Transmission X-ray Microscopy Research Articles

Molecular Sorption Mechanisms of Cr(III) to Organo-Ferrihydrite Coprecipitates Using Synchrotron-Based EXAFS and STXM Techniques.

Ubiquitous organo-ferrihydrite coprecipitates (OFC) significantly affect the mobility and availability of Cr in soil through sorption, but the underlying sorption mechanisms remain unclear at the molecular level. Due to the potential formation of OFC in agricultural soils with returned crop straws, we synthesized OFC with rice/rape straw-derived carbon (C) sources and different loadings. The molecular sorption mechanisms of Cr(III) to the synthesized OFC under different conditions were investigated by Cr K-edge extended X-ray absorption fine structure (EXAFS) spectroscopy and scanning transmission X-ray microscopy (STXM). Cr(III) sorption by OFC decreased with increasing C loading and decreasing pH, regardless of C sources. Moreover, inhibition of Cr(III) sorption to OFC with high C loading occurred when ionic strength (IS) increased, suggesting the presence of outer-sphere complexed Cr(III). EXAFS analysis revealed that more Cr(III) were bound to ferrihydrite of the OFC at a relatively high pH, and organically bound Cr(III) enhanced when increasing C loading and decreasing IS. STXM analysis strongly suggested that C loading reduced Cr(III) sorption through blocking the binding sites on the ferrihydrite, which overwhelmed Cr(III) retention by the direct binding of Cr(III) to carboxyl of the particulate organic matter (OM) and OM coated on the Fh fractions of the OFC. These findings facilitated the comprehensive understanding of the sorption mechanisms of Cr(III) to OFC at the molecular level, which will assist the prediction of Cr(III) mobility in soils, particularly for Cr(III)-contaminated agricultural soils with the application of crop straws.

Ketonic decarboxylation and esterification of propionic acid over beta zeolites

Abstract The present work reports the nanocrystalline Beta zeolites synthesis from the high concentration hydrogels and their behavior in the propionic acid esterification with cyclohexanol and in the ketonic decarboxylation of propionic acid. The solids were characterized by X-ray diffraction, N2-adsorption, transmission and scanning electron microscopy, diffuse reflectance infrared spectroscopy. Three types of acid sites has been evidenced in Beta zeolites: external silanol groups (Si–OH) (with weakly acidity), Si–OH–Al groups (with strong Bronsted acidity) and silanol nests associated with the defect sites (with Lewis acidity). In the propionic acid esterification with cyclohexanol, the highest cyclohexyl propionate yield was obtained over the sample with the highest specific surface area, the highest mesopore volume and the highest Bronsted acidity. In the propionic acid ketonic decarboxylation, the catalyst with the lowest ratio Bronsted acid sites/Lewis acid sites showed the highest activity and selectivity towards 3-pentanone compared to the other two which are more selective towards propanol.

Detonation synthesis of ZrO2 by means of an ammonium nitrate-based explosive emulsion

A zirconium (IV) oxide powder was successfully synthesized from the detonation of an explosive emulsion previously mixed with zirconium sulfate tetrahydrate salt (Zr(SO4)2·4H2O) as a ceramic precursor. After detonation of the energetic mixture in a detonation tank, the as-synthesized ceramic material was purified and characterized by X-ray diffraction, transmission and scanning electron microscopy techniques, nitrogen physisorption and dynamic light scattering. The ceramic powder is made of crystalline nanosized particles exhibiting a homogeneous sphere-like morphology. An attempt to explain the oxide ceramic synthetic mechanism is discussed. The detonation synthetic route implementing high temperatures and high pressures in a short time may be seen as an encouraging method for large-scale production of nanopowder.

Multimodal imaging and machine learning to enhance microscope images of shale

A machine learning based image processing workflow is presented to enhance shale source rock microscopic images obtained using diverse imaging platforms. Images were acquired from a 30μm diameter cylindrical Vaca Muerta shale sample using both nondestructive Transmission X-ray Microscopy (TXM, alternately referred to as nano computed tomography) and destructive Focused Ion Beam-Scanning Electron Microscopy (FIB-SEM). Output cross-sectional images from each modality were aligned using a combination of manual and automated registration techniques to create a registered image dataset. We then apply this dataset for two image processing tasks: prediction of image cross sections with SEM-like resolution from nondestructive TXM data and repair of charged region artifacts (localized accumulation of electrons) within SEM images. The image processing algorithms for both tasks use deep learning models, specifically image-to-image Convolutional Neural Networks (CNNs) and conditional Generative Adversarial Networks (cGANs). In the image enhancement tasks, we are able to achieve significant qualitative and quantitative improvement in TXM images. The best model reaches an average Peak Signal to Noise Ratio (PSNR) of 15.8 dB. Conditioning on TXM data is also shown to reduce artifacts from SEM charging, achieving an average PSNR of 25.8 dB. Our results suggest that properly trained and validated networks are capable of significant enhancement of images obtained using nondestructive techniques, thereby improving interpretation of two- and three-dimensional images while preserving samples for future use.

Direct Imaging of the ac Component of Pumped Spin Polarization with Element Specificity

Spin pumping in a ferromagnet/nonferromagnet heterostructure is directly imaged with spatial resolution as well as element selectivity. The time-resolved detection in scanning transmission x-ray microscopy allows to directly probe the spatial extent of the ac spin polarization in Co-doped ZnO which is generated by spin pumping from an adjacent permalloy microstrip. Comparing the relative phases of the dynamic magnetization component of the two constituents is possible and found to be antiphase. The correlation between the distribution of the magnetic excitation in the permalloy and the Co-doped ZnO reveals that laterally there is no one-to-one correlation. The observed distribution is rather complex, but integrating over larger areas clearly demonstrates that the spin polarization in the nonferromagnet extends laterally beyond the region of the ferromagnetic microstrip. Therefore the observations are better explained by a local spin pumping efficieny and a lateral propagation of the ac spin polarization in the nonferromagnet over the range of a few micrometers.

Local oxidation states of Ni, Co, and Mn atoms within pristine and charged LixNi0.88Co0.08Mn0.04O2 primary particles

Pristine and charged (4.35 V at 1st cycle charge) primary particle samples of LixNi0.88Co0.08Mn0.04O2 lithium-ion battery (LIB) cathode material have been prepared by a sonication method. The local oxidation states of Ni, Co, and Mn atoms within these samples have been estimated from the local Ni L3-edge, Co L3-edge, Mn L3-edge, and O K-edge spectra measured by scanning transmission X-ray microscopy (STXM) with around 30 nm lateral space resolution. The average oxidation state of the Mn atoms has been estimated as about 4+, and that of the Co atoms as about 3+, over the whole particle area for both the pristine and charged samples. For the Ni atoms, with space integration over the particles, the average oxidation state was estimated as about 2.5+ for the pristine sample and 3.0–3.2+ for the charged sample. The space-resolved spectral features indicate that, for the pristine sample, the average oxidation state of the Ni atoms is 2.2–2.5+ in the outside (surface) area, and 2.9–3.0+ in the inside (bulk) area of the particles. For the charged particles, the average oxidation state of the Ni atoms ranged from about 2.4+ to 3.4+, although in most areas it was 3.0+ or higher. The O K-edge spectra, correspondingly, showed different features according to the sample and the location within the particles. The O K-edge spectral feature changes have been interpreted with reference to the hybridization between the 2p orbitals of O and the 3d orbitals of the Ni4+–Ni2+, Co3+, and Mn4+ cations.

Regulation mechanisms of humic acid on Pb stress in tea plant (Camellia sinensis L.)

Though the interaction between humic acid (HA) and heavy metals has been widely reported, the effects of HA on the toxicity of heavy metals to plants are still in debate. In this study, the regulation mechanisms of HA on Pb stress in tea plant (Camellia sinensis L.) was investigated through hydroponic experiments, and the experimental results were explained by using transmission electron microscope (TEM), scanning transmission X-ray microscopes (STXM) and isobaric tags for relative and absolute quantitation (iTRAQ) differential proteomics. Significant alleviation of Pb stress was found with HA coexistence. TEM results showed that HA greatly mitigated the damage of cells caused by Pb stress. Compared with sole Pb treatment, the addition of HA increased the contents of pectin and pectic acid in the cell wall by 10.5% and 30.5%, while arabinose (Ara) and galactose (Gal) decreased by 20.5% and 15.9%, respectively, which were beneficial for increasing Pb adsorption capacity of the cell wall and promoting cell elongation. Moreover, iTRAQ differential proteomics analysis proved that HA strengthened the antioxidant system, promoted the synthesis of cell wall, and stabilized protein and sulfur-containing substance metabolism in molecular level. Notably, the concentration of calcium (Ca) in the cell wall of HA coexistence treatment was 47.4% higher than Pb treatment. STXM results also indicated that the distribution of Ca in the cell wall was restored with the presence of HA. This might promote the formation of the egg-box model, thus alleviating Pb stress in cells. Our results reveal the regulation mechanisms of HA on Pb detoxification in plants and provide useful information for improving the safety of agricultural products.

Weak Stripe Angle Determination by Quantitative x-ray Magnetic Microscopy

High-resolution scanning transmission x-ray microscopy (STXM) can provide quantitative access to local magnetization canting angles relative to the surface. We use this cutting-edge microscopy technique to probe the weak stripe magnetic texture hosted by a 180-nm-thick ${\mathrm{Co}}_{40}{\mathrm{Fe}}_{40}{\mathrm{B}}_{20}$ layer. We report a full set of measurements of the weak stripe canting angle, as well as a method that uses only a single-impinging-direction x-ray beam to extract the angle. This method also allows the spatial profile to be extracted with 30 nm resolution, and the canting angle versus applied field can be measured. Combining these information, the macroscopic magnetization versus applied field loop on a complex spin texture can be reconstructed in an unprecedented way and shows undoubtedly that flux closure domains exist. These results show that the presence of flux closure domains, at the surface of such a thick film, is difficult to demonstrate by means of the STXM technique. Beyond the characterization of the weak stripe angle, this quantitative x-ray magnetic microscopy can be used to study the local textures hosted in all materials exhibiting some circular x-ray magnetic dichroism.

A self-healing liquid metal anode with PEO-Based polymer electrolytes for rechargeable lithium batteries

Ga-Sn liquid metal material is demonstrated as a self-healing anode system due to its fluidity via operando synchrotron-based transmission X-ray microscopy and X-ray diffraction experiments. Cracks formed due to volume expansions can be recovered by the fluidity of the liquid metals. By incorporating with a poly(ethylene oxide) (PEO)-based electrolyte at 60 °C, the Ga-Sn anode shows a reversible lithium insertion and extraction process with a high initial discharge specific capacity of 682 mAh g − 1, followed by delivering a capacity of 462 mAh g − 1 in the second cycle at C/20 rate. Compared with its solid counterparts, the Ga-Sn liquid metal anode demonstrates a better capability to maintain its mechanical integrity and better contact with PEO solid electrolytes due to its advantageous features of the liquid. This study suggests a potential strategy to use liquid metal alloys with polymer solid electrolyte to solve the challenges in rechargeable lithium batteries.

In Operando X-ray Studies of High-Performance Lithium-Ion Storage in Keplerate-Type Polyoxometalate Anodes.

Polyoxometalates (POMs) have emerged as potential anode materials for lithium-ion batteries (LIBs) owing to their ability to transfer multiple electrons. Although POM anode materials exhibit notable results in LIBs, their energy-storage mechanisms have not been well-investigated. Here, we utilize various in operando and ex situ techniques to verify the charge-storage mechanisms of a Keplerate-type POM Na2K23{[(MoVI)MoVI5O21(H2O)3(KSO4)]12 [(VIVO)30(H2O)20(SO4)0.5]}·ca200H2O ({Mo72V30}) anode in LIBs. The {Mo72V30} anode provides a high reversible capacity of up to ∼1300 mA h g-1 without capacity fading for up to 100 cycles. The lithium-ion storage mechanism was studied systematically through in operando synchrotron X-ray absorption near-edge structure, ex situ X-ray diffraction, ex situ extended X-ray absorption fine structure, ex situ transmission electron microscopy, in operando synchrotron transmission X-ray microscopy, and in operando Raman spectroscopy. Based on the abovementioned results, we propose that the open hollow-ball structure of the {Mo72V30} molecular cluster serves as an electron/ion sponge that can store a large number of lithium ions and electrons reversibly via multiple and reversible redox reactions (Mo6+ ↔ Mo1+ and V5+/V4+↔ V1+) with fast lithium diffusion kinetics (DLi+: 10-9-10-10 cm2 s-1). No obvious volumetric expansion of the microsized {Mo72V30} particle is observed during the lithiation/delithiation process, which leads to high cycling stability. This study provides comprehensive analytical methods for understanding the lithium-ion storage mechanism of such complicated POMs, which is important for further studies of POM electrodes in energy-storage applications.

Intracellular amorphous Ca-carbonate and magnetite biomineralization by a magnetotactic bacterium affiliated to the Alphaproteobacteria.

Bacteria synthesize a wide range of intracellular submicrometer-sized inorganic precipitates of diverse chemical compositions and structures, called biominerals. Their occurrences, functions and ultrastructures are not yet fully described despite great advances in our knowledge of microbial diversity. Here, we report bacteria inhabiting the sediments and water column of the permanently stratified ferruginous Lake Pavin, that have the peculiarity to biomineralize both intracellular magnetic particles and calcium carbonate granules. Based on an ultrastructural characterization using transmission electron microscopy (TEM) and synchrotron-based scanning transmission X-ray microscopy (STXM), we showed that the calcium carbonate granules are amorphous and contained within membrane-delimited vesicles. Single-cell sorting, correlative fluorescent in situ hybridization (FISH), scanning electron microscopy (SEM) and molecular typing of populations inhabiting sediments affiliated these bacteria to a new genus of the Alphaproteobacteria. The partially assembled genome sequence of a representative isolate revealed an atypical structure of the magnetosome gene cluster while geochemical analyses indicate that calcium carbonate production is an active process that costs energy to the cell to maintain an environment suitable for their formation. This discovery further expands the diversity of organisms capable of intracellular Ca-carbonate biomineralization. If the role of such biomineralization is still unclear, cell behaviour suggests that it may participate to cell motility in aquatic habitats as magnetite biomineralization does.

Integration between bacterial consortium and magnetite (Fe3O4) nanoparticles for the treatment of oily industrial wastewater.

The study aimed to investigate the efficiency of exogenous bacterial consortium (Enterobacter cloacae and Pseudomonas otitidis) decorated (immobilized) with Fe3O4 Nanoparticles for the treatment of petroleum hydrocarbon-contaminated wastewater. Glycine coated magnetite Nanoparticles (Fe3O4 NPs) were prepared using reverse co-precipitation method and were characterized using X-ray diffraction, transmission and scanning electron microscopy and vibrating sample magnetometer. They were used to decorate exogenous bacterial consortium (Enterobacter cloacae and Pseudomonas otitidis) at 3 different Fe3O4/bacteria ratios (1:1, 1:3 and 3:1 w/w). Bioremediation of oil contaminated wastewater collected from one of the petroleum distribution companies, Alexandria was conducted for 168h using Fe3O4/bacterial association at the best ratio (3:1) and compared with non-decorated consortium and the indigenous bacteria in the control. Analysis indicated crystalline structure of Fe3O4 NPs with spherical particles (size: 15-20nm) and superparamagnetic properties. Glycine modified-Fe3O4 exhibited high ability to immobilize bacteria which acquired its magnetic properties. The highest coating efficiency (92%) was achieved at 3:1 Fe3O4/bacteria ratio after 1 h. This ratio positively affected bacterial growth reaching the highest growth rate (5.07 fold higher than the control) after 4h. The highest removal efficiencies of the total suspended solids (TSS), chemical oxygen demands (COD), oil and grease (O&G) and total petroleum hydrocarbons (TPH) recording 96, 65.4, 83.9 and 85% reaching residual concentrations of 9.5, 598, 99 and 60mg/l respectively were achieved after 4h by the Fe3O4-bacteria assembly. Compared with the maximum permissible limits of the tested parameters, TSS residue was highly compiled with its limit (50mg/l), while COD, O&G and TPH were 7.5, 9.9, and 120-folds higher than their limits (100, 15 and 0.5mg/l respectively). To the best of our knowledge it is first time to use integrated Enterobacter cloacae and Pseudomonas otitidis consortium decorated with Fe3O4 NPs for the treatment of petroleum hydrocarbon-contaminated wastewater. The proposed system proved to be a very efficient, economical and applicable for the removal of the included contaminants in very short running time which increases its biotechnological added value.

Azimuthal-rotation sample holder for molecular orientation analysis.

In this study, an azimuthal-rotation sample holder compatible with scanning transmission X-ray microscopy was developed. This holder exhibits improvement in the accuracy of rotation angles and reduces the displacement of the rotation axes during azimuthal rotation by using a crossed roller bearing. Toevaluate the performance of the holder, the authors investigated the dependence of the optical density around the C K-edge absorption of π-orbital-oriented domains in natural spherical graphite on the rotational angle by using linearly horizontally and vertically polarized undulator radiation. Based on the dependence of the optical density ratio between C 1s → π* and 1s → σ* excitation on the polarization angle of the X-rays, the average two-dimensional orientation angle of the π orbital in each position in a natural spherical graphite sample was visualized.

In situ synthesis and long-term stabilization of nanosilver in poly(vinyl acetate-co-butyl acrylate-co-neodecanoate) matrix for antibacterial applications

Although the synthesis and the study of properties of silver nanoparticles (AgNP) have been the subject of much research, it is also of great interest the development of new hybrid nanomaterials based on AgNP and the corresponding stabilization by means of new substrates, especially polymeric ones like vinylacrylic and derivatives, extensively used in industrial applications. These types of substrates in addition to stabilizing these nanoparticles take advantage of the synergy of properties between both types of materials. The purpose of this research is the in situ synthesis of AgNP in poly (vinyl acetate-co-butyl acrylate-co-neodecanoate) (VAVTD) terpolymer water emulsion as stabilization matrix and the corresponding characterization. UV-VIS, X-ray photoelectron spectroscopy (XPS), transmission (TEM) and scanning electron microscopy (SEM) were used to characterize these AgNP polymer hybrids. Additionally, preliminary work was carried out to assess the biofilm formation of a multiple antibiotic resistance (MAR) strain of Pseudomonas aeruginosa on these AgNP/VAVTD hybrids in order to explore their use in antibacterial applications. The results show that VAVTD terpolymer water emulsion, in low concentrations, is a very good substrate to stabilize AgNP particles as evidenced by the SEM and TEM studies, and the relatively small displacement in the corresponding UV spectra of AgNP particles, even after 45 d of ageing. It was also found a significant reduction of P. aeruginosa cell viability in biofilms formed at 1 and 7 d (p < 0.05) on VAVDT/AgNP hybrid materials, suggesting potential antibacterial properties. Our results also provide important insights to the current knowledge in control strategies for MAR bacterial infections, such as those caused by P. aeruginosa, while avoiding the spreading of resistant strains in healthcare facilities and multiple environments related to human everyday live, especially for surfaces that require antibacterial protection.

Comparison of Enhanced Photocatalytic Degradation Efficiency and Toxicity Evaluations of CeO2 Nanoparticles Synthesized Through Double-Modulation

We demonstrated that Fe/Cr doped and pH-modified CeO2 nanoparticles (NPs) exhibit enhanced photocatalytic performance as compared to bare CeO2 NPs, using photocatalytic degradation. To assess the toxicity level of these double-modified CeO2 NPs on the human skin, they were introduced into HaCaT cells. The results of our conventional cellular toxicity assays (neutral red uptake and 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide for assays) indicated that Cr@CeOx NPs prompt severe negative effects on the viability of human cells. Moreover, the results obtained by scanning transmission X-ray microscopy and bio-transmission electron microscope analysis showed that most of the NPs were localized outside the nucleus of the cells. Thus, serious genetic toxicity was unlikely. Overall, this study highlights the need to prevent the development of Cr@CeOx NP toxicity. Moreover, further research should aim to improve the photocatalytic properties and activity of these NPs while accounting for their stability issues.

Revealing Nanoscale Chemical Heterogeneities in Polycrystalline Mo-BiVO4 Thin Films.

The activity of polycrystalline thin film photoelectrodes is impacted by local variations of the material properties due to the exposure of different crystal facets and the presence of grain/domain boundaries. Here a multi-modal approach is applied to correlate nanoscale heterogeneities in chemical composition and electronic structure with nanoscale morphology in polycrystalline Mo-BiVO4 . By using scanning transmission X-ray microscopy, the characteristic structure of polycrystalline film is used to disentangle the different X-ray absorption spectra corresponding to grain centers and grain boundaries. Comparing both spectra reveals phase segregation of V2 O5 at grain boundaries of Mo-BiVO4 thin films, which is further supported by X-ray photoelectron spectroscopy and many-body density functional theory calculations. Theoretical calculations also enable to predict the X-ray absorption spectral fingerprint of polarons in Mo-BiVO4 . After photo-electrochemical operation, the degraded Mo-BiVO4 films show similar grain center and grain boundary spectra indicating V2 O5 dissolution in the course of the reaction. Overall, these findings provide valuable insights into the degradation mechanism and the impact of material heterogeneities on the material performance and stability of polycrystalline photoelectrodes.

The Effect of the Starting Mineralogical Mixture on the Nature of Fe-Serpentines Obtained during Hydrothermal Synthesis AT 90°C

AbstractThe formation conditions and stability fields of Fe-serpentines are still poorly understood in both terrestrial (natural or anthropic) and extraterrestrial environments. Knowledge of the effects of physical-chemical parameters on compositional and structural features of Fe-serpentines is lacking, and only a few thermodynamic parameters of these minerals are available in the literature. To fill these gaps, the synthesis of these minerals, while controlling all the physicochemical experimental parameters, was undertaken. Two hydrothermal syntheses were carried out at 90°C to investigate the effect of two different starting mineralogical mixtures on the nature of Fe-serpentines. The run products were identified by several analytical techniques (powder X-ray diffraction, transmission, and scanning electron microscopy). Berthierine crystals were synthesized from a starting mixture of kaolinite and metal iron. The berthierines synthesized show different morphologies and iron contents (~3–38 at.%). From a starting mineralogical mixture composed of quartz and metal iron, cronstedtite crystallizes. Most of the crystals are 1M polytypes. Magnetite is always associated with both berthierine and cronstedtite. Lepidocrocite was observed only in the experiment with kaolinite. These experimental results demonstrated that Fe enrichment in serpentines depends on the silicate precursor (kaolinite or quartz) of the starting mixture. The results are also in agreement with the geochemical equilibrium predicted by thermodynamic modeling, i.e. the formation of berthierine and cronstedtite in association with magnetite at the expense of metal iron and silicates.

Pushing the temporal resolution in absorption and Zernike phase contrast nanotomography: enabling fast in situ experiments.

Hard X-ray nanotomography enables 3D investigations of a wide range of samples with high resolution (<100 nm) with both synchrotron-based and laboratory-based setups. However, the advantage of synchrotron-based setups is the high flux, enabling time resolution, which cannot be achieved at laboratory sources. Here, the nanotomography setup at the imaging beamline P05 at PETRA III is presented, which offers high time resolution not only in absorption but for the first time also in Zernike phase contrast. Two test samples are used to evaluate the image quality in both contrast modalities based on the quantitative analysis of contrast-to-noise ratio (CNR) and spatial resolution. High-quality scans can be recorded in 15 min and fast scans down to 3 min are also possible without significant loss of image quality. At scan times well below 3 min, the CNR values decrease significantly and classical image-filtering techniques reach their limitation. A machine-learning approach shows promising results, enabling acquisition of a full tomography in only 6 s. Overall, the transmission X-ray microscopy instrument offers high temporal resolution inabsorption and Zernike phase contrast, enabling in situ experiments at thebeamline.

Application of FIB-SEM Techniques for the Advanced Characterization of Earth and Planetary Materials.

Advanced microanalytical techniques such as high-resolution transmission electron microscopy (HRTEM), atom probe tomography (APT), and synchrotron-based scanning transmission X-ray microscopy (STXM) enable one to characterize the structure and chemical and isotopic compositions of natural materials down towards the atomic scale. Dual focused ion beam-scanning electron microscopy (FIB-SEM) is a powerful tool for site-specific sample preparation and subsequent analysis by TEM, APT, and STXM to the highest energy and spatial resolutions. FIB-SEM also works as a stand-alone technique for three-dimensional (3D) tomography. In this review, we will outline the principles and challenges when using FIB-SEM for the advanced characterization of natural materials in the Earth and Planetary Sciences. More specifically, we aim to highlight the state-of-the-art applications of FIB-SEM using examples including (a) traditional FIB ultrathin sample preparation of small particles in the study of space weathering of lunar soil grains, (b) migration of Pb isotopes in zircons by FIB-based APT, (c) coordinated synchrotron-based STXM characterization of extraterrestrial organic material in carbonaceous chondrite, and finally (d) FIB-based 3D tomography of oil shale pores by slice and view methods. Dual beam FIB-SEM is a powerful analytical platform, the scope of which, for technological development and adaptation, is vast and exciting in the field of Earth and Planetary Sciences. For example, dual beam FIB-SEM will be a vital technique for the characterization of fine-grained asteroid and lunar samples returned to the Earth in the near future.

Combining Soft- and Hard-Templating Approaches in MWW-Type Zeolites.

A combination of hard-templating (HT) and soft-templating (ST) approaches was studied to obtain MWW-type materials with intermediate physicochemical properties. The HT methodology involved the introduction of carbon particles as hard templates during gel synthesis to obtain a layered zeolitic precursor (LZP) with particles possessing a microspherical morphology. The LZP obtained was treated with surfactants as soft templates to expand the layers of the LZP, followed by a pillaring procedure. The materials were characterized by X-ray diffraction, transmission and scanning electron microscopy, elemental analysis and N2 adsorption. The results demonstrate that the obtained material possesses intermediate properties from both approaches, with interparticle mesopores/macropores and pore sizes between 18 and 46 Å. However, the ST procedure causes a partial disruption of some microspheres, forming small crystallite aggregates, and results in a decrease in the number of interparticle mesopores/macropores previously formed by the HT method.