scholarly journals Correlative Microscopy: a tool for understanding soil weathering in modern analogues of early terrestrial biospheres

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
R. L. Mitchell ◽  
P. Davies ◽  
P. Kenrick ◽  
T. Volkenandt ◽  
C. Pleydell-Pearce ◽  
...  
Keyword(s):  
Ion Beam ◽  
Ground Cover ◽  
Soil Core ◽  
Correlative Microscopy ◽  
X Ray ◽  
Soil Weathering ◽  
Biological Communities ◽  
Weathering Processes ◽  
Correlative Imaging ◽  
Focussed Ion Beam

AbstractCorrelative imaging provides a method of investigating complex systems by combining analytical (chemistry) and imaging (tomography) information across dimensions (2D-3D) and scales (centimetres-nanometres). We studied weathering processes in a modern cryptogamic ground cover from Iceland, containing early colonizing, and evolutionary ancient, communities of mosses, lichens, fungi, and bacteria. Targeted multi-scale X-ray Microscopy of a grain in-situ within a soil core revealed networks of surficial and internal features (tunnels) originating from organic-rich surface holes. Further targeted 2D grain characterisation by optical microscopy (OM), scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (SEM–EDS), following an intermediate manual correlative preparation step, revealed Fe-rich nodules within the tunnels. Finally, nanotomographic imaging by focussed ion beam microscopy (FIB-SEM) revealed coccoid and filamentous-like structures within subsurface tunnels, as well as accumulations of Fe and S in grain surface crusts, which may represent a biological rock varnish/glaze. We attribute these features to biological processes. This work highlights the advantages and novelty of the correlative imaging approach, across scales, dimensions, and modes, to investigate biological weathering processes. Further, we demonstrate correlative microscopy as a means of identifying fingerprints of biological communities, which could be used in the geologic rock record and on extra-terrestrial bodies.

scholarly journals Revealing Inflammatory Indications Induced by Titanium Alloy Wear Debris in Periprosthetic Tissue by Label-Free Correlative High-Resolution Ion, Electron and Optical Microspectroscopy

Materials ◽  
2021 ◽  
Vol 14 (11) ◽  
pp. 3048
Author(s):  
Rok Podlipec ◽  
Esther Punzón-Quijorna ◽  
Luka Pirker ◽  
Mitja Kelemen ◽  
Primož Vavpetič ◽  
...  
Keyword(s):  
Titanium Alloy ◽  
High Resolution ◽  
Wear Debris ◽  
Ion Beam ◽  
Quantitative Measure ◽  
Label Free ◽  
Periprosthetic Tissue ◽  
Correlative Microscopy ◽  
X Ray ◽  
Tissue Reactions

The metallic-associated adverse local tissue reactions (ALTR) and events accompanying worn-broken implant materials are still poorly understood on the subcellular and molecular level. Current immunohistochemical techniques lack spatial resolution and chemical sensitivity to investigate causal relations between material and biological response on submicron and even nanoscale. In our study, new insights of titanium alloy debris-tissue interaction were revealed by the implementation of label-free high-resolution correlative microscopy approaches. We have successfully characterized its chemical and biological impact on the periprosthetic tissue obtained at revision surgery of a fractured titanium-alloy modular neck of a patient with hip osteoarthritis. We applied a combination of photon, electron and ion beam micro-spectroscopy techniques, including hybrid optical fluorescence and reflectance micro-spectroscopy, scanning electron microscopy (SEM), Energy-dispersive X-ray Spectroscopy (EDS), helium ion microscopy (HIM) and micro-particle-induced X-ray emission (micro-PIXE). Micron-sized wear debris were found as the main cause of the tissue oxidative stress exhibited through lipopigments accumulation in the nearby lysosome. This may explain the indications of chronic inflammation from prior histologic examination. Furthermore, insights on extensive fretting and corrosion of the debris on nm scale and a quantitative measure of significant Al and V release into the tissue together with hydroxyapatite-like layer formation particularly bound to the regions with the highest Al content were revealed. The functional and structural information obtained at molecular and subcellular level contributes to a better understanding of the macroscopic inflammatory processes observed in the tissue level. The established label-free correlative microscopy approach can efficiently be adopted to study any other clinical cases related to ALTR.

Imaging of retina cellular and subcellular structures using ptychographic hard X-ray tomography

2021 ◽  
Vol 134 (19) ◽  
Author(s):  
Valerie Panneels ◽  
Ana Diaz ◽  
Cornelia Imsand ◽  
Manuel Guizar-Sicairos ◽  
Elisabeth Müller ◽  
...  
Keyword(s):  
Focused Ion Beam ◽  
Ion Beam ◽  
Plexiform Layer ◽  
Wild Type Mouse ◽  
Small Region ◽  
Mouse Retina ◽  
Imaging Method ◽  
Scanning Method ◽  
X Ray ◽  
Correlative Imaging

ABSTRACT Ptychographic hard X-ray computed tomography (PXCT) is a recent method allowing imaging with quantitative electron-density contrast. Here, we imaged, at cryogenic temperature and without sectioning, cellular and subcellular structures of a chemically fixed and stained wild-type mouse retina, including axons and synapses, with complete isotropic 3D information over tens of microns. Comparison with tomograms of degenerative retina from a mouse model of retinitis pigmentosa illustrates the potential of this method for analyzing disease processes like neurodegeneration at sub-200 nm resolution. As a non-destructive imaging method, PXCT is very suitable for correlative imaging. Within the outer plexiform layer containing the photoreceptor synapses, we identified somatic synapses. We used a small region inside the X-ray-imaged sample for further high-resolution focused ion beam/scanning electron microscope tomography. The subcellular structures of synapses obtained with the X-ray technique matched the electron microscopy data, demonstrating that PXCT is a powerful scanning method for tissue volumes of more than 60 cells and sensitive enough for identification of regions as small as 200 nm, which remain available for further structural and biochemical investigations.

Advances in 3D characterisation for correlative microscopy in geosciences

2021 ◽  
Author(s):  
Rich Taylor
Keyword(s):  
Electron Microscopy ◽  
Femtosecond Laser ◽  
Electron Backscatter Diffraction ◽  
Ion Beam ◽  
Region Of Interest ◽  
Machine Learning Algorithms ◽  
Three Dimensions ◽  
X Ray ◽  
Nano Scale ◽  
Focussed Ion Beam

<p>The proliferation of modern techniques available for petrologists has resulted in an explosion of detailed information on mineral compositions and processes over the last decade. One area of research that is undergoing dramatic advances is the non-destructive interrogation of samples in three dimensions through X-ray microscopy (XRM). Techniques such as ZEISS Versa and Ultra XRM can be performed at a variety of scales and resolutions, resulting in micro-to-nano scale information on geological samples. Such techniques can be correlated with each other i.e. expanding nanoscale resolution to a large sample or internal calibration of X-ray intensity to identify mineral assemblages, or even correlation with other techniques such as electron microscopy (EM). X-ray techniques are also particularly adaptable to digital resolution enhancements through software processes such as machine learning algorithms.</p><p>Collecting 3D information for petrological investigations can often require ground truthing of mineralogical and compositional interpretations. The more developed the 3D microscopy becomes, the more we are increasingly interested in features that are deeply buried within our samples. This means the corresponding techniques for excavating a region of interest also need to advance in both speed and accuracy.</p><p>The ZEISS Crossbeam-Laser (XBL) system provides a unique capability of rapidly excavating to a point of interest within a 3D sample volume. The XBL is already seeing use in material sciences, with a standard XB chamber with focussed Ion Beam (FIB) and Electron Microscopy (EM), and a correlated femtosecond laser chamber for rapid material removal. Sample data collected through XRM can be correlated to the XBL stage so that any internal features located by XRM have their coordinates automatically available in three dimensions. The femtosecond laser can excavate to a region of interest (RoI) within the sample within seconds or minutes, dramatically reducing preparation time compared to standard FIB/PFIB. The laser cut surface can be used for analysis techniques such as energy dispersive spectroscopy (EDS) and electron backscatter diffraction (EBSD), even prior to final polishing with the focussed ion beam (FIB).</p><p>Here we show the XRM-XBL workflow in high grade metamorphic rocks for identifying minerals in context for geochronology and micro-to-nano scale textures.</p>

Identification and removal of opaque defects on X-ray masks in a focussed ion beam repair system

1987 ◽  
Vol 6 (1-4) ◽  
pp. 617-622 ◽  
Author(s):  
U. Weigmann ◽  
H. Burghause ◽  
H. Schaffer
Keyword(s):  
Ion Beam ◽  
Repair System ◽  
X Ray ◽  
Focussed Ion Beam

scholarly journals Simulating permeability reduction by clay mineral nanopores in a tight sandstone by combining computer X-ray microtomography and focussed ion beam scanning electron microscopy imaging

Solid Earth ◽  
2021 ◽  
Vol 12 (1) ◽  
pp. 1-14
Author(s):  
Arne Jacob ◽  
Markus Peltz ◽  
Sina Hale ◽  
Frieder Enzmann ◽  
Olga Moravcova ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Clay Mineral ◽  
Ion Beam ◽  
Reservoir Rock ◽  
Beam Scanning ◽  
X Ray ◽  
Tight Reservoir ◽  
Focussed Ion Beam ◽  
Scanning Electron

Abstract. Computer X-ray microtomography (µXCT) represents a powerful tool for investigating the physical properties of porous rocks. While calculated porosities determined by this method typically match experimental measurements, computed permeabilities are often overestimated by more than 1 order of magnitude. This effect increases towards smaller pore sizes, as shown in this study, in which nanostructural features related to clay minerals reduce the permeability of tight reservoir sandstone samples. Focussed ion beam scanning electron microscopy (FIB-SEM) tomography was applied to determine the permeability effects of illites at the nanometre scale, and Navier–Stokes equations were applied to calculate the permeability of these domains. With these data, microporous domains (porous voxels) were defined using microtomography images of a tight reservoir sample. The distribution of these domains could be extrapolated by calibration against size distributions measured in FIB-SEM images. For this, we assumed a mean permeability for the dominant clay mineral (illite) in the rock and assigned it to the microporous domains within the structure. The results prove the applicability of our novel approach by combining FIB-SEM with X-ray tomographic rock core scans to achieve a good correspondence between measured and simulated permeabilities. This methodology results in a more accurate representation of reservoir rock permeability in comparison to that estimated purely based on µXCT images.

scholarly journals Glancing-incidence focussed ion beam milling: A coherent X-ray diffraction study of 3D nano-scale lattice strains and crystal defects

2018 ◽  
Vol 154 ◽  
pp. 113-123 ◽  
Author(s):  
Felix Hofmann ◽  
Ross J. Harder ◽  
Wenjun Liu ◽  
Yuzi Liu ◽  
Ian K. Robinson ◽  
...  
Keyword(s):  
Diffraction Study ◽  
Ion Beam ◽  
Crystal Defects ◽  
X Ray Diffraction ◽  
X Ray ◽  
Nano Scale ◽  
Lattice Strains ◽  
Focussed Ion Beam

μ-EXAFS and μ-XRD study of selected regions of a Al–Fe–Cr–Ti complex alloy

2011 ◽  
Vol 1 (SRMS-7) ◽  
Author(s):  
E. Liotti ◽  
S. C. Hogg ◽  
C.A. Kirk ◽  
P. Quinn ◽  
P. S. Grant
Keyword(s):  
Ion Beam ◽  
High Strength ◽  
Al Alloy ◽  
Second Phase ◽  
Preparation Technique ◽  
Complex Alloy ◽  
X Ray ◽  
Key Factor ◽  
Focussed Ion Beam ◽  
Beam Transmission

Al3Ti, Al13Cr2 and Al13Fe4 are important intermetallics in a number of Al alloy systems including complex ultra-high-strength systems with excellent elevated-temperature performance. A full knowledge of their properties and crystallographic structures is a key factor for the understanding of these complex alloys. In the present study samples of the three pure intermetallics were prepared and regions of interest identified in a billet of Al93Fe3Cr2Ti2 alloys and 20 × 10 × 2 µm samples extracted utilizing a Focussed Ion Beam Transmission Electron Microscopy (FIB TEM) sample preparation technique. Using the microfocus spectroscopy beamline I18 at Diamond Light Source we were able to examine 5 µm sections of the samples using X-ray Diffraction (μ-XRD) and Extended X-ray Absorption Fine Structure (μ-EXAFS) in an attempt to describe the local structure of the second-phase particles and characterized the microstructure of the FIBed samples to selectively illuminate the different phases.

The Alteration and Natural Consolidation Effects of a Ceramic Vessel in Archaeological Excavation From San Lorenzo Tenochtitlán, Veracruz, Mexico

1996 ◽  
Vol 462 ◽  
Author(s):  
M.E. Guevara ◽  
M. Lopez ◽  
A. Cruz-Lara ◽  
A. Cyphers ◽  
J.E. Gama
Keyword(s):  
Amorphous Materials ◽  
X Ray Diffraction ◽  
Archaeological Excavation ◽  
X Ray ◽  
Soil Weathering ◽  
San Lorenzo ◽  
Weathering Processes ◽  
Ceramic Vessel ◽  
Petrographic Thin Section ◽  
Early Formative

ABSTRACTA study of a ceramic vessel from San Lorenzo Tenochtitlán, Veracruz, México (Early Formative 1550–900 b.C.) was developed using three selected analytical methods: Petrographic thin section, X-ray Diffraction and Scanning Electron Microscopy. The results suggested, that the soil weathering processes on the ceramic vessel generated phenomenons, such as an increase in porosity, a decrease in bulk-density and loss in structural stability.On the other hand, the presence of amorphous materials (SiO2, FeO3) in the soil, interacted with the ceramic giving it a natural consolidation. The consequences of our study are discussed in detail.

The Basic Physical Principles of Ion, Electron, and X-Ray Detectors and Their Application to Microanalysis

1985 ◽  
Vol 43 ◽  
pp. 154-157
Author(s):  
A.J. Tousimis
Keyword(s):  
Ion Beam ◽  
Depth Resolution ◽  
Sample Surface ◽  
High Energy ◽  
X Rays ◽  
X Ray ◽  
Electrons And Ions ◽  
Spatial Depth ◽  
Minimum Surface Area ◽  
Physical Principles

An integral and of prime importance of any microtopography and microanalysis instrument system is its electron, x-ray and ion detector(s). The resolution and sensitivity of the electron microscope (TEM, SEM, STEM) and microanalyzers (SIMS and electron probe x-ray microanalyzers) are closely related to those of the sensing and recording devices incorporated with them.Table I lists characteristic sensitivities, minimum surface area and depth analyzed by various methods. Smaller ion, electron and x-ray beam diameters than those listed, are possible with currently available electromagnetic or electrostatic columns. Therefore, improvements in sensitivity and spatial/depth resolution of microanalysis will follow that of the detectors. In most of these methods, the sample surface is subjected to a stationary, line or raster scanning photon, electron or ion beam. The resultant radiation: photons (low energy) or high energy (x-rays), electrons and ions are detected and analyzed.

3D Observation of Elemental Distribution of Si-Device using a Dedicated FIB/STEM System

2005 ◽  
Author(s):  
T. Yaguchi ◽  
M. Konno ◽  
T. Kamino ◽  
M. Ogasawara ◽  
K. Kaji ◽  
...  
Keyword(s):  
Focused Ion Beam ◽  
Ion Beam ◽  
Three Dimensional ◽  
Elemental Distribution ◽  
Multivariate Statistical ◽  
X Ray ◽  
Sample Rotation ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Elemental Maps

Abstract A technique for preparation of a pillar shaped sample and its multi-directional observation of the sample using a focused ion beam (FIB) / scanning transmission electron microscopy (STEM) system has been developed. The system employs an FIB/STEM compatible sample rotation holder with a specially designed rotation mechanism, which allows the sample to be rotated 360 degrees [1-3]. This technique was used for the three dimensional (3D) elemental mapping of a contact plug of a Si device in 90 nm technology. A specimen containing a contact plug was shaped to a pillar sample with a cross section of 200 nm x 200 nm and a 5 um length. Elemental analysis was performed with a 200 kV HD-2300 STEM equipped with the EDAX genesis Energy dispersive X-ray spectroscopy (EDX) system. Spectrum imaging combined with multivariate statistical analysis (MSA) [4, 5] was used to enhance the weak X-ray signals of the doped area, which contain a low concentration of As-K. The distributions of elements, especially the dopant As, were successfully enhanced by MSA. The elemental maps were .. reconstructed from the maps.

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