X-ray Tomographic Microscopy Research Articles

The role of CO2 flushing in triggering the ‘Millennium’ eruption and recent unrests at Changbaishan volcano (China/North Korea)

ABSTRACT The impact of large-scale caldera-forming eruptions on our society and climate can be considerable. The triggering mechanisms of these eruptions and the instability of their magmatic systems are still elusive. Here we use X-ray tomographic microscopy, glass geochemistry and volatile element concentration data on the products of the 946 CE ‘Millennium’ eruption (ME) of Changbaishan volcano (China/North Korea) with the aim to identify the triggering mechanism of the eruption. ME emitted rhyolites and trachytes whose textural parameters suggest vesiculation events related to crystallization and magma ascent in the conduit, and to the arrival of new gas in the magmatic system. Solubility models show that the CO2 and H2O dissolved in the glass are consistent with a pressure of 100–200 MPa. Literature data from fluid inclusions in minerals indicate that the residing magma was CO2 free before the eruption, whereas the CO2 content in the glass reaches 600 ppm at the flash of the ME event. We find that a single, shallow magma reservoir localized between 7.5 and 3.7 km depth in which rhyolites occupies the top and trachytes the bottom is fully destabilized by the arrival of external CO2-rich fluids. Such fluids are released from a deeper, carbonate-rich mantle source. Our results and those of independent geophysical data show that the ME magmatic system is still active, and the continuous upraising of fluids from depth may drive unrest episodes like that recorded in 2002–2006. Our findings elucidate the role of deep, mantle-derived fluids in driving large-scale explosive eruptions. We provide evidence that volcanic unrests may not mirror the internal dynamics of magmatic reservoirs.

Wicking dynamics in yarns

The spontaneous imbibition of a liquid within porous media, known as wicking, can display uncommon features in textiles and yarns. Yarns exhibited step-wise wicking dynamics not captured by current models. HypothesisWicking dynamics in yarns not only depend on inter-fiber pore filling, but are mainly determined by the pore-to-pore transition processes and the structure of the pore network. ExperimentsFast X-ray tomographic microscopy is employed to reveal the pore scale processes and neutron radiography for the macroscopic water uptake in yarns. A semi-empirical pore network model is presented that employs the measured pore network topology and pore scale dynamics to reproduce the experimentally observed wicking dynamics in yarns. FindingsThe yarn pore system is a sparse network of long and narrow pores that promotes step-wise uptake dynamics. Wicking in yarns displays fast pore filling events in the order of seconds and long waiting times between filling events up to several minutes while navigating the pore network. As main result, we find that a few filling events directly determine the macroscopic behavior of wicking in the sparse pore network of yarns. It is necessary to consider pore-to-pore transition waiting times and the pore network structure to explain the characteristics of wicking dynamics in yarns.

Mild-intensity physical activity prevents cardiac and osseous iron deposition without affecting bone mechanical property or porosity in thalassemic mice

Thalassemia causes anemia, ineffective erythropoiesis, bone loss and iron accumulation in several tissues, e.g., liver, bone and heart, the last of which leads to lethal cardiomyopathy and arrhythmia. Although exercise reportedly improves bone density in thalassemic mice, exercise performance is compromised and might pose risk of cardiovascular accident in thalassemic patients. Therefore, we sought to explore whether mild-intensity physical activity (MPA) with 30–50% of maximal oxygen consumption was sufficient to benefit the heart and bone. Herein, male hemizygous β-globin knockout (BKO) mice and wild-type littermates were subjected to voluntary wheel running 1 h/day, 5 days/week for 3 months (MPA group) or kept sedentary (SDN; control). As determined by atomic absorption spectroscopy, BKO-MPA mice had less iron accumulation in heart and bone tissues compared with BKO-SDN mice. Meanwhile, the circulating level of fibroblast growth factor-23—a factor known to reduce serum iron and intestinal calcium absorption—was increased early in young BKO-MPA mice. Nevertheless, MPA did not affect duodenal calcium transport or body calcium retention. Although MPA restored the aberrant bone calcium-phosphorus ratio to normal range, it did not change vertebral calcium content or femoral mechanical properties. Microstructural porosity in tibia of BKO-MPA mice remained unaltered as determined by synchrotron radiation X-ray tomographic microscopy. In conclusion, MPA prevents cardiac and bone iron accumulation, which is beneficial to thalassemic patients with limited physical fitness or deteriorated cardiac performance. However, in contrast to moderate-intensity exercise, MPA does not improve bone mechanical properties or reduce bone porosity.

Semisolid Pharmaceutical Product Characterization Using Non-invasive X-ray Microscopy and AI-Based Image Analytics.

This work reports the use of X-ray microscopy (XRM) imaging to characterize the microstructure of semisolid formulations containing multiple immiscible phases. For emulsion-based semisolid formulations, the disperse phase globule size and its distribution can be critical quality attributes of the product. Optical microscopy and light diffraction techniques are traditionally used to characterize globule size distribution. These techniques are subjected to sample preparation bias and present challenges from matrix interference and data processing. XRM imaging is an emergent technique that when combined with intelligent data processing has been used to characterize microstructures of pharmaceutical dosage forms including oral solid formulations, controlled release microspheres, and lyophilized products. This work described our first attempt to use XRM imaging to characterize two complex emulsion-based semisolid formulations, a petrolatum-based ointment with a dispersed phase comprising a hydrophilic liquid, and an oil-in-water cream. This initial assessment of technology showed that microstructure details such as globule size distribution, volume fraction, spatial distribution uniformity, inter-globule spacing, and globule sphericity could be obtained and parameterized. It was concluded that XRM imaging, combined with artificial intelligence-based image processing is feasible to generate advanced characterization of semisolid formulation microstructure through 3D visualization and parameterization of globule attributes. This technique holds promise to provide significantly richer microstructure details of semisolid formulations. When fully developed and validated, it is potentially useful for quantitative comparison of microstructure equivalence of semisolid formulations.

Morphology changes in Fe-Cr porous alloys upon high-temperature oxidation quantified by X-ray tomographic microscopy

The effect of high-temperature oxidation at 850 °C (10 h, 30 h, 100 h) and 900 °C (10 h) on porous (∼30 % porosity) ferritic stainless steel (Fe22Cr) has been investigated using synchrotron tomographic microscopy, which allowed for visualisation, separation and quantitative analysis of the metallic core, closed pores, open pores and oxide scale phase. The same regions within the samples were investigated before and after oxidation performed at different conditions. Quantitative analysis of the tomographic data provided information on changes upon oxidation of the relative volume of the different phases, the specific surface area (SSA) of the metallic core, the thickness of the oxide scale and pore size distribution. The results were discussed in the context of thermogravimetric analysis of the samples and supported by SEM imaging. It was observed that oxidation leads to an increase of the SSA of steel and the largest increase (∼50 %) was obtained for the sample processed for 100 h at 850 °C. It is demonstrated the open porosity forms a network of connected channels within the sample and it dominates in the volume. In addition, the 3D imaging revealed breakaway oxidation areas for samples, for which this phenomenon remained undetected using 2D SEM analysis.

Conductive Heat Transfer in Partially Saturated Gas Diffusion Layers with Evaporative Cooling

Heat transport is an important, though often neglected function of gas diffusion layers (GDLs) of polymer electrolyte membrane fuel cells. Thermal conductivity is a key property, especially in partially water saturated GDLs and when the phase change of water is considered, such as required for evaporative cooling applications. Continuum models require effective transport properties as input, which in this work were determined for different types of dry and partially saturated commercial GDLs (Toray 060 and 120, Freudenberg H23). Three-dimensional microstructures and phase distributions were recorded using X-ray tomographic microscopy, digitalized and used in direct pore-level simulations. The governing energy conservation equation was solved in the three phases (gas, liquid, solid) with interfacial heat transfer between the phases to determine the effective thermal conductivity. Correlations for through-plane effective thermal conductivity in the different GDL types as a function of saturation are provided. An energy sink term, accounting for the evaporation of water, was added, enabling a quantification of the effective conductive heat transfer in GDLs with evaporative cooling. The water distribution (clustered or layered) in the GDLs was found to be a key factor for the thermal conduction and evaporative cooling ability.

Characterization of Ancient Burial Pottery of Ban Muang Bua Archaeological Site (Northeastern Thailand) Using X-ray Spectroscopies

Ancient potteries found at Ban Muang Bua, located in northeastern Thailand, associate with Thung Kula Ronghai culture. Most of them are products used in daily life and grave goods. The potsherds were examined using techniques based on X-ray spectroscopy. Elemental composition and morphology were analyzed using proton-induced X-ray emission spectroscopy (PIXE) and scanning electron microscopy coupled with energy-dispersive X-ray spectroscopy (SEM-EDS). Three-dimensional analysis was performed using X-ray tomographic microscopy based on synchrotron radiation (SR XTM). Irregular plate-like particles of composites with a wide range of size distribution were found in the potsherds. The major (O, Si, and Al), minor (C, Fe, Ca, and K), and trace elements (P, S, Ti, Na, Mg, and Zn) which were observed can provide the information about raw materials and production of pottery. The 3D tomographic images show the internal feature of these samples. The combination of SEM-EDS, PIXE, and SR XTM is a powerful tool for archaeological research especially in terms of composition and internal structure. The results imply that the raw materials of pottery were sandy soil derived from marine sands, clays, and salt deposits that were mostly iron-rich-kaolin clay. The production was carried out with low firing temperatures (~600–900 °C) in open-air kilns.

Performance Evaluation of Silane in Concrete Bridge Decks Using Transmission X-ray Microscopy

The corrosion of steel reinforcement in concrete structures is a most widespread problem. Silane is commonly used as a surface treatment material to reduce the entry of moisture containing harmful chemicals into the concrete matrix, thereby restricting corrosion. There is not a standard test method to evaluate the long-term performance of such sealers when applied on concrete. Moreover, the literature does not have a definitive conclusion on the performance of silanes. In this work, transmission X-ray microscopy (TXM) and optical imaging were used to investigate the mass transport properties and silane thickness of field samples treated with silane to gain insight into the performance of silane coatings. Quantitative measurements using optical staining techniques showed that the average measured silane thickness for all 14 projects was 2.5 mm. The TXM results revealed that, on average, the samples with silane coatings exhibited 8.5 times less penetration of outside chemicals, at a depth of 2 mm, as compared to uncracked samples without silane coatings. This work shows that silanes are a useful and practical tool to significantly reduce the permeability of in-service concrete and resist corrosion.

Diverse and complex developmental mechanisms of early Ediacaran embryo-like fossils from the Weng'an Biota, southwest China.

The origin and early evolution of animal development remain among the many deep, unresolved problems in evolutionary biology. As a compelling case for the existence of pre-Cambrian animals, the Ediacaran embryo-like fossils (EELFs) from the Weng'an Biota (approx. 609 Myr old, Doushantuo Formation, South China) have great potential to cast light on the origin and early evolution of animal development. However, their biological implications can be fully realized only when their phylogenetic positions are correctly established, and unfortunately, this is the key problem under debate. As a significant feature of developmental biology, the cell division pattern (CDP) characterized by the dynamic spatial arrangement of cells and associated developmental mechanisms is critical to reassess these hypotheses and evaluate the diversity of the EELFs; however, their phylogenetic implications have not been fully realized. Additionally, the scarcity of fossil specimens representing late developmental stages with cell differentiation accounts for much of this debate too. Here, we reconstructed a large number of EELFs using submicron resolution X-ray tomographic microscopy and focused on the CDPs and associated developmental mechanisms as well as features of cell differentiation. Four types of CDPs and specimens with cell differentiation were identified. Contrary to the prevailing view, our results together with recent studies suggest that the diversity and complexity of developmental mechanisms documented by the EELFs are much higher than is often claimed. The diverse CDPs and associated development features including palintomic cleavage, maternal nutrition, asymmetric cell divisions, symmetry breaking, establishment of polarity or axis, spatial cell migration and differentiation constrain some, if not all, EELFs as total-group metazoans.This article is part of the theme issue ‘The impact of Chinese palaeontology on evolutionary research’.

Effects of Silver Diamine Nitrate and Silver Diamine Fluoride on Dentin Remineralization and Cytotoxicity to Dental Pulp Cells: An In Vitro Study.

Silver diamine nitrate (SDN) is expected to help control caries similar to silver diamine fluoride (SDF). The aim of this study was to determine the mineral precipitation in demineralized dentin and the cytotoxicity of SDN and SDF to dental pulp cells. Demineralized dentin specimens were prepared, and SDF, SDN, or water (control) was applied. The specimens were then remineralized in simulated body fluid for 2 weeks. The mineral precipitation in the specimens was examined using FTIR-ATR, SEM-EDX, and synchrotron radiation X-ray tomographic microscopy (SRXTM). Additionally, the cytotoxicity of SDF and SDN to human dental pulp stem cells was analyzed using an MTT assay. The increase in FTIR spectra attributable to apatite formation in demineralized dentin in the SDF group was significantly higher compared to the SDN and control groups (p < 0.05). Dentinal tubule occlusion by the precipitation of silver salts was detected in both SDF and SDN groups. The mineral density as shown in SRXTM images and cytotoxicity of both SDN and SDF groups were comparable (p > 0.05). In conclusion, SDF demonstrated superior in vitro apatite formation compared to SDN. However, the degree of mineral precipitation and cytotoxic effects of both were similar.

Synchrotron Radiation Study on Ancient Burnt Rice Found at Archaeological Sites in Thailand

Rice is the food staple for most of the world’s population especially Asians. It is also the essence of life of people in Thailand. Archaeological evidence based on the paddy rice reveals the rice planting in northeastern Thailand over 5,000 years ago. The burnt rice grains have been found in many archaeological sites in Thailand, which are involved with the religious ceremony and home prosperity. In this work, the synchrotron radiation has been applied to investigate the elemental distribution, chemical composition and bio-molecular structure, and three-dimensional segmentation of the ancient burnt rice samples from Nakorn Nayok (Ban Dong Lakon), Suphan Buri (U-Thong), and Prachin Buri (Sri Mahosot) using micro-beam XRF (SR μ-XRF), Infrared spectroscopy (SR IR), and X-ray tomographic microscopy based on synchrotron radiation (SR XTM), respectively. Field emission scanning electron microscope (FE SEM) incorporated with energy dispersive spectrometer (EDS) have been carried out in order to characterize the structure and composition of samples. It has been found that the grains are oblong in shape with a rough surface. Major elements in the grains are C, Si, Ca, and Al. Other trace elements such as Ti, Cr, Mn, Fe, Ni, Cu, and Zn are also detected. The IR spectra provide some information about molecular bonds. The tomographic investigations reveal the internal structure of ancient burnt rice.

Effect of height to diameter ratio on dynamic characteristics of cemented tailings backfills with fiber reinforcement through impact loading

The safety and durability of underground backfilled stopes of metalliferous mines are so crucial owing to several dynamic events such as rock bursting, loads triggered by blasting, and loading conditions under stress. Besides, the effect of height to diameter ratio on dynamic properties of fiber reinforced paste backfill has not yet been explored suitably, but this factor is vital to determine the design properties of mining with backfill. This study deals the findings of the dynamic tests done on fiber reinforced cemented tailings backfills (FRCTB) considering different height to diameter ratios under impact loading. A cement mortar mixed with polypropylene fiber with 12 mm length was made, cast in six diverse molds (H × D: 25 × 50; 30 × 50; 35 × 50; 40 × 50; 45 × 50; and 50 × 50 mm), and experimented through Split-Hopkinson pressure bar (SHPB) setup. Later, internal crack formation within FRCTB was observed by employing a computerized X-ray imaging (CT) and scanning-electron microscope (SEM) system. The results indicated that fracture number/path and failure damage of FRCTB decreases with increasing H/D ratio while their dynamic strengths drop with growing mean strain rate. Fractures arise because of the greatest micro-cracks as a function of stress application. These cracks rise with an increase in specimen size, resulting in lower strengths. Through SEM and CT observations, it is found that polypropylene fiber boosts the cementation of FRCTB and frequent hydration products are attached to fiber surface. Assessing research findings in mine backfill applications will help the better consideration of FRCTB dynamic characteristics, and the actual strength resistance and dynamic durability design of deep mining with backfilling.

Determination of the Porosity and its Heterogeneity of Fuel Cell Microporous Layers by X-Ray Tomographic Microscopy

Determination of the Porosity and its Heterogeneity of Fuel Cell Microporous Layers by X-Ray Tomographic Microscopy

Deep learning based classification of dynamic processes in time-resolved X-ray tomographic microscopy

Time-resolved X-ray tomographic microscopy is an invaluable technique to investigate dynamic processes in 3D for extended time periods. Because of the limited signal-to-noise ratio caused by the short exposure times and sparse angular sampling frequency, obtaining quantitative information through post-processing remains challenging and requires intensive manual labor. This severely limits the accessible experimental parameter space and so, prevents fully exploiting the capabilities of the dedicated time-resolved X-ray tomographic stations. Though automatic approaches, often exploiting iterative reconstruction methods, are currently being developed, the required computational costs typically remain high. Here, we propose a highly efficient reconstruction and classification pipeline (SIRT-FBP-MS-D-DIFF) that combines an algebraic filter approximation and machine learning to significantly reduce the computational time. The dynamic features are reconstructed by standard filtered back-projection with an algebraic filter to approximate iterative reconstruction quality in a computationally efficient manner. The raw reconstructions are post-processed with a trained convolutional neural network to extract the dynamic features from the low signal-to-noise ratio reconstructions in a fully automatic manner. The capabilities of the proposed pipeline are demonstrated on three different dynamic fuel cell datasets, one exploited for training and two for testing without network retraining. The proposed approach enables automatic processing of several hundreds of datasets in a single day on a single GPU node readily available at most institutions, so extending the possibilities in future dynamic X-ray tomographic investigations.

Porosity and Fracture Changes of Coal under Uniaxial Strain Conditions Based on the X-ray Microscopic Imaging Technology

Porosity and Fracture Changes of Coal under Uniaxial Strain Conditions Based on the X-ray Microscopic Imaging Technology

Growth and feeding ecology of coniform conodonts.

Conodonts were the first vertebrates to develop mineralized dental tools, known as elements. Recent research suggests that conodonts were macrophagous predators and/or scavengers but we do not know how this feeding habit emerged in the earliest coniform conodonts, since most studies focus on the derived, ‘complex’ conodonts. Previous modelling of element position and mechanical properties indicate they were capable of food processing. A direct test would be provided through evidence of in vivo element crown tissue damage or through in vivo incorporated chemical proxies for a shift in their trophic position during ontogeny. Here we focus on coniform elements from two conodont taxa, the phylogenetically primitive Proconodontus muelleri Miller, 1969 from the late Cambrian and the more derived Panderodus equicostatus Rhodes, 1954 from the Silurian. Proposing that this extremely small sample is, however, representative for these taxa, we aim to describe in detail the growth of an element from each of these taxa in order to the test the following hypotheses: (1) Panderodus and Proconodontus processed hard food, which led to damage of their elements consistent with prey capture function; and (2) both genera shifted towards higher trophic levels during ontogeny. We employed backscatter electron (BSE) imaging, energy-dispersive X-ray spectroscopy (EDX) and synchrotron radiation X-ray tomographic microscopy (SRXTM) to identify growth increments, wear and damage surfaces, and the Sr/Ca ratio in bioapatite as a proxy for the trophic position. Using these data, we can identify whether they exhibit determinate or indeterminate growth and whether both species followed linear or allometric growth dynamics. Growth increments (27 in Pa. equicostatus and 58 in Pr. muelleri) were formed in bundles of 4–7 increments in Pa. equicostatus and 7–9 in Pr. muelleri. We interpret the bundles as analogous to Retzius periodicity in vertebrate teeth. Based on applied optimal resource allocation models, internal periodicity might explain indeterminate growth in both species. They also allow us to interpret the almost linear growth of both individuals as an indicator that there was no size-dependent increase in mortality in the ecosystems where they lived e.g., as would be the case in the presence of larger predators. Our findings show that periodic growth was present in early conodonts and preceded tissue repair in response to wear and damage. We found no microwear and the Sr/Ca ratio, and therefore the trophic position, did not change substantially during the lifetimes of either individual. Trophic ecology of coniform conodonts differed from the predatory and/or scavenger lifestyle documented for “complex” conodonts. We propose that conodonts adapted their life histories to top-down controlled ecosystems during the Nekton Revolution.

Mineral chemistry and 3D tomography of a Chang’E 5 high-Ti basalt: implication for the lunar thermal evolution history

In December 2020, Chang’E-5 (CE-5), China’s first lunar sample return mission, successfully collected samples totaling 1731 g from the northern Oceanus Procellarum. The landing site was located in a young mare plain, a great distance from those of Apollo and Luna missions. These young mare basalts bear critical scientific significance as they could shed light on the nature of the lunar interior (composition and structure) as well as the recent volcanism on the Moon. In this article, we investigated a CE-5 basalt sample (CE5C0000YJYX065) using a combination of state-of-art techniques, including high resolution X-ray tomographic microscopy (HR-XTM), energy dispersive X-ray spectroscopy (EDS)-based scanning electron microscope (SEM), and electron probe microanalysis (EPMA) to reveal its 3D petrology and minerology. Our results show that this sample has a fine- to medium-grained subophitic texture, with sparse olivine phenocrysts setting in the groundmass of pyroxene, plagioclase, ilmenite and trace amounts of other phases. It has an extremely high ilmenite modal abundance (17.8 vol%) and contains a significant amount (0.5 vol%) of Ca-phosphate grains. The mineral chemistry is in excellent agreement with that of Apollo and Luna high-Ti basalts. The major phase pyroxenes also display strong chemical zoning with compositions following the trends observed in Apollo high-Ti basalts. Based on current data, we came to the conclusion that CE5C0000YJYX065 is a high-Ti mare basalt with a rare earth element (REE) enriched signature. This provides a rigid ground-truth for the geological context at the CE-5 landing site and clarifies the ambiguity inferred from remote sensing surveys.

Bilaterally Asymmetric Helical Myofibrils in Ascidian Tadpole Larvae.

The locomotor system is highly bilateral at the macroscopic level. Homochirality of biological molecules is fully compatible with the bilateral body. However, whether and how single-handed cells contribute to the bilateral locomotor system is obscure. Here, exploiting the small number of cells in the swimming tadpole larva of the ascidian Ciona, we analyzed morphology of the tail at cellular and subcellular scales. Quantitative phase-contrast X-ray tomographic microscopy revealed a high-density midline structure ventral to the notochord in the tail. Muscle cell nuclei on each side of the notochord were roughly bilaterally aligned. However, fluorescence microscopy detected left-right asymmetry of myofibril inclination relative to the longitudinal axis of the tail. Zernike phase-contrast X-ray tomographic microscopy revealed the presence of left-handed helices of myofibrils in muscle cells on both sides. Therefore, the locomotor system of ascidian larvae harbors symmetry-breaking left-handed helical cells, while maintaining bilaterally symmetrical cell alignment. These results suggest that bilateral animals can override cellular homochirality to generate the bilateral locomotor systems at the supracellular scale.

Laser Structured Gas Diffusion Layers for Improved Water Transport and Fuel Cell Performance

Polymer electrolyte fuel cells are promising energy converters for future green energy systems. For wide commercial use, still cost reductions by increasing the power density are required. Structurally optimized gas diffusion layers (GDLs), allowing for cell operation at high current densities with reduced mass transport losses, are an essential component for this development. Here we demonstrate that GDLs modified with perforations can improve water transport in the high current density regions and increase fuel cell performance. Laser perforation prior to GDL hydrophobization circumvents previously observed flooding problems and allows for stable operation. The advanced pattern, connecting channel and land regions drains pores, hence decreasing the liquid water fraction, especially close to the GDL and catalyst layer interface. Operando dynamic X-ray tomographic microscopy (XTM) is employed to understand water transport in the modified structure, and the competition with random break-through of water clusters to the channel is analyzed. The detailed and time-resolved insights allow us to propose guidelines for future advanced patterning geometries, suggesting denser perforations and methods to counteract the observed high frequency resistance (HFR) increase. Furthermore, this approach can act as model system for next generation GDLs and lead to a more rational design of transport layers.

Chemical Heterogeneity in PAN/LLZTO Composite Electrolytes by Synchrotron Imaging

Solid polymer/ceramic composite electrolytes are promising for batteries due to their attractive thermal stability and mechanical properties. Chemical heterogeneity in solid composite electrolytes, such as the inhomogeneity in the ceramic phase and salt distribution at the polymer/ceramic interface, is critical to the performance of solid composite electrolytes. However, such heterogeneity has not been well understood yet. In this work, we use Synchrotron-based X-ray fluorescence imaging (XRF) and Transmission X-ray Microscope (TXM) to image nanoscale chemical heterogeneity in polyacrylamide/Li7+xLa3Zr2−xTaxO12 (LLZTO) composite electrolytes and investigate the effects of lithium salt, salt concentration, and plasticizer. We find that LLZTO particles show strong inter- and intra-particles chemical heterogeneities, and the off-stoichiometry of Zr in an LLZTO particle is unlikely to be only balanced by Ta substitution. Moreover, statistical analysis suggests that LiI tends to accumulate at the ceramic/polymer interface at a low concentration of 5 wt%, but no such tendency was observed in samples with 10 wt% LiI. However, composite electrolytes with LiTFSI show interfacial accumulation at both 5 wt% and 10 wt%. This report provides insight into element distributions in solid composite electrolytes, and we hope further researches can shed light on the connections between chemical heterogeneity and ionic transport pathway inside.