Chemical Species Identification in an SEM by Changes in Emitted X-Ray Energies

Author(s):  
R. H. Duff

A material irradiated with electrons emits x-rays having energies characteristic of the elements present. Chemical combination between elements results in a small shift of the peak energies of these characteristic x-rays because chemical bonds between different elements have different energies. The energy differences of the characteristic x-rays resulting from valence electron transitions can be used to identify the chemical species present and to obtain information about the chemical bond itself. Although these peak-energy shifts have been well known for a number of years, their use for chemical-species identification in small volumes of material was not realized until the development of the electron microprobe.

1995 ◽  
Vol 417 ◽  
Author(s):  
Hiroyuki Fujiwara ◽  
Toshihiro Ii ◽  
Isamu Shimizu

AbstractHigh-quality (ZnS)n(ZnSe)12n and (ZnSe)n(ZnTe)11n (n=1∼4) crystals were grown at a low temperature of 200°C by hydrogen radical-enhanced chemical vapor deposition. From satellite peaks in x-ray diffraction spectra, these periodic structure crystals were confirmed to be grown coherently on substrates, in spite of large lattice mismatches between the grown layers and the substrates (͛=4∼7%). In photoluminescence (PL) spectra of these films, strong band-edge emissions were predominantly observed, resulting from a suppression of deep-level emissions. We found that the PL peak energy of (ZnSe)n(ZnTe)11n shifts systematically to lower energy by 200 meV with changes in the number of ZnSe layers (n), while relatively small shift of 13 meV was observed in (ZnS)n(ZnSe)12n. These discrepancy can be attributed to the difference of band-lineups or chemical natures of constituent atoms in these crystals.


2014 ◽  
Vol 228 (10-12) ◽  
Author(s):  
Thomas Gorniak ◽  
Axel Rosenhahn

AbstractImaging is one of the key drivers for new scientific insights – from the observation of distant stars in astronomy to microscopic studies of sub-cellular structures in biology. In the latter case, X-rays are a versatile probe due to their small wavelength and thus high spatial sensitivity. We give an overview of applicable lensless, coherent imaging approaches relying on scattering with a focus on ptychographic microscopy and discuss the experimental requirements for the soft X-ray scattering experiment HORST. Besides the experiment itself, we highlight the importance of sample environments, especially when biological specimens are investigated. Here, the water window is of central importance. In addition to exploitation of the contrast and resolution, resonant ptychography allows to distinguish chemical species at high spatial resolution with both phase and amplitude contrast.


An interesting way in which an excited atom can emit its excess energy has been brought to light by the experiments of Robinson and of Auger. If, for example, an atom is ionised in the K state, then it may emit a quantum of radiation of some line of its K X-ray spectrum by means of a transition of an electron to the K level, but as an alternative method it may emit an electron instead, thus leaving the atom doubly ionised. One such process might be represented as [L I → K, L II → ∝] and the energy E of the ejected electron would be given by E = K abs — L Iabs — L IIabs — δ, where δ is a small correcting term to take into account that the work required to remove an electron from an ionised atom is slightly greater than that necessary in the case of a normal atom. Processes of this kind are essentially different from those giving rise to radiation since two electrons instead of one are concerned in the transition. The entire process must be considered as occurring simultaneously, and, to take as an example the case already mentioned, it has no meaning to attempt to state whether it is an L I electron which goes to the K state, and an L II electron which is ejected or vice versa . Two points of interest in this phenomenon are the investigation of the magnitude of the correction term δ, and of the relative probabilities of the different types of transition. It will be seen later that the possible transitions are considerably more numerous than with single electron transitions which give rise to radiation. This phenomenon has been studied by Robinson by analysing the ejected electrons with a magnetic field. A thin layer of the element under investigation is placed in the position of the source in the well-known semi-circular focussing apparatus, and is irradiated with X-rays of sufficiently high frequency to be able to eject electrons from the K state. There then follows a further electronic emission from these ionised atoms in the manner already described. Both sets of electrons are recorded photographically, and the various groups show up as lines or narrow bands on the photographic plate. A difficulty inherent in the nature of the experiment is that the groups of homogeneous electrons become slightly diffuse in emerging from the target which must have a certain thickness in order to yield groups of reasonable intensity.


2018 ◽  
Vol 616 ◽  
pp. A138 ◽  
Author(s):  
G. Oganesyan ◽  
L. Nava ◽  
G. Ghirlanda ◽  
A. Celotti

Detection of prompt emission by Swift-XRT provides a unique tool to study how the prompt spectrum of gamma-ray bursts (GRBs) extends down to the soft X-ray band. This energy band is particularly important for prompt emission studies, since it is towards low energies that the observed spectral shape is in disagreement with the synchrotron predictions. Unfortunately, the number of cases where XRT started observing the GRB location during the prompt phase is very limited. In this work, we collect a sample of 34 GRBs and perform joint XRT+BAT spectral analysis of prompt radiation, extending a previous study focused on the 14 brightest cases. Fermi-GBM observations are included in the analysis when available (11 cases), allowing the characterization of prompt spectra from soft X-rays to MeV energies. In 62% of the spectra, the XRT data reveal a hardening of the spectrum, well described by introducing an additional, low-energy power-law segment (with index α1) into the empirical fitting function. The break energy below which the spectrum hardens has values between 3 keV and 22 keV. A second power-law (α2) describes the spectrum between the break energy and the peak energy. The mean values of the photon indices are 〈α1〉 = −0.51 (σ = 0.24) and 〈α2〉 = −1.56 (σ = 0.26). These are consistent, within one σ, with the synchrotron values in fast cooling regime. As a test, if we exclude XRT data from the fits we find typical results: the spectrum below the peak energy is described by a power law with 〈α〉 = −1.15. This shows the relevance of soft X-ray data in revealing prompt emission spectra consistent with synchrotron spectra. Finally, we do not find any correlation between the presence of the X-ray break energy and the flux, fluence, or duration of the prompt emission.


2020 ◽  
Vol 6 (37) ◽  
pp. eabb3615 ◽  
Author(s):  
A. Pattammattel ◽  
R. Tappero ◽  
M. Ge ◽  
Y. S. Chu ◽  
X. Huang ◽  
...  

Resolving chemical species at the nanoscale is of paramount importance to many scientific and technological developments across a broad spectrum of disciplines. Hard x-rays with excellent penetration power and high chemical sensitivity are suitable for speciation of heterogeneous (thick) materials. Here, we report nanoscale chemical speciation by combining scanning nanoprobe and fluorescence-yield x-ray absorption near-edge structure (nano-XANES). First, the resolving power of nano-XANES was demonstrated by mapping Fe(0) and Fe(III) states of a reference sample composed of stainless steel and hematite nanoparticles with 50-nm scanning steps. Nano-XANES was then used to study the trace secondary phases in lithium iron phosphate (LFP) particles. We observed individual Fe-phosphide nanoparticles in pristine LFP, whereas partially (de)lithiated particles showed Fe-phosphide nanonetworks. These findings shed light on the contradictory reports on Fe-phosphide morphology in the literature. Nano-XANES bridges the capability gap of spectromicroscopy methods and provides exciting research opportunities across multiple disciplines.


1993 ◽  
Vol 03 (02) ◽  
pp. 177-183 ◽  
Author(s):  
J. Iihara ◽  
J. Kawai ◽  
T. Sekine ◽  
K. Yoshihara

Si K x-ray spectra in SiO 2- Na 2 O were measured with a double-crystal spectrometer. Remarkable change of peak energy, FWHM and intensity were found, depending on sodium contents. Theoretical spectra of Si K β x-ray were calculated to explain the change of x-ray intensity.


1994 ◽  
Vol 144 ◽  
pp. 82
Author(s):  
E. Hildner

AbstractOver the last twenty years, orbiting coronagraphs have vastly increased the amount of observational material for the whitelight corona. Spanning almost two solar cycles, and augmented by ground-based K-coronameter, emission-line, and eclipse observations, these data allow us to assess,inter alia: the typical and atypical behavior of the corona; how the corona evolves on time scales from minutes to a decade; and (in some respects) the relation between photospheric, coronal, and interplanetary features. This talk will review recent results on these three topics. A remark or two will attempt to relate the whitelight corona between 1.5 and 6 R⊙to the corona seen at lower altitudes in soft X-rays (e.g., with Yohkoh). The whitelight emission depends only on integrated electron density independent of temperature, whereas the soft X-ray emission depends upon the integral of electron density squared times a temperature function. The properties of coronal mass ejections (CMEs) will be reviewed briefly and their relationships to other solar and interplanetary phenomena will be noted.


Author(s):  
E. A. Kenik ◽  
J. Bentley

Cliff and Lorimer (1) have proposed a simple approach to thin foil x-ray analy sis based on the ratio of x-ray peak intensities. However, there are several experimental pitfalls which must be recognized in obtaining the desired x-ray intensities. Undesirable x-ray induced fluorescence of the specimen can result from various mechanisms and leads to x-ray intensities not characteristic of electron excitation and further results in incorrect intensity ratios.In measuring the x-ray intensity ratio for NiAl as a function of foil thickness, Zaluzec and Fraser (2) found the ratio was not constant for thicknesses where absorption could be neglected. They demonstrated that this effect originated from x-ray induced fluorescence by blocking the beam with lead foil. The primary x-rays arise in the illumination system and result in varying intensity ratios and a finite x-ray spectrum even when the specimen is not intercepting the electron beam, an ‘in-hole’ spectrum. We have developed a second technique for detecting x-ray induced fluorescence based on the magnitude of the ‘in-hole’ spectrum with different filament emission currents and condenser apertures.


Author(s):  
W. Brünger

Reconstructive tomography is a new technique in diagnostic radiology for imaging cross-sectional planes of the human body /1/. A collimated beam of X-rays is scanned through a thin slice of the body and the transmitted intensity is recorded by a detector giving a linear shadow graph or projection (see fig. 1). Many of these projections at different angles are used to reconstruct the body-layer, usually with the aid of a computer. The picture element size of present tomographic scanners is approximately 1.1 mm2.Micro tomography can be realized using the very fine X-ray source generated by the focused electron beam of a scanning electron microscope (see fig. 2). The translation of the X-ray source is done by a line scan of the electron beam on a polished target surface /2/. Projections at different angles are produced by rotating the object.During the registration of a single scan the electron beam is deflected in one direction only, while both deflections are operating in the display tube.


Author(s):  
L. T. Germinario

Understanding the role of metal cluster composition in determining catalytic selectivity and activity is of major interest in heterogeneous catalysis. The electron microscope is well established as a powerful tool for ultrastructural and compositional characterization of support and catalyst. Because the spatial resolution of x-ray microanalysis is defined by the smallest beam diameter into which the required number of electrons can be focused, the dedicated STEM with FEG is the instrument of choice. The main sources of errors in energy dispersive x-ray analysis (EDS) are: (1) beam-induced changes in specimen composition, (2) specimen drift, (3) instrumental factors which produce background radiation, and (4) basic statistical limitations which result in the detection of a finite number of x-ray photons. Digital beam techniques have been described for supported single-element metal clusters with spatial resolutions of about 10 nm. However, the detection of spurious characteristic x-rays away from catalyst particles produced images requiring several image processing steps.


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