Electron Microprobe Research Articles

Phase equilibria of the Nb–Si-Gd ternary system at 1273K

The phase equilibria of the Nb–Si-Gd ternary system at 1273K in all the composition ranges were investigated by X-ray diffraction (XRD), electron probe microanalysis (EPMA), and Scanning electron microscopy (SEM) equipped with Energy dispersive spectroscopy (EDS). The isothermal section comprises 12 single-phase regions, 22 two-phase regions, and 11 three-phase regions. The existing of Nb3Si phase was confirmed at 1273K by couple diffusion. A new ternary compound Gd2Nb3Si4 was discovered and its crystal structure was analyzed by the Rietveld method with Rwp = 2.11%, Rp = 1.54%, Rexp = 0.75%. It belongs to the space group P41212 (No.92) with the lattice parameter a = b = 6.99048Å, c = 12.94393Å, α = β = γ = 90°.

Phase relations in the Gd2O3-Sm2O3-ZrO2 system: Experimental studies and thermodynamic modeling

Sm2Zr2O7 and Gd2Zr2O7 are two promising transparent ceramic materials with high density and effective atomic number. However, the phase diagram of Gd2O3-Sm2O3-ZrO2 system has not been systematically studied. To determine the phase relationship of the ternary system Gd2O3-Sm2O3-ZrO2 at 1600°C and 1400°C, a serious of ceramic samples were prepared and studied by X-ray diffraction, scanning electron microscope, and electron probe microanalysis. In the range of 66.6 mol.% ZrO2, the solubility of Gd2O3 is 20–22.5 mol.% at 1600°C, and the binary intermediate phases Sm2Zr2O7 and Gd2Zr2O7 form a continuous solid solution at 1400°C. Using the experimental data as a foundation, thermodynamic modeling was performed using the approach. Based on the experimental data, the mixing parameters of fluorite, B and C phases were optimized, and thermodynamic modeling was performed using the CALPHAD (CALculation of PHAse Diagram) method. For the first time, a self-consistent database for Gd2O3-Sm2O3-ZrO2 ternary system was established.

Application of Digital Image Correlation for Strain Mapping of Structural Elements and Materials

Application of Digital Image Correlation for Strain Mapping of Structural Elements and Materials

Modelling and optimising the performance of graphene oxide-Cu2SnS3-polyaniline nanocomposite as an adsorbent for mercury ion removal.

Finding a cost-effective, efficient, and environmentally friendly technique for the removal of mercury ion (Hg2+) in water and wastewater can be a challenging task. This paper presents a novel and efficient adsorbent known as the graphene oxide-Cu2SnS3-polyaniline (GO-CTS-PANI) nanocomposite, which was synthesised and utilised to eliminate Hg2+ from water samples. The soft-soft interaction between Hg2+ and sulphur atoms besides chelating interaction between -N and Hg2+ is the main mechanism for Hg2+ adsorption onto the GO-CTS-PANI adsorbent. Various characterisation techniques, including Fourier transform infrared spectrophotometry (FT-IR), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectroscopy (EDX), transmission electron microscopy (TEM), elemental mapping analysis, and X-ray diffraction analysis (XRD), were employed to analyse the adsorbent. The Box-Behnken method, utilising Design Expert Version 7.0.0, was employed to optimise the crucial factors influencing the adsorption process, such as pH, adsorbent quantity, and contact time. The results indicated that the most efficient adsorption occurred at pH 6.5, with 12mg of GO-CTS-PANI adsorbent, and 30-min contact time that results in a maximum removal rate of 95% for 50mg/L Hg2+ ions. The study also investigated the isotherm and kinetics of the adsorption process that the adsorption of Hg2+ onto the adsorbent happened in sequential layers (Freundlich isotherm) and followed by the pseudo-second-order kinetic model. Furthermore, response surface methodology (RSM) analysis indicates that pH is the most influential parameter in enhancing adsorption efficiency. In addition to traditional models, this study employed some artificial intelligence (AI) methods including the Random Forest algorithm to enhance the prediction of adsorption process efficiency. The findings demonstrated that the Random Forest algorithm exhibited high accuracy with a correlation coefficient of 0.98 between actual and predicted adsorption rates. This study highlights the potential of the GO-CTS-PANI nanocomposite for effectively removing of Hg2+ ions from water resources.

Novel single phase warm white-emitting phosphor BaLaGaO4:Dy3+,Sm3+ with high thermal stability and color stability

In this study, new phosphors BaLaGaO4 (BLGO) doped with dysprosium (Dy3+) and samarium (Sm3+) ions were created using a high-temperature solid-state method. Characterizations with X-ray diffraction (XRD), scanning electron microscope (SEM), energy dispersive X-ray spectroscopy (EDS), and elemental mapping revealed successful doping and uniform elemental distribution. Then the samples were tested for photoluminescence (PL) spectra, the results indicated that the BaLaGaO4:xDy3+ (BLGO:xDy3+) phosphors emitted strong blue and yellow light upon excitation at 350 nm. The emission peaks were located at 480 and 572 nm, respectively. By introducing different proportions of Sm3+ ions, the BaLaGaO4:0.04Dy3+,ySm3+ (BLGO:0.04Dy3+,ySm3+) samples could be excited at 365 nm, and enhancing the red emission component of the phosphor. Meantime, with increasing Sm3+ content, the correlated color temperature (CCT) decreased from 5507 to 3767 K. And the emission spectrum and decay lifetime of BLGO:0.04Dy3+,ySm3+ confirmed the energy transfer from Dy3+ to Sm3+. Furthermore, at 423 K, the luminous intensity of BLGO:0.04Dy3+,0.04Sm3+ retained 86 % of its strength at 298 K, and the chromaticity shift (ΔS) was only 0.00574, which indicated that the sample had excellent thermal stability and excellent color stability. Finally, using the prepared sample and a 365 nm light-emitting diode (LED) chip, a white light-emitting diode (WLED) was fabricated. The CCT of the manufactured WLED also showed a corresponding reduction (from 3423 to 2814 K). Moreover, under the working conditions of 3.4 V and 0.6A, the thermal imaging obtained after 90 min of WLED operation shows the stability of the packaged WLED at high temperature. These researches show that the phosphor has potential application value in indoor lighting technologies.

Petrological, chemical, and chronological study of breccias in the Chang'e‐5 soil

AbstractWe carried out a petrological, mineralogical, and geochemical study of fragmental and regolith breccia clasts separated from two Chang'e‐5 (CE‐5) soil samples, CE5C0000YJYX03501GP and CE5C0400, which provide an opportunity to investigate the compositional change of regolith at the landing site through time. Fragmental breccia CE‐5‐B3 contains a diverse range of basaltic clasts and basaltic mineral fragments, and some rare Mg‐suite‐like minerals. Regolith breccias CE‐5‐B006, CE‐5‐B007, CE‐5‐B010‐08, CE‐5‐B010‐09, CE‐5‐B011‐07, and CE‐5‐B016‐03 contain mare basaltic fragments, mare vitrophyric clasts, rare Mg‐rich fragments possibly derived from the Mg‐suite rocks, and impact‐derived glass spherules. Pb‐isotope data obtained for baddeleyite grains found both inside some of the basaltic clasts identified in breccia fragments and in the breccia matrices yield Pb/Pb dates similar to the 2 Ga crystallization age of the CE‐5 basalt fragments, extracted directly from the soil sample. Seventy‐four Pb isotope analyses of Ca‐phosphate grains also indicate that the majority of these grains have Pb/Pb dates of 2 Ga, suggesting that they originate from the CE‐5 basalts. In addition, a Pb–Pb isochron drawn through analyses of four Ca‐phosphates in breccia CE5‐B006 yielded an intercept corresponding to a date of 3871 ± 46 Ma, which is the best possible estimate of the formation age of these four grains. Electron probe microanalysis shows that the breccias contain components similar to CE‐5 mare basalt fragments extracted directly from the soil sample, implying that the fragmental and regolith breccia fragments are mostly composed of material sourced from the underlying basalts. The general absence of impact melt breccia clasts, along with the general lack of Fe–Ni metal and absence of added meteoritic debris all suggest that the regolith at the CE‐5 landing site is immature and dominated by material mixed together by small local impact cratering events. Trace element analyses show that the glass beads in the regolith breccias have a Th abundance of 4.06–5.28 μg g−1. This is similar to the Th content of the regolith above the Em4 unit at the landing site as measured from orbit, as well as the estimated bulk Th content of CE‐5 basalts, suggesting that Th of the local regolith is predominantly sourced from the underlying mare basalts, without significant Th addition from Th‐rich exotic clasts sourced from evolved lunar lithologies.

On the crystal-chemistry of inderite, Mg[B3O3(OH)5](H2O)4·H2O

The crystal chemistry of inderite, a hydrous borate with known ideal formula MgB3O3(OH)5·5H2O from the Kramer deposit, was re-investigated by electron probe micro-analysis in wavelength dispersive mode, laser ablation-(multi collector-)inductively coupled plasma-mass spectrometry and single-crystal neutron diffraction. The chemical data prove that the real composition of the investigated inderite is substantially identical to the ideal one, with insignificant content of potential isomorphic substituents, so that, excluding B, inderite does not contain any other industrially-relevant element (e.g., Li concentration is lower than 2.5 wt ppm, Be or REE lower than 0.1 wt ppm). The average δ11BNIST951 value of ca. − 7 ‰ lies within the range of values in which the source of boron is ascribable to terrestrial reservoirs (e.g., hydrothermal brines), rather than to marine ones. Neutron structure refinements, at both 280 and 10 K, confirm that the building units of the structure of inderite consist of: two BO2(OH)2 tetrahedra (B-ion in sp3 electronic configuration) and one BO2(OH) triangle (B-ion in sp2 electronic configuration), linked by corner-sharing to form a (soroborate) B3O3(OH)5 ring, and a Mg-octahedron Mg(OH)2(OH2)4. The B3O3(OH)5 ring and the Mg-octahedron are connected, by corner-sharing, to form an isolated Mg(H2O)4B3O3(OH)5 (molecular) cluster. The tri-dimensional edifice of inderite is therefore built by heteropolyhedral Mg(H2O)4B3O3(OH)5 clusters mutually connected by H-bonds, mediated by the zeolitic (“interstitial”) H2O molecules lying between the clusters, so that the correct form of the chemical formula of inderite is Mg[B3O3(OH)5](H2O)4·H2O, rather than MgB3O3(OH)5·5H2O. All the thirteen independent oxygen sites of the structure are involved in H-bonding, as donors or as acceptors. This confirms the pervasive nature and the important role played by the H-bonding network on the structural stability of inderite. The differences between the crystal structure of the two dimorphs inderite and kurnakovite are discussed.

A high-resolution map of functional miR-181 response elements in the thymus reveals the role of coding sequence targeting and an alternative seed match.

MicroRNAs (miRNAs) are critical post-transcriptional regulators in many biological processes. They act by guiding RNA-induced silencing complexes to miRNA response elements (MREs) in target mRNAs, inducing translational inhibition and/or mRNA degradation. Functional MREs are expected to predominantly occur in the 3' untranslated region and involve perfect base-pairing of the miRNA seed. Here, we generate a high-resolution map of miR-181a/b-1 (miR-181) MREs to define the targeting rules of miR-181 in developing murine Tcells. By combining a multi-omics approach with computational high-resolution analyses, we uncover novel miR-181 targets and demonstrate that miR-181 acts predominantly through RNA destabilization. Importantly, we discover an alternative seed match and identify a distinct set of targets with repeat elements in the coding sequence which are targeted by miR-181 and mediate translational inhibition. In conclusion, deep profiling of MREs in primary cells is critical to expand physiologically relevant targetomes and establish context-dependent miRNA targeting rules.

Exploring the gene expression network involved in the heat stress response of a thermotolerant tomato genotype

BackgroundThe increase in temperatures due to the current climate change dramatically affects crop cultivation, resulting in yield losses and altered fruit quality. Tomato is one of the most extensively grown and consumed horticultural products, and although it can withstand a wide range of climatic conditions, heat stress can affect plant growth and development specially on the reproductive stage, severely influencing the final yield. In the present work, the heat stress response mechanisms of one thermotolerant genotype (E42) were investigated by exploring its regulatory gene network. This was achieved through a promoter analysis based on the identification of the heat stress elements (HSEs) mapping in the promoters, combined with a gene co-expression network analysis aimed at identifying interactions among heat-related genes.ResultsResults highlighted 82 genes presenting HSEs in the promoter and belonging to one of the 52 gene networks obtained by the GCN analysis; 61 of these also interact with heat shock factors (Hsfs). Finally, a list of 13 candidate genes including two Hsfs, nine heat shock proteins (Hsps) and two GDSL esterase/lipase (GELPs) were retrieved by focusing on those E42 genes exhibiting HSEs in the promoters, interacting with Hsfs and showing variants, compared to Heinz reference genome, with HIGH and/or MODERATE impact on the translated protein. Among these, the Gene Ontology annotation analysis evidenced that only LeHsp100 (Solyc02g088610) belongs to a network specifically involved in the response to heat stress.ConclusionsAs a whole, the combination of bioinformatic analyses carried out on genomic and trascriptomic data available for tomato, together with polymorphisms detected in HS-related genes of the thermotolerant E42 allowed to determine a subset of candidate genes involved in the HS response in tomato. This study provides a novel approach in the investigation of abiotic stress response mechanisms and further studies will be conducted to validate the role of the highlighted genes.

Zhonghongite, Cu29 (As, Sb)12S33, a new mineral from the high-sulfidation vein of Jiama porphyry system, Tibet, China

Abstract Zhonghongite (IMA2023-046), ideally Cu29(As, Sb)12S33, is a new mineral discovered in the high-sulfidation vein of the Jiama deposit (E 91°45′, N 29°42′), southern Tibet, China. It forms complex intergrowths with watanabeite and tennantite-tetrahedrite, creating veined or massive aggregates ranging from millimeters to centimeters in size. The single crystals of zhonghongite are anhedral grains, with sizes ranging from several micrometers to approximately 100 micrometers. The mineral is gray in color with a black streak and metallic luster. It is brittle, with uneven fractures, and has a calculated density of 4.925g/cm3. The average values of electron microprobe analyses (wt.%) are as follow: Cu 42.19, As 11.11, Sb 16.09, S 25.45, Hg 3.73, Mn 0.67, and Te 0.28. The empirical formula, based on 33 sulfur apfu, is (Cu27.60Hg0.77Mn0.51Fe0.07Ag0.02)Σ28.97(As6.16Sb5.49Te0.09)Σ11.74S33. In zhonghongite, the substitution of Sb for As is limited, with the atomic ratio of As/(As+Sb) ranging from 0.457 to 0.629. Hg, Mn, and Fe, together with minor Cu, are divalent and serve for charge balance. Zhonghongite is orthorhombic, space group F2mm (42), a = 10.37741(5) Å, b = 14.69821(9) Å, c = 36.7645(2) Å and V = 5607.66(5) Å3. The crystal structure has been solved and refined by single-crystal X-ray diffraction with a final R1 = 0.0235 for 27028 (2467 unique) reflections. It is composed of individual AsS3 tripyramids and clustered tripyramids As4S7, CuS4 tetrahedra and CuS3 planar triangles, connected through corner S atoms in tetrahedral coordination and octahedral coordination with Cu and/or As. The structure is a derivative of tetrahedrite-type structure. Zhonghongite was formed under high-temperature conditions and is classified as an intermediate-sulfidation state mineral.

Weld interface metallurgy of dissimilar alloys welded by TIG technique

Abstract TIG welding is an important joining technique for fabricating quality structural components with industrial capability. Dissimilar alloy plates were combined using double-sided tungsten inert gas (TIG) welding. Microstructure evaluation of joints were anayzed by using scanning electron microscopy, optical microscope, energy dispersion spectrometry, elemental mapping, electron back scatter diffraction. DSAW technique increased joint penetration and reduced distortion of joints. In the weld metal zone, austenite, delta ferrite and lath martensite were dominant. The weld pool had high density of Cr7C3 and Fe3C phases and low density of CrFe7C0.45, FeNi, martensite, and Fe3Ni2 phases.

Ultralight molybdenite-doped and phosphate rich alginate composites exhibiting superb chelating ability for UO22+: Adsorption thermodynamics, kinetics and mechanistic evaluation

In the present research work, molybdenite-doped and phosphate-rich alginate composites (MDPA) were developed for uranium removal from aqueous medium and characterized through different analytical techniques such as XPS, FTIR, XRD, SEM-EDS, and elemental mapping. The mass ratio of molybdenite in different MDPA hydrogel beads was optimized, and it was concluded that MDPA-II material (having 22.5% w/w MoS2) has superb chelating ability for UO22+ ions from aqueous solution. The XPS data showed the involvement of S coordination with UO22+ species. It proves that the UO22+ ions bonded to MoS2 surfaces by forming a U-S bond. Moreover, phosphate (OPO3-) group of phytic acid and SMo=S linkages of molybdenite reinforced inner-spherical complexation with UO22+ ions. Kinetics followed pseudo-second-order rate model (R2≈0.99) and equilibrium sorption data found in close agreement with the Langmuir and Temkin models (R2≈0.99). The qm (mg/g) at 298 K was found to be 311.16±7.76 mg/g at optimized pH of 4.5. The study shows the improved sorption performance of MDPA-II hydrogel beads for the uranium competitive recovery.

Exploring the Limits of Fe-Rich Chemistries in Na-Based CaFe2O4-Type Postspinel Oxides.

Structural trends, physical properties, and electrochemical performances of the NaFexRu2-xO4 system have been investigated. Synthesis attempts using both conventional solid-state routes and high-pressure methods were explored for the compositional range 1.0 ≤ x ≤ 1.67. Based on Rietveld refinements against powder X-ray diffraction data, analyses of 57Fe Mössbauer spectroscopy data, and elemental analysis by electron microprobe, the existence of a confined compositional solid solution (1 ≤ x ≤ 1.3) adopting the CaFe2O4-type postspinel structure is demonstrated. This is contrasted with the NaFexTi2-xO4 system, for which no evidence of a solid solution is observed. However, for all explored synthetic routes of NaFexRu2-xO4 compositions, a trivalent iron oxidation state is maintained. Structural analysis and qualitative bond valence energy landscape models reveal that the progressive integration of iron into the postspinel framework results in narrowed sodium ion diffusion channels, restricting electrochemical deintercalation of sodium. Consequently, the CaFe2O4-type iron-rich compounds explored in this study demonstrate limited potential as positive electrode materials for sodium batteries. It is expected that this fundamental insight will help guide the exploration of alternative NaM2O4-based positive electrode materials with similar structure types.

Synthesis of S-Allyl-O, O′-Dibutyl Phosphorodithioate and Its Adsorption Mechanism on Chalcopyrite Surface

The demand for non-ferrous copper metals has increased dramatically with the development of the global economy; accordingly, some refractory copper sulfide ores with low grade and their associated minerals are beginning to be utilized, making the flotation separation of copper concentrates exceptionally difficult, especially the separation of chalcopyrite and pyrite. In this paper, S-allyl-O, O′-dibutyl phosphorodithioate (ADTP) was synthesized by a one-pot method and used as a chalcopyrite collector in the flotation separation of chalcopyrite and pyrite. Flotation experiments results have shown that ADTP exhibits better selectivity and greater collecting power for chalcopyrite under neutral or weak base conditions. The 95% recovery of chalcopyrite can be achieved at pH 8.0 and 8.0 mg/L ADTP. From the analysis results of the contact angle, the SEM-EDS spectrogram, and elemental mapping, it was found that ADTP adsorbed uniformly on a chalcopyrite surface and made a significant contribution to the hydrophobicity of the surface. Confirmed by FTIR and XPS analysis, ADTP was able to form P–S–Cu bonds on a chalcopyrite surface, proving that it was adsorbed on the chalcopyrite surface in the form of chemisorption.

Genetic types and provenance indication of clastic amphibole in the South Yellow Sea

The main focus of studying sediment sources in marine areas is to determine the properties of clastic minerals originating from different rivers. Variations in the characteristics of clastic minerals occur due to differences in the types of source rocks within the watershed. Determining the source rock of clastic minerals in the marine area can improve the accuracy of provenance analysis. Electron probe microanalysis of 258 amphibole grains from six surface stations in the South Yellow Sea (SYS) was conducted to calculate the numerical and characteristic values of cations in the crystal structure. The results showed that amphibole in the SYS is mainly magnesiohornblende (52.2% ~ 81.4%) in the calcic amphibole subgroup, followed by tschermakite. The source rock types of amphibole are mainly different types of magmatic (ultrabasic, basic, and intermediate acidic) and metamorphic rocks. Amphibole derived from intermediate-acid intrusive rocks accounts for a large proportion (>40%). The genetic analysis of clastic amphibole in the SYS showed that most of the medium-acid invading amphibole belong to crust-mantle type, followed by mantle type. Most of the amphibole from metamorphic origins are of medium-low pressure type (± 80%). Combined with electron probe analysis of amphibole from the Huanghe River (the Yellow River, HH) and Changjiang River (the Yangtze River, CJ), the amphibole in the SYS exhibits characteristics inherited from these two rivers. The northern sea area has a strong resemblance to the sediments from the HH, while the southern area is more influenced by sediments supply from the CJ. The central area represents a mixed zone with a higher sediment supply from the HH. The clastic amphibole deduces the type of source rock in different watersheds, serving as a crucial link between the source rock, watershed, and marine area, providing a basis for provenance analysis.

Preparation, microstructure and mechanical properties of novel WC-(Ti,Ta,Mo,V,Cr)(C,N)-Co high-entropy composites

In this work, novel WC-(Ti,Ta,Mo,V,Cr)(C,N)-Co (WC-HECN-Co) high-entropy composite powders were prepared by carbothermal reduction nitriding at 1400 °C and subsequently sintered by spark plasma sintering (SPS) to obtain cemented carbide. The preparation, microstructure and mechanical properties were investigated. The results show that, during the synthesis of WC-HECN-Co, phase evolution follows: (oxide raw material) → (WO3, CoWO4, WO2, V2O5, Ta2O5, Cr2O2.4, CoO, V6O11, TiMoO5, Co3W3C) → (W2C, Co3W3C, WC, WO3, Ta2O5, VO2, Ti6O11) → (WC, Co3W3C, TiTaC2, Ti6O11, Co) → (WC, Co3W3C, HECN, Co) → (WC, HECN, Co). The TEM elemental mapping results show that Ta, Ti, Mo, V and Cr are uniformly distributed with the WC grains to form a composite hard phase that is well bonded with Co. With the temperature increase, the Vickers hardness of SPS sintered WC-HECN-Co bulks gradually increased and the fracture toughness showed a trend of increasing and then decreasing. The Vickers hardness and fracture toughness of the WC-HECN-Co composite reached 1439 Kg·mm−2 and 12.19 MPa·m1/2, respectively. The fracture mechanism of sintered samples is jointly influenced by intergranular fracture and transgranular fracture. This study provides a novel strategy to develop high-performance cemented carbides that contain high-entropy carbonitrides.

Inflammation subsequent to mild iron excess differentially alters regional brain iron metabolism, oxidation and neuroinflammation status in mice

Iron dyshomeostasis and neuroinflammation, characteristic features of the aged brain, and exacerbated in neurodegenerative disease, may induce oxidative stress-mediated neurodegeneration. In this study, the effects of potential priming with mild systemic iron injections on subsequent lipopolysaccharide (LPS)-induced inflammation in adult C57Bl/6J mice were examined. After cognitive testing, regional brain tissues were dissected for iron (metal) measurements by total reflection X-ray fluorescence and synchrotron radiation X-Ray fluorescence-based elemental mapping; and iron regulatory, ferroptosis-related, and glia-specific protein analysis, and lipid peroxidation by western blotting. Microglial morphology and astrogliosis were assessed by immunohistochemistry. Iron only treatment enhanced cognitive performance on the novel object location task compared with iron priming and subsequent LPS-induced inflammation. LPS-induced inflammation, with or without iron treatment, attenuated hippocampal heme oxygenase-1 and augmented 4-hydroxynonenal levels. Conversely, in the cortex, elevated ferritin light chain and xCT (light chain of System Xc−) were observed in response to LPS-induced inflammation, without and with iron-priming. Increased microglial branch/process lengths and astrocyte immunoreactivity were also increased by combined iron and LPS in both the hippocampus and cortex. Here, we demonstrate iron priming and subsequent LPS-induced inflammation led to iron dyshomeostasis, compromised antioxidant function, increased lipid peroxidation and altered neuroinflammatory state in a brain region-dependent manner.

In Operando study of Microsupercapacitors with Gel Electrolytes using nano‐beam synchrotron X‐ray diffraction.

Synchrotron radiation X‐ray diffraction (XRD) with nanoscale beam size was used here for in situ and in operando study of micro‐supercapacitors (MSC) with gel electrolyte and MXene Ti3C2Tx electrodes. The electrode structure was characterized as a function of applied voltage and distance from the gap separating electrodes using microscopic cells with cylindrical shape designed for transmission mode XRD. The devices with gel electrolytes based on H2SO4 (with H2O/PVA and DMSO/PVA) showed stable performance with no changes in MXene structure under voltage swaps between positive and negative values. Experiments with KI‐based electrolytes demonstrated changes of MXene structure correlated with decrease of energy storage parameters under conditions of increased operation voltage starting from 0.8V. The best performance of MSC was observed when no changes in MXene structure occur after switch of applied voltage polarity. The changes of inter‐layer distance of Mxene upon swap of applied voltage correlate with decrease of device performance and are undesirable for stable operation of MSC’s. We also tested feasibility of X‐ray fluorescence (XRF) for characterization of electrolyte ion migration in MSCs using 2D element mapping. Irreversible sorption of iodine by MXene was found using XRF mapping of charged electrodes using standard in‐plane MSC device and KI electrolyte.

The die for the production of the hammered kaptorgas from Kouřim, Central Bohemia

Kaptorgas were small trapezoidal boxes with lids worn by women and girls in early medieval central Europe as magic or protective amulets. The paper presents a new find of a bronze cast die for hammering the front side of kaptorgas, which was excavated at the Nad Dolnicí settlement site located in the hinterland of the important central Bohemian hillfort of Kouřim. The die was used to produce type 1A kaptorgas with a motif of a four-legged eared gryphon with an indication of a wing and a tail ending in a floral decorative element. Although kaptorgas with this particular motif have not been recorded in Bohemia, it has analogies in Bulgaria and Poland. Based on the stylistic assessment of this originally Mediterranean motif and the chronology of type IA kaptorgas in Bohemia, the die can be dated to the 10th and beginning of the 11th century. X-Ray fluorescence analysis and elemental mapping of the object's surface show that it was made from bronze with a significant lead admixture and a small admixture of zinc. The die is discussed in terms of the spread of Mediterranean motifs and their adaptation by local craftsmen.

MOF-derived porous In2O3 nanospheres sensitized by CdS quantum dots: A ppb-level NO2 sensor with ultra-high response at room-temperature

NO2 is one of the most important atmosphere pollutants, causing great harm to the human body at very low concentrations (ppb levels). Herein, a novel fabrication idea for gas sensing materials was reported to detect ppb-level NO2 via MOF-derived porous In2O3 nanospheres (NSs) sensitized by CdS quantum dots (QDs). The good distribution of CdS QDs (2.5–4.0nm) on porous In2O3 NSs was verified by the transmission electron microscopy and element mapping analyses. In comparison to In2O3 NSs, the CdS@In2O3 composite nanospheres (CNSs) exhibited exceptional responses to ppb-level concentrations of NO2 (S=425.1@100 ppb) at room temperature (RT, 25 ºC), while also demonstrating good selectivity and response reproducibility. These improvements in sensing performance were attributed to the synergies of the electronic effects of CdS QDs, MOF-derived porous nanostructures, and enhanced adsorption of NO2 and active O2– by well-dispersed CdS QDs. This work emphasizes that the MOF-derived In2O3 porous NSs sensitized by CdS QDs can accurately detect ppb-level concentrations of the NO2 at RT.