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Nine halloysite nanotubes (HNTs) have been examined using scanning electron microscopy (SEM), atomic force microscopy (AFM) and (cross-sectional) transmission electron microscopy (TEM) to evaluate details of their external and internal morphologies. The samples span morphologies within the cylindrical to prismatic-polygonal framework proposed by Hillier et al. (2016). The 'carpet roll' model assumed in the conceptualization of most technological applications of HNTs is shown to be far too simplistic. Both cylindrical and prismatic forms have abundant edge steps traversing their surfaces that, by analogy with plates of kaolinite, correspond to prism faces. The mean value for the diameter of the central lumen of the tubes is 12 nm. Numerous slit-like nanopores, with diameters up to 18 nm, also occur between packets of layers, particularly in prismatic forms at the junction between a central cylindrical core and outer packets of planar layers. These pores expose aluminol and siloxane surfaces, but unlike the lumen, which is assumed only to expose an aluminol surface, they do not extend along the entire length of the nanotube. Edge steps seen most clearly by AFM correspond in height to the packets of layers seen in TEM. TEM cross-sections suggest that tube growth occurs by accretion of a spiralled thickening wedge of layers evolving from cylindrical to polygonal form and reveal that planar sectors may be joined by either abrupt angular junctions or by short sections of curved layers. A more realistic model of the internal and external morphologies of HNTs is proposed to assist with understanding of the behaviour of HNTs in technological applications.

Granite-related wolframite-quartz veins are the world's most important tungsten mineralization and production resource. Recent progress in revealing their hydrothermal processes has been greatly facilitated by the use of infrared microscopy and laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) analysis of both quartz- and wolframite-hosted fluid inclusions. However, owing to the paucity of detailed petrography, previous fluid inclusion studies on coexisting wolframite and quartz are associated with a certain degree of ambiguity. To better understand the fluid processes forming these two minerals, free-grown crystals of intergrown wolframite and quartz from the giant Yaogangxian W deposit in South China were studied using integrated in situ analytical methods including cathodoluminescence (CL) imaging, infrared microthermometry, Raman microspectroscopy, and fluid inclusion LA-ICP-MS analysis. Detailed crystal-scale petrography with critical help from CL imaging shows repetition of quartz, wolframite, and muscovite in the depositional sequence, which comprises a paragenesis far more complex than previous comparable studies. The reconstruction of fluid history in coexisting wolframite and quartz recognizes at least four successive fluid inclusion generations, two of which were entrapped concurrently with wolframite deposition. Fluctuations of fluid temperature and salinity during precipitation of coexisting wolframite and quartz are reflected by our microthermometry results, according to which wolframite-hosted fluid inclusions do not display higher homogenization temperature or salinity than those in quartz. However, LA-ICP-MS analysis shows that both primary fluid inclusions in wolframite and quartz-hosted fluid inclusions associated intimately with wolframite deposition are characterized by strong enrichment in Sr and depletion in B and As compared to quartz-hosted fluid inclusions that are not associated with wolframite deposition. The chemical similarity between the two fluid inclusion generations associated with wolframite deposition implies episodic tungsten mineralization derived from fluids exhibiting distinct chemical signatures. Multiple chemical criteria including incompatible elements and Br/Cl ratios of fluid inclusions in both minerals suggest a magmatic-sourced fluid with the possible addition of sedimentary and meteoric water. Combined with microthermometry and Raman results, fluid chemical evolution in terms of B, As, S, Sr, W, Mn, Fe, and carbonic volatiles collectively imply fluid phase separation and mixing with sedimentary fluid may have played important roles in wolframite deposition, whereas fluid cooling and addition of Fe and Mn do not appear to be the major driving factor. This study also shows that fluid inclusions in both wolframite and coexisting quartz may contain a substantial amount of carbonic volatiles (CO2 ± CH4) and H3BO3. Ignoring the occurrence of these components can result in significant overestimation of apparent salinity and miscalculation of LA-ICP-MS elemental concentrations. We suggest that these effects should be considered critically to avoid misinterpretation of fluid inclusion data, especially for granite-related tungsten-tin deposits.

Crystallization of groundmass minerals may record the physicochemical conditions of magmatic processes upon eruption and is thus a topic of interdisciplinary research in the disciplines of mineralogy, petrology, and volcanology. Recent studies have reported that the groundmass crystals of some volcanic rocks exhibit a break in their crystal size distribution (CSD) slopes that range from a few micrometers to hundreds of nanometers. The crystals consisting of the finer parts of the break were defined as nanolites. In this study, we report the presence of nanometer-scale crystals down to 1 nm in the pyroclasts of the 2011 eruption of Shinmoedake, the Kirishima volcano group, based on field emission-scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). We discovered a gap (hiatus) from ∼100 to ∼30 nm in the size distribution of pyroxene in a dense juvenile fragment of a vulcanian explosion. The pyroxene crystals ∼20-30 nm on a diameter were ferroaugite (C2/c), while those a few hundred nanometers in width had a composite structure consisting of the domains of orthopyroxene (Pbca), augite (C2/c), and sub-calcic augite (C2/c). In high-angle annular dark-field scanning TEM images of the same sample, bright spots ∼1-2 nm in diameter were recognized with a gap in size from ∼10-20 nm titanomagnetite (Fd,3m). They are presumed to have Fe-rich compositions, although their phases were too small to be determined. In addition, we found that crystals smaller than a few tens of nanometers for pyroxene and 100 nm for plagioclase did not exist or their number densities were too low for accurate determination. This indicates that there are practical minimum sizes of the crystals. These observations show that nucleation of the nanoscale crystals almost paused (froze) in the late stage of groundmass crystallization, possibly due to a decrease in undercooling, increase in interfacial free energy, and decrease in diffusivity in a dehydrated melt, whereas crystal growth was mostly continuous. In this paper, we introduce the novel term \"ultrananolite,\" to refer to crystals smaller than 30 nm in diameter, and redefine \"nanolite\" simply as those 30 nm to 1 µm in width, complementing the size interval of crystals in volcanic groundmass smaller than microlites (1-30 µm). In the transient nucleation process, the presence of subcritical size clusters is required. The observed ultrananolite-sized particles might partly include subcritical clusters. The difference in the slope of CSDs, presence of gaps in size distribution, and minimum crystal size among the eruption styles of the 2011 Shinmoedake eruption may be interpreted by considering the difference in magma residence time and fragmentation pressure in the shallow conduit, and possibly the rewelding process in the crater.

The Neoproterozoic sulfur isotope (δ34S) record is characterized by anomalously high δ34Spyrite values. Many δ34Spyrite values are higher than the contemporaneous δ34Ssulfate (i.e., δ34Spyrite > δ34Ssulfate), showing reversed fractionation. This phenomenon has been reported from the Neoproterozoic post-glacial strata globally and is called \"Neoproterozoic superheavy pyrite.\" The commonly assumed biogenic genesis of superheavy pyrite conflicts with current understanding of the marine sulfur cycle. Various models have been proposed to interpret this phenomenon, including extremely low concentrations of sulfate in seawaters or pore waters, or the existence of a geographically isolated and geochemically stratified ocean. Implicit and fundamental in all these published models is the assumption of a biogenic origin for pyrite genesis, which hypothesizes that the superheavy pyrite is syngenetic (in the water column) or early diagenetic (in shallow marine sediments) in origin and formed via microbial sulfate reduction (MSR). In this study, the Cryogenian Datangpo Formation in South China, which preserves some of the highest δ34Spyrite values up to +70 ppm, is studied by secondary ion mass spectrometry (SIMS) at unprecedented spatial resolutions (2 µm). Based on textures and the new sulfur isotope results, we propose that the Datangpo superheavy pyrite formed via thermochemical sulfate reduction (TSR) in hydrothermal fluids during late burial diagenesis and, therefore, lacks a biogeochemical connection to the Neoproterozoic sulfur cycle. Our study demonstrates that SEM-SIMS is an effective approach to assess the genesis of sedimentary pyrite using combined SEM petrography and micrometer-scale δ34S measurements by SIMS. The possibility that pervasive TSR has overprinted the primary δ34Spyrite signals during late diagenesis in other localities may necessitate the reappraisal of some of the δ34Spyrite profiles associated with superheavy pyrite throughout Earth's history.

In January 2020, a workshop was held at EMBL-EBI (Hinxton, UK) to discuss data requirements for the deposition and validation of cryoEM structures, with a focus on single-particle analysis. The meeting was attended by 47 experts in data processing, model building and refinement, validation, and archiving of such structures. This report describes the workshop's motivation and history, the topics discussed, and the resulting consensus recommendations. Some challenges for future methods-development efforts in this area are also highlighted, as is the implementation to date of some of the recommendations.

The terminal Ediacaran Period is signaled worldwide by the first appearance of skeletonizing tubular metazoan fossils, e.g., Cloudina Germs, 1972 and Sinotubulites Chen, Chen, and Qian, 1981. Although recent efforts have focused on evaluating the taxic composition and preservation of such assemblages from the southwestern United States, comparable forms reported in the 1980s from Mexico remain to be re-examined. Here, we reassess the latest Ediacaran skeletal materials from the La Ciénega Formation of the Caborca region in Sonora, Mexico, using a combination of analytical methods: optical microscopy of extracted fossils, thin-section petrography, scanning electron microscopy and energy dispersive X-ray spectroscopy, and X-ray tomographic microscopy. From our examination, we conclude that the La Ciénega hosts a polytaxic assemblage of latest Ediacaran tubular organisms that have been preserved through two taphonomic pathways: coarse silicification and calcareous recrystallization preserving finer details. Further, these fossils show signs that their shells might not have been inflexible or completely mineralized in vivo, and that they might also record tentatively interpreted predation traces in the form of drill holes or puncture marks. This work, along with ongoing efforts around the world, helps to provide a framework for biostratigraphic correlation and possible subdivision of the Ediacaran Period, and further shapes our view of metazoan evolution and ecology in the interval directly preceding the Cambrian explosion.

The occurrence of minor elements in the structure of biogenic diatomaceous opal-A is an important issue because it is closely related to biogeochemical processes driven by the precipitation, sedimentation, and storage of diatoms, as well as to the properties and applications of diatomite, which is the sedimentary rock composed of diatomaceous opal-A. However, to date, there is no direct microscopic evidence for the existence of minor elements, such as Al, Fe, and Mg, in the structure of diatomaceous opal-A, because such evidence requires observation of the internal structure of frustules to exclude the disturbance of impurity minerals, which is technically challenging using conventional techniques. In this work, transmission electron microscopy (TEM) and scanning electron microscopy (SEM) combined with energy-dispersive X-ray spectroscopy (EDS) mapping analysis were performed on diatomaceous opal-A from three typical diatomite specimens that were pretreated using focused ion beam (FIB) thinning. This technique produces a slice of a diatom frustule for direct TEM observation of the internal structure of the diatomaceous opal-A. The results of this work clearly indicate that minor elements, such as Al, Fe, Ca, and Mg, conclusively exist within the siliceous framework of diatomaceous opal-A. The contents of these minor elements are at atomic ratio levels of 1 (minor element)/10 000 (Si) - 1/100, regardless of the genus of the diatoms. The occurrence of minor elements in the internal structure is likely through biological uptake during biosynthesis by living diatoms. Moreover, surface coatings composed of aluminosilicates on diatom frustules are common, and the contents of elements such as Al and Fe are tens or hundreds of times higher in the coatings than in the internal siliceous structure of diatomaceous opal-A. The discovery of the incorporation of the above-mentioned minor elements in the diatomaceous opal-A structure, both in the internal Si-O framework and on the surface, updates the knowledge about the properties of diatomite.

Natural samples of the rare earth element (REE)-bearing silicate minerals cerite, mosandrite, kainosite, zircon, and eudialyte were studied using reflectance spectroscopy in the visible to short-wave infrared regions (500 to 2500 nm) and further characterized by scanning electron microscopy and electron microprobe analysis. Spectral features of these minerals are driven primarily by 4f-4f intraconfigurational electronic transitions of trivalent lanthanides, as well as 5f-5f electronic transitions of uranium and vibrational overtones and combinations of H2O and OH-. Spectra of eudialyte are also impacted by relative amounts of IVFe2+ and VFe2+. Respective spectra of these REE-bearing silicate minerals are sufficiently distinct to enable spectral classification. Spectral variability (e.g., band depths and locations) of some specific REE-related absorptions, such as an Er3+- and Yb3+-related absorption near 978 nm and Nd3+-related absorptions near 746, 803, and 875 nm, are interpreted to be driven by cation site differences in the crystal structures. This work adds to the growing understanding of REE-bearing mineral reflectance spectroscopy, which facilitates detection, identification, and quantification of REE-bearing silicate minerals in remote sensing applications. This is especially relevant for hyperspectral imaging spectroscopy with high spatial resolutions where the spectral response of a pixel becomes increasingly dominated by mineralogy rather than lithology.

Interstratified clay minerals reflect the weathering degree and record climatic conditions and the pedogenic processes in the soil. It is hard to distinguish a few layers of interstratified clay minerals from the chlorite matrix, due to their similar two-dimensional tetrahedral-octahedral-tetrahedral (TOT) structure and electron-beam sensitive nature during transmission electron microscopy (TEM) imaging. Here, we used multiple advanced TEM techniques including low-dose high-resolution TEM (HRTEM), high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) imaging combined with energy-dispersive spectroscopic (EDS) mapping to study interstratified layers in a chlorite sample from Changping, Beijing, China. We demonstrated an interstratified mica or pyrophyllite monolayer could be well distinguished from the chlorite matrix by projected atomic structures, lattice spacings, and chemical compositions with advanced TEM techniques. Further investigation showed two different transformation mechanisms from mica or pyrophyllite to chlorite: either a 4 Å increase or decrease in the lattice spacing. This characterization approach can be extended to the studies of other electron-beam sensitive minerals.

Pozzolanic reaction of volcanic ash with hydrated lime is thought to dominate the cementing fabric and durability of 2000-year-old Roman harbor concrete. Pliny the Elder, however, in first century CE emphasized rock-like cementitious processes involving volcanic ash (pulvis) \"that as soon as it comes into contact with the waves of the sea and is submerged becomes a single stone mass (fierem unum lapidem), impregnable to the waves and every day stronger\" (Naturalis Historia 35.166). Pozzolanic crystallization of Al-tobermorite, a rare, hydrothermal, calcium-silicate-hydrate mineral with cation exchange capabilities, has been previously recognized in relict lime clasts of the concrete. Synchrotron-based X-ray microdiffraction maps of cementitious microstructures in Baianus Sinus and Portus Neronis submarine breakwaters and a Portus Cosanus subaerial pier now reveal that Al-tobermorite also occurs in the leached perimeters of feldspar fragments, zeolitized pumice vesicles, and in situ phillipsite fabrics in relict pores. Production of alkaline pore fluids through dissolution-precipitation, cation-exchange and/or carbonation reactions with Campi Flegrei ash components, similar to processes in altered trachytic and basaltic tuffs, created multiple pathways to post-pozzolanic phillipsite and Al-tobermorite crystallization at ambient seawater and surface temperatures. Long-term chemical resilience of the concrete evidently relied on water-rock interactions, as Pliny the Elder inferred. Raman spectroscopic analyses of Baianus Sinus Al-tobermorite in diverse microstructural environments indicate a cross-linked structure with Al3+ substitution for Si4+ in Q3 tetrahedral sites, and suggest coupled [Al3++Na+] substitution and potential for cation exchange. The mineral fabrics provide a geoarchaeological prototype for developing cementitious processes through low-temperature rock-fluid interactions, subsequent to an initial phase of reaction with lime that defines the activity of natural pozzolans. These processes have relevance to carbonation reactions in storage reservoirs for CO2 in pyroclastic rocks, production of alkali-activated mineral cements in maritime concretes, and regenerative cementitious resilience in waste encapsulations using natural volcanic pozzolans.