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A comprehensive approach is taken to investigate the “Hungarian mine green” pigment, including a historical overview, analysis of the pigment on artworks, and its laboratory replication. It is known that in the past, the pigment is collected in wooden reservoirs in which copper (Cu) compounds precipitated from drainage water during copper mining at Špania Dolina–Piesky and Ľubietová deposits, Slovakia. Microsamples of four polychrome wooden sculptures from the 16th‐17th centuries are examined. Posnjakite (Cu4SO4(OH)6·H2O) and malachite (Cu2(CO3)(OH)2) are most frequently detected by X‐ray powder microdiffraction. In rock samples from the mine site, brochantite (Cu4SO4(OH)6) and malachite are dominant, and in recent precipitates, only langite (Cu4SO4(OH)6·2H2O) is detected, remained in contact with leaking water. In the laboratory, the pigment is prepared by gradually enriching the starting CuSO4·5H2O solution with NaHCO3 in two series of experiments. The initial concentration of the reactants reflected the ratio of Cu2+: HCO3− = 1:1 found in the mine waters at the site, from which langite crystallizes. However, langite does not formed, while brochantite gradually transformed into posnjakite and subsequently malachite. The co‐occurrence of basic copper sulfates and carbonates and the characteristic grain morphology proved to be the main indicators of the pigment in artworks. Hungarian mine green, a pigment precipitated from drainage water containing basic copper sulfates and carbonates, represented an important product for painters with the peak of its production in the 16th and 17th centuries in the Banská Bystrica region (Slovakia). Morphological and compositional fingerprints have been described based on microanalysis of Late Gothic artworks and pigment's replication in the laboratory.

Magma ascent and eruption are driven by a set of internally and externally generated stresses that act upon the magma. We present microstructural maps around melt inclusions in quartz crystals from six large rhyolitic eruptions using synchrotron Laue X-ray microdiffraction to quantify elastic residual strain and stress. We measure plastic strain using average diffraction peak width and lattice misorientation, highlighting dislocations and subgrain boundaries. Quartz crystals across studied magma systems preserve similar and relatively small magnitudes of elastic residual stress (mean 53–135 MPa, median 46–116 MPa) in comparison to the strength of quartz (~ 10 GPa). However, the distribution of strain in the lattice around inclusions varies between samples. We hypothesize that dislocation and twin systems may be established during compaction of crystal-rich magma, which affects the magnitude and distribution of preserved elastic strains. Given the lack of stress-free haloes around faceted inclusions, we conclude that most residual strain and stress was imparted after inclusion faceting. Fragmentation may be one of the final strain events that superimposes stresses of ~ 100 MPa across all studied crystals. Overall, volcanic quartz crystals preserve complex, overprinted deformation textures indicating that quartz crystals have prolonged deformation histories throughout storage, fragmentation, and eruption.

Contradictory evidence from biogeomorphological studies has increased the debate on the extent of lichen contribution to differential rock surface weathering in both natural and cultural settings. This study, undertaken in Côa Valley Archaeological Park, aimed at evaluating the effect of rock surface orientation on the weathering ability of dominant lichens. Hyphal penetration and oxalate formation at the lichen-rock interface were evaluated as proxies of physical and chemical weathering, respectively. A new protocol of pixel-based supervised image classification for the analysis of periodic acid-Schiff stained cross-sections of colonized schist revealed that hyphal spread of individual species was not influenced by surface orientation. However, hyphal spread was significantly higher in species dominant on northwest facing surfaces. An apparently opposite effect was noticed in terms of calcium oxalate accumulation at the lichen-rock interface; it was detected by Raman spectroscopy and complementary X-ray microdiffraction on southeast facing surfaces only. These results suggest that lichen-induced physical weathering may be most severe on northwest facing surfaces by means of an indirect effect of surface orientation on species abundance, and thus dependent on the species, whereas lichen-induced chemical weathering is apparently higher on southeast facing surfaces and dependent on micro-environmental conditions, giving only weak support to the hypothesis that lichens are responsible for the currently observed pattern of rock-art distribution in Côa Valley. Assumptions about the drivers of open-air rock-art distribution patterns elsewhere should also consider the micro-environmental controls of lichen-induced weathering, to avoid biased measures of lichen contribution to rock-art deterioration.

Shear banding is a ubiquitous phenomenon of severe plastic deformation, and damage accumulation in shear bands often results in the catastrophic failure of a material. Despite extensive studies, the microscopic mechanisms of strain localization and deformation damage in shear bands remain elusive due to their spatial−temporal complexities embedded in bulk materials. Here we conducted synchrotron-based X-ray microdiffraction (μXRD) experiments to map out the 3D lattice strain field with a submicron resolution around fatigue shear bands in a stainless steel. Both in situ and postmortem μXRD results revealed large lattice strain gradients at intersections of the primary and secondary shear bands. Such strain gradients resulted in severe mechanical heterogeneities across the fatigue shear bands, leading to reduced fatigue limits in the high-cycle regime. The ability to spatially quantify the localized strain gradients with submicron resolution through μXRD opens opportunities for understanding the microscopic mechanisms of damage and failure in bulk materials.

Poly(L-lactide) (PLLA) is the structural material of the first clinically approved bioresorbable vascular scaffold (BVS), a promising alternative to permanent metal stents for treatment of coronary heart disease. BVSs are transient implants that support the occluded artery for 6 mo and are completely resorbed in 2 y. Clinical trials of BVSs report restoration of arterial vasomotion and elimination of serious complications such as late stent thrombosis. It is remarkable that a scaffold made from PLLA, known as a brittle polymer, does not fracture when crimped onto a balloon catheter or during deployment in the artery. We used X-ray microdiffraction to discover how PLLA acquired ductile character and found that the crimping process creates localized regions of extreme anisotropy; PLLA chains in the scaffold change orientation from the hoop direction to the radial direction on micrometer-scale distances. This multiplicity of morphologies in the crimped scaffold works in tandem to enable a low-stress response during deployment, which avoids fracture of the PLLA hoops and leaves them with the strength needed to support the artery. Thus, the transformations of the semicrystalline PLLA microstructure during crimping explain the unexpected strength and ductility of the current BVS and point the way to thinner resorbable scaffolds in the future.

Heterostructured materials (HSMs) have shown great potential for breaking the strength-ductility tradeoff. HSMs consist of heterogeneous zones that may have different sizes, shapes, compositions, structures, etc. Interactions and competitions among them often lead to unprecedented properties. However, due to the complex structures in a broad range of length scales, it is challenging to unravel deformation physics and strengthening mechanisms underlying extraordinary mechanical properties. Synchrotron x-rays provide powerful techniques and indispensable tools for investigating HSMs at various length scales. Here, we will present in situ high-energy x-ray diffraction and Laue x-ray microdiffraction techniques and their application in studying the HSMs. The principles of these techniques will be briefly introduced. We will focus on their application in studying stress partitioning and plastic accommodation during tensile deformation, thermo-driven and/or stress-driven phase transformations and various deformation microstructures like geometrically necessary dislocations and local stress/strain distributions, etc., in HSMs. Some important findings will be summarized. Challenging issues remain in studying HSMs and will be discussed.

Laue microdiffraction is an X-ray diffraction technique that allows for the non-destructive acquisition of spatial maps of crystallographic orientation and the strain state of (poly)crystalline specimens. To do so, diffraction patterns, consisting of thousands of Laue spots, are collected and analyzed at each location of the spatial maps. Each spot of these so-called Laue patterns has to be accurately characterized with respect to its position, size and shape for subsequent analyses including indexing and strain analysis. In the present paper, several approaches for estimating these descriptors that have been proposed in the literature, such as methods based on image moments or function fitting, are reviewed. However, with the increasing size and quantity of Laue image data measured at synchrotron sources, some datasets become unfeasible in terms of computational requirements. Moreover, for irregular Laue spots resulting, e.g., from overlaps and extended crystal defects, the exact shape and, more importantly, the position are ill-defined. To tackle these shortcomings, a procedure using convolutional neural networks is presented, allowing for a significant acceleration of the characterization of Laue spots, while simultaneously estimating the quality of a Laue spot for further analyses. When tested on unseen Laue spots, this approach led to an acceleration of 77 times using a GPU while maintaining high levels of accuracy.

Scanning X-ray microdiffraction is applied to determine the structural variations of cellulose microfibrils among the fiber cells, vessel cells and ray cells of beechwood. A longitudinal section of beechwood was raster scanned with an X-ray microbeam. This allows to collect diffraction patterns from cell walls of distinct cell types. While the diffraction patterns from fiber cells are dominated by the cellulose signal with a longitudinal orientation, the diffraction patterns from ray and vessel cells show transversal fiber alignment, however to a lower degree of orientation. Moreover, the scattering pattern at small angle region of ray and vessel cells become less pronounced than to fiber cells. These results suggest that the crystalline cellulose of fiber cells has a completely different structure at the meso and molecular level when compared to ray and vessel cellulose within beechwood.

The sea urchin tooth is a remarkable grinding tool. Even though the tooth is composed almost entirely of calcite, it is used to grind holes into a rocky substrate itself often composed of calcite. Here, we use 3 complementary high-resolution tools to probe aspects of the structure of the grinding tip: X-ray photoelectron emission spectromicroscopy (X-PEEM), X-ray microdiffraction, and NanoSIMS. We confirm that the needles and plates are aligned and show here that even the high Mg polycrystalline matrix constituents are aligned with the other 2 structural elements when imaged at 20-nm resolution. Furthermore, we show that the entire tooth is composed of 2 cooriented polycrystalline blocks that differ in their orientations by only a few degrees. A unique feature of the grinding tip is that the structural elements from each coaligned block interdigitate. This interdigitation may influence the fracture process by creating a corrugated grinding surface. We also show that the overall Mg content of the tooth structural elements increases toward the grinding tip. This probably contributes to the increasing hardness of the tooth from the periphery to the tip. Clearly the formation of the tooth, and the tooth tip in particular, is amazingly well controlled. The improved understanding of these structural features could lead to the design of better mechanical grinding and cutting tools.

Biodegradable polymers open the way to treatment of heart disease using transient implants (bioresorbable vascular scaffolds, BVSs) that overcome the most serious complication associated with permanent metal stents—late stent thrombosis. Here, we address the long-standing paradox that the clinically approved BVS maintains its radial strength even after 9 mo of hydrolysis, which induces a ∼40% decrease in the poly L-lactide molecular weight (Mn). X-ray microdiffraction evidence of nonuniform hydrolysis in the scaffold reveals that regions subjected to tensile stress during crimping develop a microstructure that provides strength and resists hydrolysis. These beneficial morphological changes occur where they are needed most—where stress is localized when a radial load is placed on the scaffold. We hypothesize that the observed decrease in Mn reflects the majority of the material, which is undeformed during crimping. Thus, the global measures of degradation may be decoupled from the localized, degradation-resistant regions that confer the ability to support the artery for the first several months after implantation.