High-resolution X-ray Research Articles

Molecular structure and evolution mechanism of shale kerogen: Insights from thermal simulation and spectroscopic analysis

During thermal evolution, the kerogen in shale formation undergoes significant chemical, structural and compositional changes, continuously influencing the shale storage capacity, hydrocarbon generation potential, and gas occurrence state. This study systematically examines the chemical structural changes during the thermal evolution of Longmaxi shale kerogen using hydrothermal laboratory experiments from 420 to 850 °C. Additionally, a range of characterization techniques, including Fourier Transform Infrared (FTIR) spectroscopy, Raman spectroscopy, High-Resolution Transmission Electron Microscopy (HRTEM), X-ray Diffraction (XRD), and Solid-state 13C Nuclear Magnetic Resonance (13C NMR), were employed to systematically investigate the kerogen structure and its evolution patterns. Results indicate that Longmaxi Formation kerogen comprises a large molecular carbon framework with aromatic structures, long-chain aliphatic components, and oxygen-containing functional groups. As thermal maturity reaches 2.6 %, the alignment of aromatic fringes gradually increased, with over 60 % aligning in the main direction. Throughout thermal evolution (1.9–3.2 %), fringes in the 5–10 Å range within aromatic structures peak at over 20.45 %, with fringes over 50 Å rapidly increasing from 3 % to over 15 %. Early in the thermal evolution, the long-chain aliphatic component of the kerogen decreases rapidly and part of the structure forms small aromatic rings through aromatisation. The mature to over-mature stage can be divided into three phases: 1) 1.7–2.4 % (loss of oxygen-containing functional groups), 2) 2.4–3.5 % (formation of larger aromatic structures via condensation reactions), 3) over 3.5 % (continued aggregation of aromatic rings, resulting in an increase in the length of aromatic fringes). At a macroscopic level, this induces changes in kerogen pore structure and carbonization features. This study thus provides new insights into the thermal evolution of shale kerogen, which in turn improve understanding of shale reservoirs for hydrocarbon exploitation.

High-Resolution Imaging and X-Ray Microanalysis of Oxide at Low Energy using Scanning Electron Microscope and Triple Beam FIB Microscope

High-Resolution Imaging and X-Ray Microanalysis of Oxide at Low Energy using Scanning Electron Microscope and Triple Beam FIB Microscope

Effect of temperature on the stability and performance of III-nitride HEMT magnetic field sensors

The study aimed to investigate the underlying physics limiting the temperature stability and performance of non-surface passivated Al0.34Ga0.66N/GaN Hall effect sensors, including contacts, under atmospheric conditions. The results obtained from analyzing the microstructural evolution in the Al0.34Ga0.66N/GaN Hall sensor heterostructure were found to correlate with the electrical performance of the Hall effect sensor. High-resolution x-ray photoelectron spectroscopy studies revealed the signature of surface oxidation in the GaN cap layer, as well as a slight out-diffusion of “Al” from the AlGaN barrier layer. To prevent the formation of a bumpy surface morphology at the Ohmic contact, we investigated the impact of “Pt” top Ohmic contacts. The application of a top “Pt” contact stack resulted in a smooth Ohmic contact surface and provided evidence that the bumpy surface morphology in Au-based Ohmic contacts is due to the formation of an Al-Au viscous alloy during rapid thermal annealing. In the early stages of thermal aging, the small drop in contact resistivity stabilized with subsequent thermal aging past the initial 550 h at 200 °C. The outcome is that the Al0.34Ga0.66N/GaN Hall effect sensors, even without surface passivation, exhibited a stable response to applied magnetic fields with no sign of significant degradation after 2800 h of thermal aging at 200 °C under atmospheric conditions. This observed stability in the Hall sensor without surface passivation can be attributed to a self-imposed surface oxidation of the cap layer during the early stages of aging, which serves as a protective layer for the device during subsequent extended periods of thermal aging at 200 °C.

Tunable charge transport properties in non-stoichiometric SrIrO3 thin films

Delving into the intricate interplay between spin-orbit coupling and Coulomb correlations in strongly correlated oxides, particularly perovskite compounds, has unveiled a rich landscape of exotic phenomena ranging from unconventional superconductivity to the emergence of topological phases. In this study, we have employed pulsed laser deposition technique to grow SrIrO3 (SIO) thin films on SrTiO3 substrates, systematically varying the oxygen content during the post-deposition annealing. X-ray photoelectron spectroscopy (XPS) provided insights into the stoichiometry and spin-orbit splitting energy of Iridium within the SIO film, while high-resolution x-ray studies meticulously examined the structural integrity of the thin films. Remarkably, our findings indicate a decrease in the metallicity of SIO thin films with reduced annealing O2 partial pressure. Furthermore, we carried out magneto-transport studies on the SIO thin films, the results revealed intriguing insights into spin transport as a function of oxygen content. The tunability of the electronic band structure of SIO films with varying oxygen vacancy is correlated with the density functional theory calculations. Our findings elucidate the intricate mechanisms dictating spin transport properties in SIO thin films, offering invaluable guidance for the design and optimization of spintronic devices based on complex oxide materials. Notably, the ability to tune bandwidth by varying post-annealing oxygen partial pressure in iridate-based spintronic materials holds significant promise for advancing technological applications in the spintronics domain.

Unraveling iron oxides as abiotic catalysts of organic phosphorus recycling in soil and sediment matrices

In biogeochemical phosphorus cycling, iron oxide minerals are acknowledged as strong adsorbents of inorganic and organic phosphorus. Dephosphorylation of organic phosphorus is attributed only to biological processes, but iron oxides could also catalyze this reaction. Evidence of this abiotic catalysis has relied on monitoring products in solution, thereby ignoring iron oxides as both catalysts and adsorbents. Here we apply high-resolution mass spectrometry and X-ray absorption spectroscopy to characterize dissolved and particulate phosphorus species, respectively. In soil and sediment samples reacted with ribonucleotides, we uncover the abiotic production of particulate inorganic phosphate associated specifically with iron oxides. Reactions of various organic phosphorus compounds with the different minerals identified in the environmental samples reveal up to twenty-fold greater catalytic reactivities with iron oxides than with silicate and aluminosilicate minerals. Importantly, accounting for inorganic phosphate both in solution and mineral-bound, the dephosphorylation rates of iron oxides were within reported enzymatic rates in soils. Our findings thus imply a missing abiotic axiom for organic phosphorus mineralization in phosphorus cycling.

Enhancement of superconductivity and structural phase transitions under pressure in FeTe0.89S0.11

The ternary iron chalcogenide, FeTe0.89S0.11 is a prominent member of the family of Fe-based superconductors with an ambient pressure Tc of around 8 K and a simple structure formed by layers of edge-sharing distorted tetrahedra separated by a van der Waals gap. Upon compression to 6 GPa, the Tc increases monotonically to 11 K. The superconductivity disappeared at about 6 GPa which was correlated to a softening of a Raman mode. High-resolution synchrotron X-ray diffraction shows that the FeTe0.89S0.11 started to transform from the monoclinic phase described by space group Cm to a disordered triclinic phase described by space group P1 at around 10 GPa (theoretical) - 14 GPa (experimental). Due to the phase transition the studied material transforms from a layered compound to a polymer, which is accompanied by a volume collapse of 4.65 %, indicating a discontinuous first-order phase transition. The disappearance of Raman modes, along with pressure independent resistivity, and ab initio calculations results support the structural and electronics phase transition. According to our results Fe(Te,S) may be useful for future high-field power applications being formed of relatively inexpensive and nontoxic elements.

Synchrotron-based x-ray diffraction analysis of energetic ion-induced strain in GaAs and 4H-SiC

Strain engineering using ion beams is a current topic of research interest in semiconductor materials. Synchrotron-based high-resolution x-ray diffraction has been utilized for strain-depth analysis in GaAs irradiated with 300 keV Ar and 4H-SiC and GaAs irradiated with 100 MeV Ag ions. The direct displacement-related defect formation, anticipated from the elastic energy loss of Ar ions, can well explain the irradiation-induced strain depth profiles. The maximum strain in GaAs is evaluated to be 0.88% after Ar irradiation. The unique energy loss depth profile of 100 MeV Ag (swift heavy ions; SHIs) and resistance of pristine 4H-SiC and GaAs to form amorphous/highly disordered ion tracks by ionization energy loss of monatomic ions allow us to examine strain buildup due to the concentrated displacement damage by the elastic energy loss near the end of ion range (∼12 μm). Interestingly, for the case of SHIs, the strain-depth evolution requires consideration of recovery by ionization energy loss component in addition to the elastic displacement damage. For GaAs, strain builds up throughout the ion range, and the maximum strain increases and then saturates at 0.37% above an ion fluence of 3×1013 Ag/cm2. For 4H-SiC, the maximum strain reaches 4.6% and then starts to recover for fluences above 1×1013 Ag/cm2. Finally, the contribution of irradiation defects and the purely mechanical contribution to the total strain have been considered to understand the response of different compounds to ion irradiation.

Effects of Fe substitution for Mn on structural, magnetic and magnetocaloric properties of TbMn2-xFexSi2

The structural and magnetic properties of TbMn2-xFexSi2 compounds (x = 0.0–0.4) have been investigated in details by high-resolution synchrotron x-ray and neutron powder diffraction, specific heat, and dc magnetization measurements. The replacement of Fe for Mn in TbMn2-xFexSi2 does not change the crystal structure but leads to a significant contraction of the unit cell (dV/dx ∼ - 6 Å3) and modification of three magnetic phase transition temperatures – the Curie temperatures Tc1, Tc2 and the Néel temperature TN. For example, the Tc1, Tc2 and TN values of TbMn2Si2 decrease from Tc1 = 50 K, Tc2 = 64 K and TN = 500 K to Tc1 = 27 K, Tc2 = 37 K and TN = 440 K for TbMn1.6Fe0.4Si2. Detailed neutron diffraction investigations have allowed us to determine the magnetic structures and construct the magnetic phase diagram as well as confirm the presence of magnetoelastic coupling effects. The significantly different responses of Tc1 and Tc2 to applied magnetic fields (e.g. dTc1/dB = 0.52 K/T and dTc2/dB = 4.7 K/T for TbMn1.6Fe0.4Si2), leads to expansion of the temperature region (ΔT = Tc2- Tc1) for the canted ferromagnetic state Fmc-ii between Tc1 and Tc2. In the case of TbMn1.6Fe0.4Si2, ΔT increases from ΔT = 9 K for applied magnetic field B = 0.2 T to ΔT = 36 K for B = 6 T, resulting in plateau-like behaviour of magnetic entropy change and enhances the relative cooling power (RCP) in this system. Under a change of magnetic field of 0 T – 5 T, the maximum value of the magnetic entropy changes -ΔSmax and adiabatic temperature change, ΔTad are derived to be -ΔSmax = 13.1 J/kg K and ΔTad = 8.4 K with the RCP = 411 J/kg for x=0.4 sample. The plateau-like magnetocaloric effect and relatively large RCP make these materials potentially suitable for application in cryogenic magnetic refrigeration.

Predicting ecology and hearing sensitivities in Parapontoporia-An extinct long-snouted dolphin.

Analyses of the cetacean (whale and dolphin) inner ear provide glimpses into the ecology and evolution of extinct and extant groups. The paleoecology of the long-snouted odontocete (toothed whale) group, Parapontoporia, is primarily marine with its depositional context also suggesting freshwater tolerance. As an extinct relative of the exclusively riverine Lipotes vexillifer, Parapontoporia provides insight into a transition from marine to freshwater environments. High-resolution X-ray CT scans (~3 microns or less) of three individual specimens from two species, P. sternbergi and P. pacifica, were acquired. Digital endocasts of the inner ear labyrinths were extracted non-destructively. Nine measurements of the inner ear were compared with an existing dataset covering 125 terrestrial and aquatic artiodactyls. These measurements were then subjected to a principal component analysis to interpret hearing sensitivities among other artiodactyls. Based on our analyses, Parapontoporia was likely to have been able to hear within narrow-band high frequency (NBHF) ranges. This finding indicates another convergence of NBHF-style hearing, or, more intriguingly, suggests that it may be an ancestral characteristic present among the longirostrine dolphins that dominated in the Miocene prior to the evolution of more modern lineages.

Mitigation of Parasitic and Drift Capacitance-Induced Nonlinear Current Responses for Stable and Sensitive Perovskite X-ray Detectors.

The development of perovskite direct X-ray detectors shows potential for advancing medical imaging and industrial inspection precision. To ensure the optimal energy conversion efficiency of X-rays for reducing radiation doses, it is necessary for perovskites with thicknesses reaching hundreds of micrometers or even several millimeters to be utilized. However, the nonlinear current response becomes uncertain with such high thicknesses. For instance, the prevailing theory regarding the rapid trapping and release of charges by shallow-level defects falls short in explaining the nonlinear current response observed in high-quality single-crystal samples. Moreover, a significant nonlinear current response can degrade the detection performance. Here, we elucidate peculiar parasitic and drift capacitance-induced nonlinear current responses in perovskites, which arise from bulk structural deficiencies and interface junction width variation in addition to shallow-level defects. Both theoretical analysis and experimental findings demonstrate the effective suppression of nonlinear current responses by establishing bulk heterojunctions and refining interface junctions. Consequently, we have successfully developed highly linear current-responsive detectors based on polycrystalline MAPbI3 thick films. Notably, these detectors achieve a record sensitivity of 2.3 × 104 μC·Gyair-1·cm-2 under 100 kVp X-ray irradiation with a low bias of 0.1 V/μm, enabling enduring and high-resolution X-ray imaging for high-density objects. Successful fabrication and testing of a 64 × 64-pixel flat-panel prototype detector affirm the widespread applicability of these strategies in rectifying nonlinear current responses in perovskite-based X-ray detectors.

Low loss ridge waveguides on the hybrid single crystalline silicon and lithium niobate thin films

The hybridization of silicon (Si) thin film and lithium niobate (LN) thin film with remarkable properties, including the excellent optical properties of LN, excellent electrical properties and mature processing advantages of Si, can provide an important material platform for integrated photonic applications. In this work, a 4-inch single crystalline Si thin film wafer was prepared using wafer bonding, grinding and polishing techniques on LN thin film substrate. The films were characterized by using high-resolution transmission electron microscopy (HRTEM). The interplanar spacings and strain of Si film were calculated by analysis of high-resolution X-ray diffraction (HRXRD). Si ridge straight waveguides were fabricated on the hybrid thin films, and the transmission loss was 1.2 dB/cm. The near-field mode distribution of the waveguide was investigated by combining FDTD (Finite-Difference Time-Domain) simulation and end coupling measurement.

Low contact resistance and high breakdown voltage of AlGaN/GaN HEMT grown on silicon using both AlN/GaN superlattice and Al0.07Ga0.93N back barrier layer

In this study, the growth of a high-quality AlGaN/GaN high electron mobility transistor (HEMT) heterostructure on silicon (Si) by metal–organic chemical vapor deposition was investigated by utilizing both the AlN/GaN superlattice (SL) and Al0.07Ga0.93N back barrier (BB) techniques. An atomic force microscope and high-resolution x-ray diffractometer confirm a low surface roughness of 0.26–0.34 nm and the formation of a high-quality AlN/GaN SL and GaN channel. The AlGaN/GaN heterostructures exhibit a high electron mobility of up to 1700 cm2 V−1∙s and a high carrier concentration density of (1.02–1.06 × 1013 cm−2) for both heterostructures. The AlGaN/GaN HEMT devices demonstrate a low specific contact resistivity (ρ c) of 2.7 × 10−6 Ω·cm2 and a low contact resistance (RC ) of 0.3 Ω·mm for the heterostructure with a BB layer. Furthermore, the DC characteristics demonstrate that incorporating Al0.07Ga0.93N BB in the heterostructure results in a 19.2% increase in lateral breakdown voltage (with a 10 µm spacing) and a 27.5% increase in vertical breakdown voltage (at 1 mA cm−2) compared to heterostructures without Al0.07Ga0.93N BB within the AlN/GaN SL structure. Moreover, an improvement of 10.6% in the maximum saturation current (I DS) and 15.2% in on-resistance (R ON) has been achieved for the device fabricated on an Al0.07Ga0.93N BB structure. The insertion loss of the buffer layer improves to −1.40 dB mm−1 at 40 GHz. Consequently, the proposed heterostructure investigated in this study demonstrates suitability for electronic device applications.

Solution processed high aspect ratio ultra-long vertically well-aligned ZnO nano scintillators for potential X-ray imaging applications

We report the photon (PL), electron (CL) and X-ray (XEL) induced luminescence characteristics of high aspect ratio ultra-long (~ 50 µm) ZnO nanorods (NRs) and discuss the potential for fast X-ray detection based on the consistent and efficient visible emission (~ 580 nm) from ZnO NRs. Nanostructured ZnO scintillators were rearranged to form a vertically well-aligned NR design in order to help light absorption and coupling resulting in luminescent and fast scintillation properties. The design of the nanorod array combines the key advantages of a low-cost growth technique together with environmentally friendly and widely available materials. A low temperature hydrothermal method was adopted to grow ZnO NRs in one cycle growth and their structural, optical and X-ray scintillation properties were investigated. The relatively short (~ 10 µm) ZnO NRs emitting in the near-band-edge region were found to be almost insensitive to X-rays. On the other hand, the higher XEL response of long ZnO NRs, which is a key parameter for evaluation of materials to be used as scintillators for high quality X-ray detection and imaging, along with a decay time response in the order of ns confirmed promising scintillation properties for fast and high-resolution X-ray detector applications.

Actinyl Electronic Structure Probed by XAS: The Role of Many-Body Effects.

A detailed analysis of the wave functions for the M5 to 5f excitations in the linear actinyls, UO22+, NpO22+, and PuO22+, and the theoretical X-ray absorption spectra obtained with these wave functions in comparison with experimental M5-edge high-resolution X-ray absorption near-edge structure (HR-XANES) spectra is presented. The wave functions include full treatment of scalar and spin-orbit relativistic effects through the use of a Dirac-Coulomb Hamiltonian; many-body effects are included in determining the wave functions. The character of the excited states and of the active spaces to describe the wave functions for these states are investigated and analyzed. It is shown that the excited states cannot, in general, be described with a single configuration but have an essential multiconfiguration character. The characterization of the properties of the excited states and the X-ray absorption spectra was achieved through the use of novel methods.

Imaging flow focusing and isolation of aqueous fluids in synthetic quartzite: implications for permeability and retained fluid fraction in deep-seated rocks

The microstructure of realistic fluid–rock systems evolves to minimize the overall interfacial energy, enabling local variations in fluid geometry beyond ideal models. Consequently, the permeability–porosity relationship and fluid distribution in these systems may deviate from theoretical expectations. Here, we aimed to better understand the permeability development and fluid retention in deep-seated rocks at low fluid fractions by using a combined approach of high-resolution synchrotron radiation X-ray computed microtomography imaging of synthesized rocks and numerical permeability computation. We first synthesized quartzite using a piston-cylinder apparatus at different fluid fractions and wetting properties (wetting and non-wetting systems with dihedral angles of 52° and 61°–71°, respectively) under conditions of efficient grain growth. Although all fluids should be connected along grain edges and tubules in the homogeneous isotropic wetting fluid–rock system enabling segregation by gravitational compaction in natural settings, the fluid connectivity rapidly decreased to ~ 0 when the total fluid fraction decreased to 0.030–0.037, as the non-ideality of quartzite, including the interfacial energy anisotropy (i.e., grain faceting), became critical. In non-wetting systems, where the minimum energy fluid fraction based solely on the dihedral angle is ~ 0.015–0.035, the isolated (disconnected) fractions was 0.048–0.062. A streamline computation in the non-wetting system revealed that with decreasing total porosity, flow focusing into fewer channels maintained permeability, allowing the effective segregation of the connected fluids. These results provide insight into how non-wetting fluids segregate from rocks and exemplify the fraction of retained fluids in non-wetting systems. Thus, the findings suggest a potential way for wetting system fluids to be transported into the deep Earth's interior, and the amount of fluids dragged down to the Earth’s interior could be higher than what was previously estimated.

Multi-scale structural characterization of ceramic-based photonic glasses for structural colors

Structural colors arise from selective light interaction with (nano)structures, which give them advantages over pigmented colors such as resistance to fading and possibility to be fabricated out of traditional low-cost and non-toxic materials. Since the color arises from the photonic (nano)structures, different structural features can impact their photonic response and thus, their color. Therefore, the detailed characterization of their structural features is crucial for further improvement of structural colors. In this work, we present a detailed multi-scale structural characterization of ceramic-based photonic glasses by using a combination of high-resolution ptychographic X-ray computed tomography and small angle X-ray scattering. Our results uncover the structure-processing-properties’ relationships of such nanoparticles-based photonic glasses and point out to the need of a review of the structural features used in simulation models concomitantly with the need for further investigations by experimentalists, where we point out exactly which structural features need to be improved.

Continuous damage of concrete structures due to reinforcement corrosion: A micromechanical and multi-physics based analysis

Deterioration of concrete and composite structures due to the corrosion of embedded steel components (rebar, structural steel components, and steel fiber, etc.) is a self-accelerating process involving multiple chemophysical processes that occur concurrently in the heterogeneous structure of concrete. The multiple-inclusion matrix of concrete and the multi-chemophysics nature of steel corrosion synergistically challenge an accurate analysis and evaluation of the deterioration process using homogeneity-based continuum mechanics. This study presents a three-dimensional micromechanical model developed for quantifying the continuous deterioration of concrete by steel corrosion. Continuous damage theory of solid-state materials was applied to a steel-concrete sample that consists of mortar, aggregate, and steel phases as were reconstructed from high-resolution X-ray CT images. With due consideration of the variations in environmental temperature and moisture, the complex chemophysical processes involved in corrosion-induced deterioration of concrete were solved concurrently using finite element analysis. Results of the study indicate that capillary suction in a variably saturated concrete plays an important role in steel corrosion and that removal of chloride by an externally applied electrical field can effectively mitigate steel corrosion and the incurred concrete deterioration.

A luminescent metal–organic framework composite as a turn-on sensor for the selective determination of monosodium glutamate in instant noodles

This work reports the development and application of a new fluorescent nanoprobe sensor depending on using luminescent metal organic framework (LMOF). The developed sensor composed of hybridized Ca 1,3,5-benzenetricarboxylic acid metal organic framework with microcrystalline cellulose (Ca-BTC/MCC MOF) as a fluorescent probe for the determination of the monosodium glutamate (MSG), a non-chromophoric food additive. The developed sensor was characterized using a high-resolution scanning electron microscope (HR-SEM), X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FTIR). The Ca-BTC/MCC MOF hybrid, examined under the HR-SEM, showed morphological features different from the MCC and the Ca-BTC MOF. The diffraction patterns of Ca-BTC/MCC composites clearly displayed the characteristic Ca-BTC MOF diffraction bands, indicating that MCC was successfully incorporated in the formation of crystalline MOF hybrids. The FTIR spectra show the bands of MCC, as well as the bands of Ca-BTC MOFs. The prepared nanoprobe was successfully applied as a sensitive sensor for the determination of MSG in food sample. The method was validated following the International ICH (Q2)R2 guidelines in terms of precision, trueness and other main analytical figures of merit, comprised the green profile and practicability metrics. A wide linearity range was achieved (5–50 µg/mL) with good correlation coefficient (R2 ≥ 0.9993). The recoveries (%) were found in the range of 100.0 to 101.5 and the RSDs (%) were in the range of 0.1 to 0.9 %.These results show that the developed nanoprobe was selective, and highly accurate to determine this important food additive in the seasonings of instant noodles, also showing a reduced environmental impact based on the metrics currently accepted for the evaluation of the green profile and practicability.

Three-dimensional characteristic and evolution of creep cavity and microcrack of HR3C austenitic heat resistant steel after long-term creep at 650 °C

Three-dimensional characteristics of creep cavities and microcracks in HR3C austenitic steel after creep at 650 °C were investigated using high resolution X-ray computed tomography (CT) and three-dimensional atomic probe (3DAP). The variation of cavity volume fraction is related to the increasing fraction of cavities undergoing growth and coalescence. Irregular lamellar or “W” shaped microcrack along the grain boundary were observed by the CT and the number large sized microcracks decreased significantly with decreasing stress levels. 3DAP results show that the concentration of P elements was high at the M23C6/γ interface at the early stage of creep. With the increase of creep time, M23C6/γ interface have been found to not only contain high concentration of P element, but also be enriched with Si. The coarsening of the carbides at the grain boundary and the enrichment of P and Si elements at the interface creates the conditions for the nucleation of creep cavities and microcracks under stress. Thus, stress has an tremendous influence on the distribution of creep cavities and the propagation path of microcracks. Additionally, with the decrease of stress, the creep damage mode changes from intergranular/transgranular mixed cracks to creep cavity.

A luminescence-derived cryptostratigraphy from the Lake Suigetsu sedimentary profile, Japan: 45,000–30,200 IntCal20 yr BP

The luminescence characteristics of sediments are affected by a variety of environmental factors, reflecting both local and broader regional influences. If seeking to apply stimulated luminescence as a ‘pure’ dating technique, variability in these external variables needs to be controlled for, involving, inter alia, lengthy pretreatment procedures and complex dose rate corrections. However, in so doing, a lot of potentially valuable palaeoenvironmental information is lost.Instead, in the present study, we explicitly analysed raw, non-pretreated sediment that preserves this wealth of contributory environmental influence. Using a SUERC portable luminescence (POSL) reader, we performed rapid profiling across a 14,800 year interval of the annually laminated (varved) Lake Suigetsu sedimentary profile, central Japan (i.e., 45,000 to 30,200 IntCal20 yr BP), producing 303 contiguous measurements with a mean sampling resolution of 49 years. To further inform our understanding of this dataset, additional follow-up laboratory dosing was performed to provide sensitivity estimates.The ‘cryptostratigraphy’ (‘hidden stratigraphy’) revealed by our data includes the identification of a step-change in luminescence parameters circa 39,200 IntCal20 yr BP, which we attribute to a major earthquake that resulted in re-routing of inflow to the lake. Further variability in the derived luminescence signals is compared with supporting high resolution x-ray fluorescence (μXRF) data and palynological data from Lake Suigetsu. A correlation between the luminescence profile (both net infra-red-stimulated and net blue light-stimulated signals) and mean annual temperature is revealed, mediated through subtle differences in sediment characteristics under warmer or cooler climatic conditions.