scholarly journals X-ray linear dichroic ptychography

2021 ◽  
Vol 118 (3) ◽  
pp. e2019068118
Author(s):  
Yuan Hung Lo ◽  
Jihan Zhou ◽  
Arjun Rana ◽  
Drew Morrill ◽  
Christian Gentry ◽  
...  
Keyword(s):  
Tooth Enamel ◽  
Phase Imaging ◽  
Crystalline Materials ◽  
X Ray ◽  
Coral Skeletons ◽  
Mineral Growth ◽  
Multiple Length Scales ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Amorphous Nanoparticle

Biominerals such as seashells, coral skeletons, bone, and tooth enamel are optically anisotropic crystalline materials with unique nanoscale and microscale organization that translates into exceptional macroscopic mechanical properties, providing inspiration for engineering new and superior biomimetic structures. Using Seriatopora aculeata coral skeleton as a model, here, we experimentally demonstrate X-ray linear dichroic ptychography and map the c-axis orientations of the aragonite (CaCO3) crystals. Linear dichroic phase imaging at the oxygen K-edge energy shows strong polarization-dependent contrast and reveals the presence of both narrow (<35°) and wide (>35°) c-axis angular spread in the coral samples. These X-ray ptychography results are corroborated by four-dimensional (4D) scanning transmission electron microscopy (STEM) on the same samples. Evidence of co-oriented, but disconnected, corallite subdomains indicates jagged crystal boundaries consistent with formation by amorphous nanoparticle attachment. We expect that the combination of X-ray linear dichroic ptychography and 4D STEM could be an important multimodal tool to study nano-crystallites, interfaces, nucleation, and mineral growth of optically anisotropic materials at multiple length scales.

Scanning Transmission Microscopy Applied to Thick Specimen

1972 ◽  
Vol 30 ◽  
pp. 452-453
Author(s):  
H. Koike ◽  
T. Matsuo ◽  
K. Ueno ◽  
M. Suzuki
Keyword(s):  
Psoas Muscle ◽  
Image Intensifier ◽  
Chromatic Aberration ◽  
Image Contrast ◽  
Transmission Microscopy ◽  
Crystalline Materials ◽  
Thick Specimen ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Electron Microscope Image

Since the identification of single atoms was achieved by Crewe et al, scanning transmission microscopy has been put into pratical use. Recently they applied this method to the quantitative mass analysis of DNA.As pointed out previously the chromatic aberration which decreases the image contrast and quality, does not affect a scanning transmission image as it does a conventional transmission electron microscope image. Thus, the STEM method is advantageous for thick specimen. Further this method employs a high sensitive photomultiplier tube which also functions as an image intensifier. This detection method is effective for the observation of living specimens or easily damaged specimens. In this respect the scanning transmission microscope with high accelerating voltage is necessary.Since Uyeda's experiments of crystalline materials, many workers have been discussed how thick specimens can be observed by CTEM. With biological specimens, R. Szirmae reported on the decrease in the image contrast of rabbit psoas muscle sections at various accelerating voltages and specimen thicknesses.

High-resolution x-ray imaging of small copper-rich precipitates in steels

1988 ◽  
Vol 46 ◽  
pp. 528-529
Author(s):  
J. R. Michael ◽  
K. A. Taylor
Keyword(s):  
Electron Microscopy ◽  
Thermomechanical Processing ◽  
Atom Probe ◽  
Ferrite Matrix ◽  
Scanning Transmission Electron Microscope ◽  
Probe Field ◽  
X Ray ◽  
Subsequent Transformation ◽  
Transmission Electron ◽  
Scanning Transmission

Although copper is considered an incidental or trace element in many commercial steels, some grades contain up to 1-2 wt.% Cu for precipitation strengthening. Previous electron microscopy and atom-probe/field-ion microscopy (AP/FIM) studies indicate that the precipitation of copper from ferrite proceeds with the formation of Cu-rich bcc zones and the subsequent transformation of these zones to fcc copper particles. However, the similarity between the atomic scattering amplitudes for iron and copper and the small misfit between between Cu-rich particles and the ferrite matrix preclude the detection of small (<5 nm) Cu-rich particles by conventional transmission electron microscopy; such particles have been imaged directly only by FIM. Here results are presented whereby the Cu Kα x-ray signal was used in a dedicated scanning transmission electron microscope (STEM) to image small Cu-rich particles in a steel. The capability to detect these small particles is expected to be helpful in understanding the behavior of copper in steels during thermomechanical processing and heat treatment.

Techniques for cryoultramicrotomy of propane jet frozen biological samples

1986 ◽  
Vol 44 ◽  
pp. 260-261
Author(s):  
B. Craig ◽  
L. Hawkey ◽  
A. LeFurgey
Keyword(s):  
Freeze Fracture ◽  
Freeze Substitution ◽  
Heart Cells ◽  
Crystal Formation ◽  
X Ray ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Chick Heart ◽  
Embryonic Chick Heart ◽  
A New Technique

Ultra-rapid freezing followed by cryoultramicrotomy is essential for the preservation of diffusible elements in situ within cells prior to scanning transmission electron microscopy and quantitative energy dispersive x-ray microanalysis. For cells or tissue fragments in suspension and for monolayer cell cultures, propane jet freezing provides cooling rates greater than 30,000°C/sec with regions up to 40μm in thickness free of significant ice crystal formation. While this method of freezing has frequently been applied prior to freeze fracture or freeze substitution, it has not been widely utilized prior to cryoultramicrotomy and subsequent x-ray microanalytical studies. This report describes methods devised in our laboratory for cryosectioning of propane jet frozen kidney proximal tubule suspensions and cultured embryonic chick heart cells, in particular a new technique for mounting frozen suspension specimens for sectioning. The techniques utilize the same specimen supports and sample holders as those used for freeze fracture and freeze substitution and should be generally applicable to any cell suspension or culture preparation.

Magnesium and sulfur in mast cell and basophil granules of lower vertebrates in relation with histamine

1992 ◽  
Vol 50 (2) ◽  
pp. 1596-1597
Author(s):  
Kenichi Takaya
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Mast Cell ◽  
Mast Cells ◽  
Tree Frog ◽  
X Ray ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Fresh Frozen ◽  
Ultrathin Sections

Mast cell and basophil granules of the vertebrate contain heparin or related sulfated proteoglycans. Histamine is also present in mammalian mast cells and basophils. However, no histamine is detected in mast cell granules of the amphibian or fish, while it is shown in those of reptiles and birds A quantitative x-ray microanalysis of mast cell granules of fresh frozen dried ultrathin sections of the tongue of Wistar rats and tree frogs disclosed high concentrations of sulfur in rat mast cell granules and those of sulfur and magnesium in the tree frog granules. Their concentrations in tree frog mast cell granules were closely correlated (r=0.94).Fresh frozen dried ultrathin sections and fresh air-dried prints of the tree frog tongue and spleen and young red-eared turtle (ca. 6 g) spleen and heart blood were examined by a quantitative energy-dispersive x-ray microanalysis (X-650, Kevex-7000) for the element constituents of the granules of mast cells and basophils. The specimens were observed by transmission electron microscopy (TEM) (80-200 kV) and followed by scanning transmission electron microscopy (STEM) under an analytical electron microscope (X-650) at an acceleration voltage of 40 kV and a specimen current of 0.2 nA. A spot analysis was performed in a STEM mode for 100 s at a specimen current of 2 nA on the mast cell and basophil granules and other areas of the cells. Histamine was examined by the o-phthalaldehyde method.

The effect of small additions of Cu on precipitation in Al-Mg-Si alloys

1990 ◽  
Vol 48 (2) ◽  
pp. 442-443
Author(s):  
M. Tamizifar ◽  
G. Cliff ◽  
R.W. Devenish ◽  
G.W. Lorimer
Keyword(s):  
Electron Microscopy ◽  
Analytical Electron Microscopy ◽  
Scanning Transmission Electron Microscope ◽  
Argon Atmosphere ◽  
Age Hardening ◽  
X Ray ◽  
Transmission Electron ◽  
Heat Treated ◽  
Analytical Electron ◽  
Scanning Transmission

Small additions of copper, <1 wt%, have a pronounced effect on the ageing response of Al-Mg-Si alloys. The object of the present investigation was to study the effect of additions of copper up to 0.5 wt% on the ageing response of a series of Al-Mg-Si alloys and to use high resolution analytical electron microscopy to determine the composition of the age hardening precipitates.The composition of the alloys investigated is given in Table 1. The alloys were heat treated in an argon atmosphere for 30m, water quenched and immediately aged either at 180°C for 15 h or given a duplex treatment of 180°C for 15 h followed by 350°C for 2 h2. The double-ageing treatment was similar to that carried out by Dumolt et al. Analyses of the precipitation were carried out with a HB 501 Scanning Transmission Electron Microscope. X-ray peak integrals were converted into weight fractions using the ratio technique of Cliff and Lorimer.

High Spatial Resolution Compositional Analysis at Interfaces

1980 ◽  
Vol 38 ◽  
pp. 356-359
Author(s):  
John B. Vander Sande ◽  
Thomas F. Kelly ◽  
Douglas Imeson
Keyword(s):  
Electron Microscope ◽  
High Spatial Resolution ◽  
Compositional Analysis ◽  
Scanning Transmission Electron Microscope ◽  
Thin Specimen ◽  
X Ray ◽  
Volume Of Interest ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Electron Energy Loss

In the scanning transmission electron microscope (STEM) a fine probe of electrons is scanned across the thin specimen, or the probe is stationarily placed on a volume of interest, and various products of the electron-specimen interaction are then collected and used for image formation or microanalysis. The microanalysis modes usually employed in STEM include, but are not restricted to, energy dispersive X-ray analysis, electron energy loss spectroscopy, and microdiffraction.

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.

scholarly journals Revisiting the Bøggild Intergrowth in Iridescent Labradorite Feldspars: Ordering, Kinetics, and Phase Equilibria

Minerals ◽  
2021 ◽  
Vol 11 (7) ◽  
pp. 727
Author(s):  
Shiyun Jin ◽  
Huifang Xu ◽  
Seungyeol Lee
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Atom Probe ◽  
Phase Region ◽  
Two Phase ◽  
Subsolidus Phase ◽  
Plagioclase Feldspar ◽  
X Ray ◽  
Transmission Electron ◽  
Scanning Transmission

The enigmatic Bøggild intergrowth in iridescent labradorite crystals was revisited in light of recent work on the incommensurately modulated structures in the intermediated plagioclase. Five igneous samples and one metamorphic labradorite sample with various compositions and lamellar thicknesses were studied in this paper. The lamellar textures were characterized with conventional transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM). The compositions of individual lamellae were analyzed with high-resolution energy-dispersive X-ray spectroscopy (EDS) mapping and atom probe tomography (APT). The average structure states of the studied samples were also compared with single-crystal X-ray diffraction data (SC-XRD). The Na-rich lamellae have a composition of An44–48, and the Ca-rich lamellae range from An56 to An63. Significant differences between the lamellar compositions of different samples were observed. The compositions of the Bøggild intergrowth do not only depend on the bulk compositions, but also on the thermal history of the host rock. The implications on the subsolidus phase relationships of the plagioclase feldspar solid solution are discussed. The results cannot be explained by a regular symmetrical solvus such as the Bøggild gap, but they support an inclined two-phase region that closes at low temperature.

scholarly journals Hydrothermal Synthesis of Iridium-Substituted NaTaO3 Perovskites

Nanomaterials ◽  
2021 ◽  
Vol 11 (6) ◽  
pp. 1537
Author(s):  
David L. Burnett ◽  
Christopher D. Vincent ◽  
Jasmine A. Clayton ◽  
Reza J. Kashtiban ◽  
Richard I. Walton
Keyword(s):  
Significant Proportion ◽  
Edge Length ◽  
Perovskite Oxide ◽  
Hydrogen Yield ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
Profile Fitting ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
One Step

Iridium-containing NaTaO3 is produced using a one-step hydrothermal crystallisation from Ta2O5 and IrCl3 in an aqueous solution of 10 M NaOH in 40 vol% H2O2 heated at 240 °C. Although a nominal replacement of 50% of Ta by Ir was attempted, the amount of Ir included in the perovskite oxide was only up to 15 mol%. The materials are formed as crystalline powders comprising cube-shaped crystallites around 100 nm in edge length, as seen by scanning transmission electron microscopy. Energy dispersive X-ray mapping shows an even dispersion of Ir through the crystallites. Profile fitting of powder X-ray diffraction (XRD) shows expanded unit cell volumes (orthorhombic space group Pbnm) compared to the parent NaTaO3, while XANES spectroscopy at the Ir LIII-edge reveals that the highest Ir-content materials contain Ir4+. The inclusion of Ir4+ into the perovskite by replacement of Ta5+ implies the presence of charge-balancing defects and upon heat treatment the iridium is extruded from the perovskite at around 600 C in air, with the presence of metallic iridium seen by in situ powder XRD. The highest Ir-content material was loaded with Pt and examined for photocatalytic evolution of H2 from aqueous methanol. Compared to the parent NaTaO3, the Ir-substituted material shows a more than ten-fold enhancement of hydrogen yield with a significant proportion ascribed to visible light absorption.

Detonation Synthesis of Nano-Size Materials

1995 ◽  
Vol 418 ◽  
Author(s):  
J. Forbes ◽  
J. Davis ◽  
C. Wong
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Nucleation And Growth ◽  
Detonation Synthesis ◽  
X Ray Diffraction ◽  
Crystalline Materials ◽  
X Ray ◽  
Transmission Electron ◽  
Nano Size

AbstractThe detonation of explosives typically creates 100's of kbar pressures and 1000's K temperatures. These pressures and temperatures last for only a fraction of a microsecond as the products expand. Nucleation and growth of crystalline materials can occur under these conditions. Recovery of these materials is difficult but can occur in some circumstances. This paper describes the detonation synthesis facility, recovery of nano-size diamond, and plans to synthesize other nano-size materials by modifying the chemical composition of explosive compounds. The characterization of nano-size diamonds by transmission electron microscopy and electron diffraction, X-ray diffraction and Raman spectroscopy will also be reported.

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