Synchrotron-based Small-angle X-ray Scattering Research Articles

Annealing of swift heavy ion tracks in amorphous silicon dioxide

The annealing kinetics of the high energy ion damage in amorphous silicon dioxide (a-SiO2) are still not well understood, despite the material's widespread application in material science, physics, geology, and biology. This study investigates how annealing temperature, duration, and ambient environment affect the recovery of irradiation damage produced along the trajectory of swift heavy ions in a-SiO2. The track-annealing kinetics and the changing ion track morphology were investigated using synchrotron-based small-angle X-ray scattering (SAXS) and etching methods. We found that track annealing proceeds quicker near the sample surface demonstrated by a changing track etch rate as a function of depth. Measurements of ion tracks using SAXS show only small changes in the radial density distribution profile of the ion tracks. Activation energy of the annealing process at different sample depths was determined and the effect of the capping layer during the annealing process was also studied. Combination of oxygen diffusion and stress relaxation may contribute to the observed behaviour of preferential and anisotropic healing of the ion track. The results add to the fundamental understanding of ion track damage recovery and may have direct implications for materials for radioactive waste storage and solid state nanopores.

Collagen arrangement and strength in sausage casings produced from natural intestines

Natural sausage casings are made from the submucosa of intestines, a collagen-rich layer traditionally obtained from bovine, porcine and ovine sources. Collagen provides strength to animal tissues, in part due to the structural arrangement of the collagen fibrils. The collagen arrangement through the intestinal submucosa is not well characterised and the relationship of this structure with strength in not well understood. Synchrotron-based small angle X-ray scattering (SAXS) was used to determine the collage fibril orientation, orientation index (OI) and D-spacing of bovine, porcine and ovine sausage casings. Tear strength was measured both parallel and perpendicular to the length of the intestine. The D-spacing is similar (64.8–65.2 nm) in materials from all three species. The collagen fibrils are arranged in planar layers (OI = 0.86–0.91 measured with X-rays edge-on) and is similar in the three species. The fibril orientation is within 7° of the longitudinal direction of the intestine. OI measured normal to the surface is highest for bovine 0.49 (0.13), then porcine 0.35 (0.06) and ovine 0.33 (0.11). When normalized for thickness the tear strengths are similar for all species: bovine 8.8 (2.3) N/mm, porcine 6.4 (0.4) N/mm and ovine 8.3 (2.5) N/mm where the differences in absolute strength (bovine 4.1 (1.0) N, porcine 2.0 (0.3) N and ovine 1.0 (0.3) N) are due to differences in thickness. The material properties of the sausage casings from all three species is similar. This is a surprising finding since in other tissues (such as dermis of different animals, and pericardium of cattle of different ages) there are marked differences in the structural arrangement of collagen and these differences lead to fundamental differences in the mechanical properties of these materials. In summary, sausage casings from different species are structurally similar, other than thickness, and it is the thickness that is responsible for the different properties in use.

Shape of nanopores in track-etched polycarbonate membranes

High aspect-ratio nanopores of nearly cylindrical geometry were fabricated by irradiation of 20 μm thick polycarbonate (PC) foils with Pb ions followed by UV sensitization and etching in 5 M NaOH at 60 °C. Synchrotron-based small-angle X-ray scattering (SAXS) was used to study the morphology and size variation of the nanopores as a function of the etching time and ion fluence. The shape of the nanopores was found to be consistent with cylindrical pores with ends tapering off towards the two polymer surfaces in the last ~1.6 μm. The tapered structure of the nanopores in track-etched PC membranes was first observed more than 40 years ago followed by many other studies suggesting that the shape of nanopores in PC membranes deviates from a perfect cylinder and nanopores narrow towards both membrane surfaces. It was also reported that the transport properties of the nanopore membranes are influenced by the tapered structure. However, quantification of the shape of nanopores has remained elusive due to inherent difficulties in imaging the pores using microscopy techniques. The present manuscript reports on the quantitative measurement of the tapered structure of nanopores using SAXS. Determination of this structure was enabled by obtaining high quality SAXS data and the development of appropriate fitting models. The etch rates for both the radius at the polymer surface and the radius of the pore in bulk were calculated. Both etch rates decrease slightly with increasing fluence. This behavior is ascribed to the overlap of track halos which are characterized by cross-linking of the polymer chains. The halo radius was estimated to be approximately 120 nm. The influence of the observed nanopore shape on the pore transport properties was estimated and found to have a significant influence on the water flow rates compared to cylindrical pores. The results enable a better understanding of track-etched membranes and facilitate improved pore design for many applications.

Transformation Pathway from CdSe Magic-Size Clusters with Absorption Doublets at 373/393 nm to Clusters at 434/460 nm.

Divergent interpretations have appeared in the literature regarding the structural nature and evolutionary behavior for photoluminescent CdSe nanospecies with sharp doublets in optical absorption. We report a comprehensive description of the transformation pathway from one CdSe nanospecies displaying an absorption doublet at 373/393 nm to another species with a doublet at 433/460 nm. These two nanospecies are zero-dimensional (0D) magic-size clusters (MSCs) with 3D quantum confinement, and are labeled dMSC-393 and dMSC-460, respectively. Synchrotron-based small-angle X-ray scattering (SAXS) returns a radius of gyration of 0.92 nm for dMSC-393 and 1.14 nm for dMSC-460, and indicates that both types are disc shaped with the exponent of the SAXS form factor equal to 2.1. The MSCs develop from their unique counterpart precursor compounds (PCs), which are labeled PC-393 and PC-460, respectively. For the dMSC-393 to dMSC-460 transformation, the proposed PC-enabled pathway is comprised of three key steps, dMSC-393 to PC-393 (Step 1), PC-393 to PC-460 (Step 2 involving monomer addition), and PC-460 to dMSC-460 (Step 3). The present study provides a framework for understanding the PC-based evolution of MSCs and how PCs enable transformations between MSCs.

Transformation Pathway from CdSe Magic‐Size Clusters with Absorption Doublets at 373/393 nm to Clusters at 434/460 nm

AbstractDivergent interpretations have appeared in the literature regarding the structural nature and evolutionary behavior for photoluminescent CdSe nanospecies with sharp doublets in optical absorption. We report a comprehensive description of the transformation pathway from one CdSe nanospecies displaying an absorption doublet at 373/393 nm to another species with a doublet at 433/460 nm. These two nanospecies are zero‐dimensional (0D) magic‐size clusters (MSCs) with 3D quantum confinement, and are labeled dMSC‐393 and dMSC‐460, respectively. Synchrotron‐based small‐angle X‐ray scattering (SAXS) returns a radius of gyration of 0.92 nm for dMSC‐393 and 1.14 nm for dMSC‐460, and indicates that both types are disc shaped with the exponent of the SAXS form factor equal to 2.1. The MSCs develop from their unique counterpart precursor compounds (PCs), which are labeled PC‐393 and PC‐460, respectively. For the dMSC‐393 to dMSC‐460 transformation, the proposed PC‐enabled pathway is comprised of three key steps, dMSC‐393 to PC‐393 (Step 1), PC‐393 to PC‐460 (Step 2 involving monomer addition), and PC‐460 to dMSC‐460 (Step 3). The present study provides a framework for understanding the PC‐based evolution of MSCs and how PCs enable transformations between MSCs.

Bovine Meniscus Middle Zone Tissue: Measurement of Collagen Fibril Behavior During Compression.

BackgroundType I collagen is the major component of the extracellular matrix of the knee’s meniscus and plays a central role in that joint’s biomechanical properties. Repair and reconstruction of tissue damage often requires a scaffold to assist the body to rebuild. The middle zone of bovine meniscus is a material that may be useful for the preparation of extracellular matrix scaffolds.MethodsHere, synchrotron-based small-angle X-ray scattering (SAXS) patterns of bovine meniscus were collected during unconfined compression. Collagen fibril orientation, D-spacing, compression distance and force were measured.ResultsThe collagen fibrils in middle zone meniscal fibrocartilage become more highly oriented perpendicular to the direction of compression. The D-spacing also increases, from 65.0 to 66.3 nm with compression up to 0.43 MPa, representing a 1.8% elongation of collagen fibrils perpendicular to the compression.ConclusionThe elasticity of the collagen fibrils under tension along their length when the meniscus is compressed, therefore, contributes to the overall elastic response of the meniscus only under loads that exceed those likely to be experienced physiologically.

Disordering of helium gas bubble superlattices in molybdenum under ion irradiation and thermal annealing

Self-organization of gas bubbles causes the formation of an ordered array of nanoscale gas bubbles (a gas bubble superlattice), a highly efficient mechanism for gas storage under irradiation. The stability of helium (He) gas bubble superlattices in molybdenum (Mo) under krypton (Kr) ion irradiation and thermal annealing has been investigated. The He gas bubble superlattices gradually become disordered under Kr ion irradiation at 300°C, and the order-disorder transformation process completes at 2.5 dpa. Both transmission electron microscopy (TEM) and synchrotron-based small-angle X-ray scattering (SAXS) reveal that the order-disorder transformation of He gas bubble superlattices is associated with a slight increase in the average bubble size. Phase-field modeling indicates that the inhomogeneous growth and coarsening of bubbles/voids cause the disordering of imperfect superlattices under irradiation and implies that highly ordered superlattices could potentially exhibit much stronger resistance to irradiation damage. Under thermal annealing, the He gas bubble superlattices in Mo become unstable and disordered at 1000°C with the bubble size increasing from ∼1.1 to ∼1.6 nm. The finding in this research provides insights into the disordering mechanisms of defect superlattices as well as guidance for designing stable defect superlattices in harsh environments.

Characterization of Tobacco Mosaic Virus Virions and Repolymerized Coat Protein Aggregates in Solution by Small-Angle X-Ray Scattering.

The structure of tobacco mosaic virus (TMV) virions and stacked disk aggregates of TMV coat protein (CP) in solution was analyzed by synchrotron-based small-angle X-ray scattering (SAXS) and negative contrast transmission electron microscopy (TEM). TMV CP aggregates had a unique stability but did not have helical symmetry. According to the TEM data, they were stacked disks associated into transversely striated rod-shaped structures 300 to 800 Å long. According to modeling based on the crystallographic model of the 4-layer TMV CP aggregate (PDB: 1EI7), the stacked disks represented hollow cylinders. The calculated SAXS pattern for the disks was compared to the experimental one over the entire measured range. The best correlation with the SAXS data was found for the model with the repeating central pair of discs; the SAXS curves for the stacked disks were virtually identical irrespectively of the protein isolation method. The positions of maxima on the scatter curves could be used as characteristic features of the studied samples; some of the peaks were assigned to the existing elements of the quaternary structure (periodicity of aggregate structure, virion helix pitch). Low-resolution structural data for the repolymerized TMV CP aggregates in solution under conditions similar to natural were produced for the first time. Analysis of such nano-size objects is essential for their application in biomedicine and biotechnology.

Coupling in vitro cell culture with synchrotron SAXS to understand the bio-interaction of lipid-based liquid crystalline nanoparticles with vascular endothelial cells.

Nonlamellar lipid-based liquid crystalline (LLC) nanoparticles possessing different internal nanostructures, specifically the 3D-ordered cubosomes (V2 phase) and the 2D-ordered hexosomes (H2 phase), are of increasing interest as drug delivery systems. To facilitate their development, it is important that we understand their interactions with healthy human umbilical vein endothelial cells (HUVECs). To this end, a 3D cells-in-a-tube model that recapitulates the basic morphology (i.e. tubular lumen) and in vivo microenvironment (i.e. physiological shear stress) of blood vessels was employed as a biomimetic testing platform, and the bio-nanoparticle interactions were compared with that of the conventional 2D planar cell culture. Confocal microscopy imaging revealed internalisation of the nanoparticles into HUVECs within 2h and that the nanoparticle-cell interactions of cubosomes and hexosomes were not significantly different from one another. Low fluid shear stress conditions (i.e. venous simulation at 0.8 dynes/cm2) were shown to impose subtle effects on the degree of nanoparticle-cell interactions as compared with the static 2D culture. The unexpected similarity of cellular interactions between cubosomes and hexosomes was clarified via a real-time phase behaviour analysis using the synchrotron-based small-angle X-ray scattering (SAXS) technique. When the nanoparticles came into contact with HUVECs under circulating conditions, the cubosomes gradually evolved into hexosomes (within 16min). In contrast, the hexosomes retained their original internal structure with minimal changes to the lattice parameters. This study highlights the need to couple cellular studies with high-resolution analytics such as time-resolved SAXS analysis to ensure that particle structures are verified in situ, enabling accurate interpretation of the dynamics of cellular interactions and potential bio-induced changes of particles intended for biomedical applications. Graphical abstract.

Annealing of ion tracks in apatite under pressure characterized in situ by small angle x-ray scattering

Fission track thermochronology is routinely used to investigate the thermal history of sedimentary basins, as well as tectonic uplift and denudation rates. While the effect of temperature on fission track annealing has been studied extensively to calibrate the application of the technique, the effect of pressure during annealing is generally considered to be negligible. However, a previous study suggested elevated pressure results in a significantly different annealing behaviour that was previously unknown. Here, we present a method to study track annealing in situ under high pressure by using synchrotron-based small angle x-ray scattering (SAXS). To simulate fission tracks in a controlled environment, ion tracks were created in apatite from Durango, Mexico using 2 GeV Au or Bi ions provided by an ion accelerator facility. Samples were annealed at 250 °C at approximately 1 GPa pressure using diamond anvil cells (DACs) with heating capabilities. Additional in situ annealing experiments at ambient pressure and temperatures between 320 and 390 °C were performed for comparison. At elevated pressure a significantly accelerated annealing rate of the tracks was observed compared with annealing at ambient pressure. However, when extrapolated to geologically relevant temperatures and pressures, the effects become very small. The measurement methodology presented provides a new avenue to study materials behaviour in extreme environments.

Mechanism of silica-lysozyme composite formation unravelled by in situ fast SAXS.

A quantitative understanding of aggregation mechanisms leading to the formation of composites of inorganic nanoparticles (NPs) and proteins in aqueous media is of paramount interest for colloid chemistry. In particular, the interactions between silica (SiO2) NPs and lysozyme (LZM) have attracted attention, because LZM is well-known to adsorb strongly to silica NPs, while at the same time preserving its enzymatic activity. The inherent nature of the aggregation processes leading to NP–LZM composites involves structural changes at length scales from few to at least hundreds of nanometres but also time scales much smaller than one second. To unravel these we used in situ synchrotron-based small-angle X-ray scattering (SAXS) and followed the subtle interparticle interactions in solution at a time resolution of 50 ms/frame (20 fps). We show that if the size of silica NPs (ca. 5 nm diameter) is matched by the dimensions of LZM, the evolving scattering patterns contain a unique structure-factor contribution originating from the presence of LZM. We developed a scattering model and applied it to analyse this structure function, which allowed us to extract structural information on the deformation of lysozyme molecules during aggregation, as well as to derive the mechanisms of composite formation.

Transformation of engineered nanomaterials through the prism of silver sulfidation.

Understanding the structure transformation of engineered nanomaterials (ENMs) is a grand measurement challenge, which impacts many aspects of ENMs applications, such as their efficacy, safety, and environmental consequence. To address the significant knowledge gap regarding the fundamental kinetic rate and extent of ENM transformation in the environment, we present a comprehensive and mechanistic structural investigation of the transformation, aggregation, and dissolution behavior of a polyvinylpyrrolidone-coated silver nanoparticle (AgNP) suspension upon sulfidation in moderately reduced hard water with fulvic acid and dissolved Na2S. This reaction is among the most prevalent and industrially and environmentally relevant ENMs transformation. Using ex situ transmission electron microscopy (TEM) and both in situ and ex situ synchrotron-based small angle X-ray scattering (SAXS) and X-ray diffraction (XRD), we find that sulfidation of faceted AgNPs strongly depends on the crystallographic orientation of the facets, with nanometer-scale passivation layers developed on {111} and {100} facets and continuous nucleation and growth on {110} facets. Nanobeam electron diffraction and atomic resolution imaging show Ag and Ag2S domains both possess a high degree of crystalline order, contradicting amorphous structures as previously reported. In situ SAXS/XRD allowed simultaneous determination of the morphological changes and extent of sulfidation of AgNPs. SAXS/XRD results strongly indicate sulfidation follows first-order reaction kinetics without any aggregation. Aided by their size monodispersity, for the first time, using direct, in situ morphology and atomic-structure probes whose results mutually corroborate, we unequivocally determined the sulfidation rate constant of AgNPs under an environmentally relevant condition (≈0.013 min−1 for 68 nm diameter AgNPs). A rigorous analysis of the long-term sulfidation product of the AgNPs under different S/Ag ratios using ex situ SAXS/XRD clearly demonstrates that the silver mass in the original AgNP and transformed Ag/Ag2S NP is preserved. This result has important environmental implications, strongly suggesting that Ag+ ions, a known highly effective antimicrobial agent, are not leached into the solution during sulfidation of AgNPs. The combined nondestructive methodology can be extended to unfold the structure transformation pathway and kinetics in a broad range of ENM systems.

A guide to high-efficiency chromium (III)-collagen cross-linking: Synchrotron SAXS and DSC study

The inefficiency of the chromium (III)-collagen cross-linking reaction during conventional leather processing results in severe environmental pollution from the waste chromium in the effluent. A mechanistic study using synchrotron-based small-angle X-ray scattering (SAXS) and differential scanning calorimetry (DSC) on ThruBlu tanned leather, revealed the effect of chromium sulphate and its pre-treatments on collagen structure and stability. By pre-treating with complexing agents such as sodium formate and disodium phthalate, as well as nanoclay (sodium montmorillonite), the uniformity through bovine hide collagen matrix were improved significantly. These pre-treatments effectively reduce the reactivity of chromium during its cross-linking reaction with collagen while retaining its bound water. However, collagen pre-treated with a covalent cross-linker (glutaraldehyde) results in a decrease in both chromium-collagen cross-linking and bound water while improving uniformity. These molecular-level insights can be developed into metrics to guide us towards a more sustainable future for the leather industry.

Nanostructure of electrospun collagen: Do electrospun collagen fibers form native structures?

Collagen extracts can be electrospun to form fibers. The nanoscale structure of these fibers is not known but is expected to affect the biocompatibility of the spun materials. Collagen extracts from Macruronus novaezelandiae (hoki) skin were electrospun to form a fibrous material. The structure of the electrospun collagen fibers was analyzed and compared with the structure of native collagen, gelatin, and electrospun gelatin. Attenuated Total Reflectance Fourier Transform Infrared spectroscopy (ATR-FTIR) and SDS-PAGE were used to characterize the basic molecular structure of the biomaterials and synchrotron-based small-angle X-ray scattering (SAXS) and Transmission electron microscope (TEM) were used to investigate the fibril nanoscale structure (molecular arrangement). ATR-FTIR and SDS-PAGE revealed characteristic patterns of intact alpha chains in the electrospun collagen and hydrolyzed fragments in electrospun gelatin, as expected. TEM revealed fibers in both the native collagen material and the electrospun samples. However, SAXS patterns showed axial periodicity was not present in the electrospun fibers. This is indicative of the spinning process forming fibers that lack internal fibril structure, in contrast to the hierarchical structure of native collagen. The architecture of collagen affects its function. By characterizing the molecular and fibril structure of electrospun collagen and comparing it with native collagen fibrils, we may inform functional studies of collagen, including its configuration for cell attachment and recognition.

Analysis of textural properties of CaO-based CO2 sorbents by ex situ USAXS

In this work, the micro-textural properties of CaO-based CO2 sorbents prepared in a thermo-gravimetric reactor were investigated by ex situ synchrotron-based Small Angle X-ray Scattering (SAXS), Ultra Small Angle X-ray Scattering (USAXS) and Wide Angle X-ray Scattering (WAXS). Six sorbent samples were produced by calcination in vacuum at different temperatures and durations of the heating step; additionally, four partially carbonated samples were produced, after calcination in vacuum, at different CaO conversions. The scattering intensity profiles were analyzed by means of the Unified Fit model. Bimodal pore size distributions (micro-pores and meso-pores) were identified and the micro-textural properties (porosity, specific surface and pore radius of gyration) of each of the two pore populations were quantified both for the calcined and for the carbonated samples. The micro-textural properties of a few calcined samples were compared with N2-adsorption measurements. For each pore population, the trends of porosity, specific surface and pore radius of gyration, in addition to the pore number density and sphericity factor, were obtained versus time during the calcination and versus the CaO conversion during the carbonation. The relevance of micro-pores with respect to macro-pores was assessed both as far as the porosity impact on the CO2 capture capacity and as far as the specific surface impact on the carbonation kinetics. For the calcined samples, the micro-textural properties of a partially calcined sample were compared with those of the completely calcined samples, and pore correlation distances were determined. For the carbonated samples, the specific surface per unit of particle volume results linearly dependent on the CaO conversion and, if expressed per unit of mass of unreacted CaO, does not change significantly for most of the CaO carbonation.

Tuning Precursor Reactivity toward Nanometer-Size Control in Palladium Nanoparticles Studied by in Situ Small Angle X-ray Scattering

Synthesis of monodisperse nanoparticles (NPs) with precisely controlled size is critical for understanding their size-dependent properties. Although significant synthetic developments have been achieved, it is still challenging to synthesize well-defined NPs in a predictive way due to a lack of in-depth mechanistic understanding of reaction kinetics. Here we use synchrotron-based small-angle X-ray scattering (SAXS) to monitor in situ the formation of palladium (Pd) NPs through thermal decomposition of Pd–TOP (TOP: trioctylphosphine) complex via the “heat-up” method. We systematically study the effects of different ligands, including oleylamine, TOP, and oleic acid, on the formation kinetics of Pd NPs. Through quantitative analysis of the real-time SAXS data, we are able to obtain a detailed picture of the size, size distribution, and concentration of Pd NPs during the syntheses, and these results show that different ligands strongly affect the precursor reactivity. We find that oleylamine does not change the reactivity of the Pd–TOP complex but promote the formation of nuclei due to strong ligand–NP binding. On the other hand, TOP and oleic acid substantially change the precursor reactivity over more than an order of magnitude, which controls the nucleation kinetics and determines the final particle size. A theoretical model is used to demonstrate that the nucleation and growth kinetics are dependent on both precursor reactivity and ligand–NP binding affinity, thus providing a framework to explain the synthesis process and the effect of the reaction conditions. Quantitative understanding of the impacts of different ligands enables the successful synthesis of a series of monodisperse Pd NPs in the broad size range from 3 to 11 nm with nanometer-size control, which serve as a model system to study their size-dependent catalytic properties. The in situ SAXS probing can be readily extended to other functional NPs to greatly advance their synthetic design.

Riddle of the Nautilus: Specific Structural Features of Its Shell

The shells of the chambered nautilus (Nautilus pompilius) are studied by X-ray structure analysis (XRD) and electron microscopy (SEM and TEM). The shell structure is examined in a nanometer scale using XRD and synchrotron-based small angle X-ray scattering (SAXS). The mineral composition of shells includes 98–99 wt % aragonite, ~1 wt % organic substance (conchiolin), 1 wt % strontianite, and 0.5 wt % calcite. Trace elements comprise Na, Mg, Al, K, Si, Fe, P, S, Zn, Sr, Ba, and Cl. The laminated layers are composed of aragonite crystals with a width of 5–10 μm and a thickness of 0.5–1 μm; the prismatic layers, with a length of 7–12 μm long and a width of 1–3 μm. According to XRD and SAXS assays, the aragonite layers are formed of flawless monocrystals lacking any internal structuring. The shell conchiolin is a polymer formed of a system of parallel fibers folded with a step of approximately 100 nm without longitudinal structuring. Presumably, the unique structure of the nautilus shells has determined the existence of Nautiloidea over 500 Ma and their preservation as fossils for over 100 Ma.

Real-Time Synchrotron Small-Angle X-ray Scattering Studies of Collagen Structure during Leather Processing

The collagen structure in skins is significantly influenced by the cross-linking chemistry adopted during leather processing. We have developed an in situ technique to measure real-time collagen structure changes using synchrotron-based small-angle X-ray scattering (SAXS). Three common mineral tanning systems, basic chromium sulfate (BCS), zirconium sulfate (ZIR) and an aluminosilicate-based reagent (ALS) were used to stabilize collagen in ovine skin. Studying the molecular changes by in situ SAXS revealed a range of tanning mechanisms: a complex combination of covalent cross-linking, electrostatic interactions and hydrogen bonding by BCS, hydrogen bonding interactions by ZIR, and the formation of colloidal aggregates by ALS. These results unravel the mechanisms of producing leathers with different properties, explaining why ZIR produces denser leathers while ALS produces softer leathers compared to conventional BCS leathers. ZIR and ALS are environment-friendly alternatives to BCS, and understanding their mechanisms is important for a more sustainable future for the leather industry.

Conical etched ion tracks in SiO2 characterised by small angle X-ray scattering

Abstract We present a systematic study of the evolution of chemically etched ion tracks formed in thermally grown a-SiO2 after irradiation with 1.1 GeV and 185 MeV Au ions. The irradiated material was subsequently etched with 2.5% hydrofluoric acid (HF) for different times yielding hollow conical shaped structures of various sizes. The characterisation of these structures was carried out by synchrotron-based small-angle X-ray scattering (SAXS) measurements, enabling the determination of the geometry and dimensions of the etched conical structures with sub-nanometre precision. The results indicate that the track etching behavior is influenced by the ion energy, and that at short etching times the latent track damage in the radial direction becomes significant.

Deer leather: analysis of the microstructure affecting pebble.

Deer leather has a characteristic pattern, referred to as 'pebble', which is accorded such importance that a lack of it renders a leather defective. Synchrotron-based small-angle X-ray scattering (SAXS), ultrasonic imaging, scanning electron microscopy, and tear tests were used to investigate the structural characteristics of well-pebbled and poorly pebbled cervine leathers. Poorly pebbled leather has a less open structure in the upper grain region than well-pebbled leather. The orientation index (OI) of leather with a poor pebble is less than that of the well-pebbled leather, particularly in the corium. The tear strength is also less for the poorly pebbled leather. The differences in structure between well- and poorly pebbled cervine leathers are not the same as the structural differences between tight and loose bovine leathers, to which they are sometimes compared. On the contrary, good pebble may reflect an internal structure similar to that of looseness. It is hoped that methods to prevent a reduction in pebbling during the processing of cervine leather may be developed by applying this knowledge of cervine leather's structural characteristics. © 2017 Society of Chemical Industry.