environmentally inert, as leachates emanating from them in the field might pose a significant risk to the environment.

CSIRO Minerals is developing new technologies and approaches for the in situ recovery (ISR) of valuable metals. ISR provides opportunities to process small and/or deep deposits and could create additional revenue for conventional uneconomic mines. Unlike for conventional processing, no standard methodology exists for characterizing sample suitability for ISR. The authors are developing a workflow to understand sample and deposit amenability to ISR processing. A South Australian low-grade iron-oxide-copper-gold sulphide ore was studied. A total of 37 drill cores samples were obtained from the ore sample for detailed mineralogical and leaching characterization. A range of characterization techniques including chemical analysis, X-ray fluorescence mapping, quantitative evaluation of minerals by scanning electron microscopy, computed tomography scanning, and bulk- and micro-X-ray diffraction analyses were applied to understand the ore mineralogy. Leaching tests at 50 °C were performed on selected samples to understanding their leaching behaviour. Mineralogical characterization found that copper was present mostly as discrete secondary copper sulphides distributed in various areas and at various specimen depths, which, in theory should be readily available for leaching, provided sufficient solution access exists. Leaching results showed steady copper recovery under the conditions tested. This study provides insight into understanding the suitability of an ore for ISR processing.

The thermal decomposition of mill scale, and the effect of mill scale addition on the formation and decomposition of Silico-Ferrite of Calcium and Aluminium (SFCA) and SFCA-I iron ore sinter bonding phases, has been investigated using in situ X-ray diffraction. Application of the external standard method of quantitative phase analysis of the in situ data collected during decomposition of the mill scale highlighted the applicability of this method for the determination of the nature and abundance of amorphous material in a mineral sample. Increasing mill scale addition from 2.6 to 10.6 and to 21.2 wt% in an otherwise synthetic sinter mixture composition designed to form SFCA did not significantly affect the thermal stability ranges of SFCA-I or SFCA, nor did it significantly affect the amount of each of SFCA or SFCA-I, which formed. This was attributed to the low impurity (i.e. Mn, Mg) concentration in the mill scale, and also the transformation to hematite during heating of the wüstite and magnetite present in the mill scale, with the hematite available for reaction to form SFCA and SFCA-I.

X-ray fluorescence spectrometry was used in mapping and spot analysis modes, to help identify which elements are useful for understanding the composition of ancient papyrus inks, for 25 papyri from four age groups. We report seven elements (Al, Si, P, S, Ca, Ti, Fe) which provide sufficient contrast to be useful for mapping analysis, and 16 elements (P, S, Cl, K, Ca, V, Mn, Ni, Cu, Zn, Rb, Sr, Nb, Ag, Ba, and Pb) which show significant differences through time. Only one element – Pb – showed sufficient contrast in the thin ink layer to be significantly different when measured on the ink and adjacent papyrus. There is greater complexity in the elemental compositions of the papyrus and ink than can be understood with a study this size and additional work is required to develop and explain the patterns observed here.

Archaeometrists use a variety of analytical methods to determine trace elements in ancient Greek silver coins, for provenance studies, understanding social and technological change, and authentication. One analytical problem which is little documented is understanding the horizontal spatial heterogeneity of coin elemental composition in micro-sampled areas, which are usually assumed to be uniform. This study analysed ten ancient Greek coins representative of silver circulating in the Aegean region in the sixth to third centuries BC. Scanning electron microscopy with energy dispersive spectrometry was used to map the spatial distribution of elements on coins that were abraded to remove the patina. Time of flight-secondary ion mass spectrometry was then conducted on selected coins, mapping an area ~100 × 100 µm and depth profiling from 0 to 10 µm. These data revealed the three-dimensional elemental complexity of the coins, in particular, the heterogeneity both in the patina and beneath it. These data will guide future authentication and provenance studies of larger sample sets of ancient Greek coins including the use of line scanning for laser ablation inductively coupled plasma mass spectrometry data collection rather than spot analyses, and non-destructive analytical techniques such as X-ray fluorescence spectrometry.