Electron holography of interfaces in electroceramics

1993 ◽  
Vol 51 ◽  
pp. 1088-1089
Author(s):  
Vinayak P. Dravid ◽  
V. Ravikumar ◽  
Richard Plass
Keyword(s):  
Space Charge ◽  
Direct Evidence ◽  
Materials Science ◽  
Theoretical Work ◽  
Electron Holography ◽  
Resolution Limit ◽  
Interference Phenomenon ◽  
X Ray ◽  
Electron Sources ◽  
Science Community

With the advent of coherent electron sources with cold field emission guns (cFEGs), it has become possible to utilize the coherent interference phenomenon and perform “practical” electron holography. Historically, holography was envisioned to extent the resolution limit by compensating coherent aberrations. Indeed such work has been done with reasonable success in a few laboratories around the world. However, it is the ability of electron holography to map electrical and magnetic fields which has caught considerable attention of materials science community.There has been considerable theoretical work on formation of space charge on surfaces and internal interfaces. In particular, formation and nature of space charge have important implications for the performance of numerous electroceramics which derive their useful properties from electrically active grain boundaries. Bonnell and coworkers, in their elegant STM experiments provided the direct evidence for GB space charge and its sign, while Chiang et al. used the indirect but powerful technique of x-ray microchemical profiling across GBs to infer the nature of space charge.

scholarly journals X-Ray Microprobe for the Microcharacterization of Materials

1988 ◽  
Vol 143 ◽  
Author(s):  
C. J. Sparks ◽  
G. E. Ice
Keyword(s):  
Energy Deposition ◽  
Materials Science ◽  
Charged Particles ◽  
Chemical Characterization ◽  
X Rays ◽  
High Brightness ◽  
X Ray ◽  
Electron Sources ◽  
Detectable Concentration ◽  
Low Levels

AbstractThe unique properties of X rays offer many advantages over those of electrons and other charged particles for the microcharacterization of materials. X rays are more efficient in exciting characteristic X-ray fluorescence and produce higher fluorescent signal-to-background ratios than obtained with electrons. Detectable limits for X rays are a few parts per billion which are 10−3 to 10−5 lower than for electrons. Energy deposition in the sample from X rays is 10–3 to 10–4 less than for electrons for the same detectable concentration. High-brightness storage rings, especially in the 7 GeV class with undulators, will have sources as brilliant as the most advanced electron probes. The highly collimated X-ray beams from undulators simplify the X-ray optics required to produce submicron X-ray probes with fluxes comparable to electron sources. Such X-ray microprobes will also produce unprecedentedly low levels of detection in diffraction, EXAFS, Auger, and photoelectron spectroscopies for structural and chemical characterization and elemental identification. These major improvements in microcharacterization capabilities will have wide-ranging ramifications not only in materials science but also in physics, chemistry, geochemistry, biology, and medicine.

XDS: a flexible beamline for X-ray diffraction and spectroscopy at the Brazilian synchrotron

2016 ◽  
Vol 23 (6) ◽  
pp. 1538-1549 ◽  
Author(s):  
F. A. Lima ◽  
M. E. Saleta ◽  
R. J. S. Pagliuca ◽  
M. A. Eleotério ◽  
R. D. Reis ◽  
...  
Keyword(s):  
High Pressures ◽  
Materials Science ◽  
Photon Flux ◽  
X Ray Diffraction ◽  
X Ray ◽  
X Ray Scattering ◽  
Science Community ◽  
Synchrotron Light ◽  
X Ray Absorption ◽  
Photon Source

The majority of the beamlines at the Brazilian Synchrotron Light Source Laboratory (LNLS) use radiation produced in the storage-ring bending magnets and are therefore currently limited in the flux that can be used in the harder part of the X-ray spectrum (above ∼10 keV). A 4 T superconducting multipolar wiggler (SCW) was recently installed at LNLS in order to improve the photon flux above 10 keV and fulfill the demands set by the materials science community. A new multi-purpose beamline was then installed at the LNLS using the SCW as a photon source. The XDS is a flexible beamline operating in the energy range between 5 and 30 keV, designed to perform experiments using absorption, diffraction and scattering techniques. Most of the work performed at the XDS beamline concentrates on X-ray absorption spectroscopy at energies above 18 keV and high-resolution diffraction experiments. More recently, new setups and photon-hungry experiments such as total X-ray scattering, X-ray diffraction under high pressures, resonant X-ray emission spectroscopy, among others, have started to become routine at XDS. Here, the XDS beamline characteristics, performance and a few new experimental possibilities are described.

Electron holography in materials science

1991 ◽  
Vol 49 ◽  
pp. 670-671
Author(s):  
Hannes Lichte ◽  
Edgar Voelkl
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Materials Science ◽  
Fourier Spectrum ◽  
Object Wave ◽  
Electron Holography ◽  
Reconstruction Procedure ◽  
Numerical Reconstruction ◽  
Transmission Electron ◽  
Unique Interpretation

The object wave o(x,y) = a(x,y)exp(iφ(x,y)) at the exit face of the specimen is described by two real functions, i.e. amplitude a(x,y) and phase φ(x,y). In stead of o(x,y), however, in conventional transmission electron microscopy one records only the real intensity I(x,y) of the image wave b(x,y) loosing the image phase. In addition, referred to the object wave, b(x,y) is heavily distorted by the aberrations of the microscope giving rise to loss of resolution. Dealing with strong objects, a unique interpretation of the micrograph in terms of amplitude and phase of the object is not possible. According to Gabor, holography helps in that it records the image wave completely by both amplitude and phase. Subsequently, by means of a numerical reconstruction procedure, b(x,y) is deconvoluted from aberrations to retrieve o(x,y). Likewise, the Fourier spectrum of the object wave is at hand. Without the restrictions sketched above, the investigation of the object can be performed by different reconstruction procedures on one hologram. The holograms were taken by means of a Philips EM420-FEG with an electron biprism at 100 kV.

Energy Dispersive X-Ray Measurements of thin Metal Foils

1976 ◽  
Vol 34 ◽  
pp. 426-427
Author(s):  
J. Bentley ◽  
E. A. Kenik
Keyword(s):  
Materials Science ◽  
Energy Dispersive Spectrometer ◽  
Thin Foil ◽  
Thin Metal ◽  
Energy Dispersive ◽  
Thin Specimen ◽  
X Ray ◽  
Metal Foils ◽  
Small Probe ◽  
Scanning Transmission

Instruments combining a 100 kV transmission electron microscope (TEM) with scanning transmission (STEM), secondary electron (SEM) and x-ray energy dispersive spectrometer (EDS) attachments to give analytical capabilities are becoming increasingly available and useful. Some typical applications in the field of materials science which make use of the small probe size and thin specimen geometry are the chemical analysis of small precipitates contained within a thin foil and the measurement of chemical concentration profiles near microstructural features such as grain boundaries, point defect clusters, dislocations, or precipitates. Quantitative x-ray analysis of bulk samples using EDS on a conventional SEM is reasonably well established, but much less work has been performed on thin metal foils using the higher accelerating voltages available in TEM based instruments.

Evidence for ordered Fe3Ni

1987 ◽  
Vol 45 ◽  
pp. 216-217
Author(s):  
K.B. Reuter ◽  
D.B. Williams ◽  
J.I. Goldstein
Keyword(s):  
Experimental Data ◽  
Martensitic Transformation ◽  
Electron Diffraction ◽  
Room Temperature ◽  
Direct Evidence ◽  
Transformation Product ◽  
Iron Meteorites ◽  
X Ray ◽  
Ni Content ◽  
Temperature Transformation

In the Fe-Ni system, although ordered FeNi and ordered Ni3Fe are experimentally well established, direct evidence for ordered Fe3Ni is unconvincing. Little experimental data for Fe3Ni exists because diffusion is sluggish at temperatures below 400°C and because alloys containing less than 29 wt% Ni undergo a martensitic transformation at room temperature. Fe-Ni phases in iron meteorites were examined in this study because iron meteorites have cooled at slow rates of about 10°C/106 years, allowing phase transformations below 400°C to occur. One low temperature transformation product, called clear taenite 2 (CT2), was of particular interest because it contains less than 30 wtZ Ni and is not martensitic. Because CT2 is only a few microns in size, the structure and Ni content were determined through electron diffraction and x-ray microanalysis. A Philips EM400T operated at 120 kV, equipped with a Tracor Northern 2000 multichannel analyzer, was used.

X-ray microprobe for materials science

1994 ◽  
Vol 52 ◽  
pp. 56-57
Author(s):  
G.E. Ice
Keyword(s):  
Crystallographic Orientation ◽  
Local Structure ◽  
Materials Science ◽  
Chemical Information ◽  
X Ray Diffraction ◽  
Ray Optics ◽  
X Ray ◽  
Novel Materials ◽  
New Information ◽  
Elemental Sensitivity

The increasing availability of synchrotron x-ray sources has stimulated the development of advanced hard x-ray (E≥5 keV) microprobes. With new x-ray optics these microprobes can achieve micron and submicron spatial resolutions. The inherent elemental and crystallographic sensitivity of an x-ray microprobe and its inherently nondestructive and penetrating nature will have important applications to materials science. For example, x-ray fluorescent microanalysis of materials can reveal elemental distributions with greater sensitivity than alternative nondestructive probes. In materials, segregation and nonuniform distributions are the rule rather than the exception. Common interfaces to whichsegregation occurs are surfaces, grain and precipitate boundaries, dislocations, and surfaces formed by defects such as vacancy and interstitial configurations. In addition to chemical information, an x-ray diffraction microprobe can reveal the local structure of a material by detecting its phase, crystallographic orientation and strain.Demonstration experiments have already exploited the penetrating nature of an x-ray microprobe and its inherent elemental sensitivity to provide new information about elemental distributions in novel materials.

X-ray mapping without STEM

1994 ◽  
Vol 52 ◽  
pp. 508-509
Author(s):  
Judith M. Brock ◽  
Max T. Otten
Keyword(s):  
Life Science ◽  
Materials Science ◽  
Chemical Elements ◽  
Full Description ◽  
Scanning System ◽  
Elemental Distribution ◽  
X Ray ◽  
Transmission Electron ◽  
Distribution Of Elements ◽  
Made In

A knowledge of the distribution of chemical elements in a specimen is often highly useful. In materials science specimens features such as grain boundaries and precipitates generally force a certain order on mental distribution, so that a single profile away from the boundary or precipitate gives a full description of all relevant data. No such simplicity can be assumed in life science specimens, where elements can occur various combinations and in different concentrations in tissue. In the latter case a two-dimensional elemental-distribution image is required to describe the material adequately. X-ray mapping provides such of the distribution of elements.The big disadvantage of x-ray mapping hitherto has been one requirement: the transmission electron microscope must have the scanning function. In cases where the STEM functionality – to record scanning images using a variety of STEM detectors – is not used, but only x-ray mapping is intended, a significant investment must still be made in the scanning system: electronics that drive the beam, detectors for generating the scanning images, and monitors for displaying and recording the images.

scholarly journals Solvent-Controlled Self-Assembled Oligopyrrolic Receptor

Molecules ◽  
2021 ◽  
Vol 26 (6) ◽  
pp. 1771
Author(s):  
Fei Wang ◽  
Kejiang Liang ◽  
Mads Christian Larsen ◽  
Steffen Bähring ◽  
Masatoshi Ishida ◽  
...  
Keyword(s):  
Materials Science ◽  
Science Research ◽  
Polymeric Chain ◽  
Supramolecular System ◽  
Receptor System ◽  
One Dimensional ◽  
X Ray ◽  
Host Guest Complex ◽  
Colorimetric Response ◽  
Strong Acids

We report a fully organic pyridine-tetrapyrrolic U-shaped acyclic receptor 10, which prefers a supramolecular pseudo-macrocyclic dimeric structure (10)2 in a less polar, non-coordinating solvent (e.g., CHCl3). Conversely, when it is crystalized from a polar, coordinating solvent (e.g., N,N-dimethylformamide, DMF), it exhibited an infinite supramolecular one-dimensional (1D) “zig-zag” polymeric chain, as inferred from the single-crystal X-ray structures. This supramolecular system acts as a potential receptor for strong acids, e.g., p-toluenesulfonic acid (PTSA), methane sulfonic acid (MSA), H2SO4, HNO3, and HCl, with a prominent colorimetric response from pale yellow to deep red. The receptor can easily be recovered from the organic solution of the host–guest complex by simple aqueous washing. It was observed that relatively stronger acids with pKa < −1.92 in water were able to interact with the receptor, as inferred from 1H NMR titration in tetrahydrofuran-d8 (THF-d8) and ultraviolet–visible (UV–vis) spectroscopic titrations in anhydrous THF at 298 K. Therefore, this new dynamic supramolecular receptor system may have potentiality in materials science research.

scholarly journals Integrated quantitative PIXE analysis and EDX spectroscopy using a laser-driven particle source

2021 ◽  
Vol 7 (3) ◽  
pp. eabc8660
Author(s):  
F. Mirani ◽  
A. Maffini ◽  
F. Casamichiela ◽  
A. Pazzaglia ◽  
A. Formenti ◽  
...  
Keyword(s):  
Experimental Investigation ◽  
Materials Science ◽  
Quantitative Information ◽  
Pixe Analysis ◽  
Materials Analysis ◽  
Particle Source ◽  
X Ray ◽  
Analysis Techniques ◽  
Sample Structure ◽  
Elemental Characterization

Among the existing elemental characterization techniques, particle-induced x-ray emission (PIXE) and energy-dispersive x-ray (EDX) spectroscopy are two of the most widely used in different scientific and technological fields. Here, we present the first quantitative laser-driven PIXE and laser-driven EDX experimental investigation performed at the Centro de Láseres Pulsados in Salamanca. Thanks to their potential for compactness and portability, laser-driven particle sources are very appealing for materials science applications, especially for materials analysis techniques. We demonstrate the possibility to exploit the x-ray signal produced by the co-irradiation with both electrons and protons to identify the elements in the sample. We show that, using the proton beam only, we can successfully obtain quantitative information about the sample structure through laser-driven PIXE analysis. These results pave the way toward the development of a compact and multifunctional apparatus for the elemental analysis of materials based on a laser-driven particle source.

scholarly journals Towards a methodology for the characterisation of the fabric of wet clays using X-ray scattering

2019 ◽  
Vol 92 ◽  
pp. 01005
Author(s):  
Georgios Birmpilis ◽  
Reza Ahmadi-Naghadeh ◽  
Jelke Dijkstra
Keyword(s):  
Materials Science ◽  
Measurement Techniques ◽  
Invasive Technique ◽  
Colloidal Systems ◽  
Characteristic Distance ◽  
X Ray ◽  
Hydrophobic Coating ◽  
X Ray Scattering ◽  
Wide Range ◽  
Ray Scattering

X-ray scattering is a promising non-invasive technique to study evolving nano- and micromechanics in clays. This study discusses the experimental considerations and a successful method to enable X-ray scattering to study clay samples at two extreme stages of consolidation. It is shown that the proposed sample environment comprising flat capillaries with a hydrophobic coating can be used for a wide range of voids ratios ranging from a clay suspension to consolidated clay samples, that are cut from larger specimens of reconstituted or natural clay. The initial X-ray scattering results using a laboratory instrument indicate that valuable information on, in principal evolving, clay fabric can be measured. Features such as characteristic distance between structural units and particle orientations are obtained for a slurry and a consolidated sample of kaolinite. Combined with other promising measurement techniques from Materials Science the proposed method will help advance the contemporary understanding on the behaviour of dense colloidal systems of clay, as it does not require detrimental sample preparation

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