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Electrical mobility demands an increase of battery energy density beyond current lithium-ion technology. A crucial bottleneck is the development of safe and reversible lithium-metal anodes, which is challenged by short circuits caused by lithium-metal dendrites and a short cycle life owing to the reactivity with electrolytes. The evolution of the lithium-metal-film morphology is relatively poorly understood because it is difficult to monitor lithium, in particular during battery operation. Here we employ operando neutron depth profiling as a noninvasive and versatile technique, complementary to microscopic techniques, providing the spatial distribution/density of lithium during plating and stripping. The evolution of the lithium-metal-density-profile is shown to depend on the current density, electrolyte composition and cycling history, and allows monitoring the amount and distribution of inactive lithium over cycling. A small amount of reversible lithium uptake in the copper current collector during plating and stripping is revealed, providing insights towards improved lithium-metal anodes. Rechargeable lithium metal batteries could offer a major leap in energy capacity but suffer from the electrolyte reactivity and dendrite growth. Here the authors apply neutron depth profiling to provide quantitative insight into the evolution of the Li-metal morphology during plating and stripping.

In-situ monazite Th–U–total Pb dating and zircon LA–ICP–MS depth-profiling was applied to metasedimentary rocks from the Vaimok Lens in the Seve Nappe Complex (SNC), Scandinavian Caledonides. Results of monazite Th–U–total Pb dating, coupled with major and trace element mapping of monazite, revealed 603 ± 16 Ma Neoproterozoic cores surrounded by rims that formed at 498 ± 10 Ma. Monazite rim formation was facilitated via dissolution–reprecipitation of Neoproterozoic monazite. The monazite rims record garnet growth as they are depleted in Y2O3 with respect to the Neoproterozoic cores. Rims are also characterized by relatively high SrO with respect to the cores. Results of the zircon depth-profiling revealed igneous zircon cores with crystallization ages typical for SNC metasediments. Multiple zircon grains also exhibit rims formed by dissolution–reprecipitation that are defined by enrichment of light rare earth elements, U, Th, P, ± Y, and ± Sr. Rims also have subdued Eu anomalies (Eu/Eu* ≈ 0.6–1.2) with respect to the cores. The age of zircon rim formation was calculated from three metasedimentary rocks: 480 ± 22 Ma; 475 ± 26 Ma; and 479 ± 38 Ma. These results show that both monazite and zircon experienced dissolution–reprecipitation under high-pressure conditions. Caledonian monazite formed coeval with garnet growth during subduction of the Vaimok Lens, whereas zircon rim formation coincided with monazite breakdown to apatite, allanite and clinozoisite during initial exhumation.

Laser-induced breakdown spectroscopy (LIBS) has emerged as a powerful analytical method for the elemental mapping and depth profiling of many materials. This review offers insight into the contemporary applications of LIBS for the depth profiling of materials whose elemental composition changes either abruptly (multilayered materials) or continuously (functionally graded or corroded materials). The spectrum of materials is discussed, spanning from laboratory-synthesized model materials to real-world products including materials for fusion reactors, photovoltaic cells, ceramic and galvanic coatings, lithium batteries, historical and archaeological artifacts, and polymeric materials. The nuances of ablation conditions and the resulting crater morphologies, which are instrumental in depth-related studies, are discussed in detail. The challenges of calibration and quantitative profiling using LIBS are also addressed. Finally, the possible directions of the evolution of LIBS applications are commented on.

For optoelectronic applications of metal–organic framework (MOF) thin films, it is important to be able to fabricate films and heterostructures that are highly oriented relative to the substrate's surface normal. However, process optimization to achieve this is difficult without sufficiently detailed structural characterization of the deposited films. It is demonstrated that 2D grazing‐incidence wide‐angle X‐ray scattering (GIWAXS) data from a laboratory system go a long way to providing such characterization and can 1) better test structural models than 1D scans, 2) provide a quantitative estimate—useful for process optimization—of the fraction of the deposited film that has the desired surface‐oriented texture (2D powder), and 3) deliver such information as a function of depth into the film—useful for heterostructure characterization. Herein, GIWAXS data collection and analysis are introduced in the context of understanding MOF thin films, then it is shown how the desired oriented fraction (2D powder fraction) of UiO‐66 fabricated by vapor‐assisted conversion can be increased from 4% to over 95% by minimizing nucleation in solution. Finally, it is demonstrated that heterostructures of UiO‐66 and UiO‐67 can be grown wherein both layers are highly ordered (UiO‐66 83%, UiO‐67 >94%) once synthetic protocols are optimized. The structure and orientation of metal‐organic framework (MOF) thin films is revealed by grazing‐incidence wide‐angle X‐ray scattering (GIWAXS) studies on lab scale equipment. The desired oriented fraction of the film versus unwanted randomly oriented crystallites is quantified. This helps with optimizing synthesis protocols and allows a two‐layer MOF heterostructure to be fabricated wherein both layers are highly oriented.

In this study, Ti-Co-Ce getter films were deposited via magnetron sputtering to investigate their activation mechanism—the thermal removal of surface passivation layers to restore gas sorption capability. The morphology before and after film activation was characterized using scanning electron microscopy (SEM) and atomic force microscopy (AFM). The oxygen content on the film surface before and after activation was measured using an energy-dispersive X-ray spectrometer (EDS), and gas desorption during activation was monitored with a quadrupole mass spectrometer (QMS). The combined results confirmed the absence of O2 desorption during activation, suggesting oxygen migration into the film bulk. Crucially, in situ X-ray photoelectron spectroscopy (XPS) combined with controlled Ar+ ion sputtering depth profiling (0–30 nm) was employed to directly probe the chemical-state evolution within the thin film before and after thermal activation at 400 °C, thereby providing direct evidence of the activation dynamics. The data reveal that within the 0–10 nm near-surface region, a strong oxygen chemical potential gradient drives rapid oxide reduction and inward migration of lattice oxygen. At depths of 20–30 nm, moderate reduction coupled with oxygen enrichment induces phase separation, while around 30 nm, a dynamic equilibrium between oxygen inflow and outflow is established. These findings provide a theoretical basis for optimizing activation processes and guiding the development of low-temperature getter materials. This work is particularly relevant for MEMS, vacuum electronics, and other applications with stringent thermal budgets, expanding the design possibilities for heat-sensitive device integration.

In this work, two thin hybrid composites based on organic-like fullerenes (bucky balls C 60 ) and inorganic compounds of lithium cobalt oxide (LiCoO 2 ) were prepared. The composites were synthesized by a combined method of ion sputtering and evaporation. The prepared samples were sandwiched between 2 gold electrodes and subjected to charging at an applied small voltage. After each charging process, the samples were analyzed using two appropriate methods—the surface morphology was monitored using AFM (Atomic Force Microscopy), and lithium depth concentration profiles were measured using NDP (Neutron Depth Profiling). The results of the measurements showed that both types of composite experienced significant changes both in the surface morphology and especially in the depth distribution of lithium. The test confirmed the expectation that the unusual hybrid combination of organic and inorganic phases is electrochemically active and exhibits characteristics of Li battery behavior.

An extremely asymmetric low-pressure discharge was used to study the composition of thin films prepared by PECVD using HMDSO as a precursor. The metallic chamber was grounded, while the powered electrode was connected to an RF generator. The ratio between the surface area of the powered and grounded electrode was about 0.03. Plasma and thin films were characterised by optical spectroscopy and XPS depth profiling, respectively. Dense luminous plasma expanded about 1 cm from the powered electrode while a visually uniform diffusing plasma of low luminosity occupied the entire volume of the discharge chamber. Experiments were performed at HMDSO partial pressure of 10 Pa and various oxygen partial pressures. At low discharge power and small oxygen concentration, a rather uniform film was deposited at different treatment times up to a minute. In these conditions, the film composition depended on both parameters. At high powers and oxygen partial pressures, the films exhibited rather unusual behaviour since the depletion of carbon was observed at prolonged deposition times. The results were explained by spontaneous changing of plasma parameters, which was in turn explained by the formation of dust in the gas phase and corresponding interaction of plasma radicals with dust particles.

The accumulation of solid electrolyte interphases (SEI) in graphite anodes related to elevated formation rates (0.1C, 1C and 2C), cycling rates (1C and 2C), and electrode-separator lamination is investigated. As shown previously, the lamination technique is beneficial for the capacity aging in graphite-LiNi1/3Mn1/3Co1/3O2 cells. Here, surface resistance growth phenomena are quantified using electrochemical impedance spectroscopy (EIS). The graphite anodes were extracted from the graphite NMC cells in their fully discharged state and irreversible accumulations of lithium in the SEI are revealed using neutron depth profiling (NDP). In this post-mortem study, NDP reveals uniform lithium accumulations as a function of depth with lithium situated at the surface of the graphite particles thus forming the SEI. The SEI was found to grow logarithmically with cycle number starting with the main formation in the initial cycles. Furthermore, the EIS measurements indicate that benefits from lamination arise from surface resistance growth phenomena aside from SEI growth in superior anode fractions.

Nitrogen puffing is routinely applied in nuclear fusion plasma experiments with tungsten walls to control the amount of power emitted from the plasma by radiation. However, as nitrogen is retained in significant amounts in tungsten it adds some complexity to the plasma-wall interaction. Basic questions concerning the interaction of nitrogen with tungsten, namely the energy and temperature dependent retention of nitrogen implanted into tungsten and the erosion of the formed tungsten nitride by deuterium, are still open. To address these questions, laboratory experiments with a mass-filtered ion source and sample analysis with in situ x-ray photoelectron spectroscopy (XPS) and nuclear reaction analysis were performed. The results of the implantation and erosion measurements were interpreted by means of simulations with a Monte-Carlo code describing the interaction of energetic particles with matter in the binary collision approximation. This required the development of a forward calculation, converting the simulated depth profiles into XPS intensity ratios. With appropriate settings, the experimental implantation and erosion results at ambient temperature are well described by the simulations. However, for increased temperatures it has been observed that there is an unexpected difference between implanting nitrogen into tungsten before heating the sample and implantation into a heated sample. The application of the developed forward calculation is not limited to the problems presented in this work but can be applied especially to all kind of XPS sputter-depth profiling measurements. Finally, simulations with the previously validated Monte-Carlo code are used to extrapolate the presented results on nitrogen retention to energies and particle compositions relevant for fusion experiments. These simulations make quantitative predictions on nitrogen retention in tungsten and on relevant time scales. The simulations also show that recoil implantation of nitrogen by deuterium significantly increases the effective implantation depth of nitrogen.

Currently two techniques exist for 3D reconstruction of biological samples by time-of-flight secondary ion mass spectrometry (ToF-SIMS). The first, based on microtomy and combining of successive section images, is successfully applied for tissues, while the second, based on sputter depth profiling, is widely used for cells. In the present work, we report the first successful adaptation of sectioning technique for ToF-SIMS 3D imaging of a single cell—fully grown mouse germinal vesicle (GV) oocyte. In addition, microtomy was combined with sputter depth profiling of individual flat sections for three-dimensional reconstruction of intracellular organelles. GV oocyte sectioning allowed us to obtain molecule-specific 3D maps free from artifacts associated with surface topography and uneven etching depth. Sputter depth profiling of individual flat slices revealed fine structure of specific organelles inside the oocyte. Different oocyte organelles (cytoplasm, germinal vesicle, membranes, cumulus cells) were presented on the ion images. Atypical nucleoli referred to as “nucleolus-like body” (NLB) was detected inside the germinal vesicle in PO3− and CN− ions generated by nucleic acids and proteins respectively. Significant difference in PO3− intensity in the NLB central area and NLB border was found. This difference appears as a bright halo around the center area. The NLB size calculated for PO3− and CN− ion images is 12.9 ± 0.2 μm and 11.9 ± 0.2 μm respectively, which suggests that bright halo of PO3− ions is a chromatin compaction on the NLB surface. Areas of approximately 1.0–2.5 μm size inside nucleoplasm with increased PO3− and CN− signal were registered in germinal vesicle. Observed compartments have different sizes and shapes, and they are likely attributed to chromocenters or chromosomes.