Voltage and Orientation Dependence of Characteristic X-Ray Production in Thin Crystals

Author(s):  
G. Thomas ◽  
K. M. Krishnan ◽  
Y. Yokota ◽  
H. Hashimoto

For crystalline materials, an incident plane wave of electrons under conditions of strong dynamical scattering sets up a standing wave within the crystal. The intensity modulations of this standing wave within the crystal unit cell are a function of the incident beam orientation and the acceleration voltage. As the scattering events (such as inner shell excitations) that lead to characteristic x-ray production are highly localized, the x-ray intensities in turn, are strongly determined by the orientation and the acceleration voltage. For a given acceleration voltage or wavelength of the incident wave, it has been shown that this orientation dependence of the characteristic x-ray emission, termed the “Borrmann effect”, can also be used as a probe for determining specific site occupations of elemental additions in single crystals.

Author(s):  
J. Taftø ◽  
O. L. Krivanek

Bragg reflection of electrons gives rise to a modulation of the wavefield over the crystal unit cell. Depending on the incident beam direction the electrons may be concentrated at one or another type of atoms or between them. Localized ionization processes will therefore show an orientation dependence, and this will affect the X-ray emission intensities as well as electron energy loss spectra. The energy loss case gives more possibilities for experimental arrangements than the X-ray emission case, in that the direction of not only the incident electron beam, but also that of the exit beam to be analyzed may be selected.Natural MgAl2O4 spinel was studied. The crystals were ground in a mortar and thin areas were analyzed with a Gatan 607 spectrometer attached to a Philips 400T electron microscope operating at lOOkV. The experiments were done for the (400)-planar case where the main atomic planes contain Al2O4. The Mg-atoms are midway between the A12O4 and may be considered as interstitials in this planar case.


1986 ◽  
Vol 53 (4) ◽  
pp. 339-348 ◽  
Author(s):  
Kannan M. Krishnan ◽  
Peter Rez ◽  
Gareth Thomas ◽  
Yasuhiro Yokota ◽  
H. Hashimoto

2018 ◽  
Vol 74 (6) ◽  
pp. 673-680 ◽  
Author(s):  
V. G. Kohn

The article reports an accurate theory of X-ray coplanar multiple diffraction for an experimental setup that consists of a generic synchrotron radiation (SR) source, double-crystal monochromator (M) and slit (S). It is called for brevity the theory of X-ray coplanar multiple SRMS diffractometry. The theory takes into account the properties of synchrotron radiation as well as the features of diffraction of radiation in the monochromator crystals and the slit. It is shown that the angular and energy dependence (AED) of the sample reflectivity registered by a detector has the form of a convolution of the AED in the case of the monochromatic plane wave with the instrumental function which describes the angular and energy spectrum of radiation incident on the sample crystal. It is shown that such a scheme allows one to measure the rocking curves close to the case of the monochromatic incident plane wave, but only using the high-order reflections by monochromator crystals. The case of four-beam (220)(331)({\overline {11}}1) diffraction in Si is considered in detail.


2001 ◽  
Vol 7 (S2) ◽  
pp. 342-343
Author(s):  
S. Köstlmeier ◽  
S. Nufer ◽  
T. Gemming ◽  
M. Rühle

The orientation dependence of the fine structure of the Al L1 and L2,3 electron energy loss (EELS) edges in (α-Al2O3 has been investigated by measurements with a dedicated scanning transmission electron microscope (VG HB501 STEM, 100 keV acceleration voltage). α-Al2O3 is an anisotropic solid with a complicated alternating stacking sequence of fee Al and hcp O planes along the [0001] direction [1]. This distingiushes the [0001] direction crystallographically, as the highest-order three-fold rotation axes (C3) of the trigonal crystal structure are parallel to [0001], whereas all other symmetry elements are of lower order. Group theory predicts, that more stringent symmetry selection rules apply when electronic transitions are excited by irradiation parallel to the low-index [0001] zone axis than by irradiation along any other arbitrary direction.Yet, even for a low-energy EELS edge (θE = 0.4 mrad) both scattering parallel and perpendicular to the incident beam direction are likely.


Author(s):  
C. S. Pande ◽  
R. L. Sabatini

The dependence of characteristic, electron induced, x-ray production on beam orientation in crystalline solids has been predicted theoretically and observed experimentally by many researchers. This effect is analogous to the Borrmann effect in x-rays. The plane electron wave entering the crystal generates Bloch waves with nodes or antinodes at the center of the atoms. The amplitude of the Bloch waves depends upon the orientation, resulting in a variation in current density over the unit cell with incident beam direction. This effect is important when measuring chemical compositions in thin films of alloys (ordered and disordered) by energy dispersive x-ray analysis or by energy loss analysis. It has so far been tacitly assumed that if thin film criteria is satisfied, this orientation effect is negligible (if not too close to a Bragg reflection).


Author(s):  
P.E. Batson ◽  
C.R.M. Grovenor ◽  
D.A. Smith ◽  
C. Wong

In this work As doped polysilicon was deposited onto (100) silicon wafers by APCVD at 660°C from a silane-arsine mixture, followed by a ten minute anneal at 1000°C, and in one case a further ten minute anneal at 700°C. Specimens for TEM and STEM analysis were prepared by chemical polishing. The microstructure, which is unchanged by the final 700°C anneal,is shown in Figure 1. It consists of numerous randomly oriented grains many of which contain twins.X-ray analysis was carried out in a VG HB5 STEM. As K α x-ray counts were collected from STEM scans across grain and twin boundaries, Figures 2-4. The incident beam size was about 1.5nm in diameter, and each of the 20 channels in the plots was sampled from a 1.6nm length of the approximately 30nm line scan across the boundary. The bright field image profile along the scanned line was monitored during the analysis to allow correlation between the image and the x-ray signal.


Author(s):  
N. J. Zaluzec

The ultimate sensitivity of microchemical analysis using x-ray emission rests in selecting those experimental conditions which will maximize the measured peak-to-background (P/B) ratio. This paper presents the results of calculations aimed at determining the influence of incident beam energy, detector/specimen geometry and specimen composition on the P/B ratio for ideally thin samples (i.e., the effects of scattering and absorption are considered negligible). As such it is assumed that the complications resulting from system peaks, bremsstrahlung fluorescence, electron tails and specimen contamination have been eliminated and that one needs only to consider the physics of the generation/emission process.The number of characteristic x-ray photons (Ip) emitted from a thin foil of thickness dt into the solid angle dΩ is given by the well-known equation


Author(s):  
B. B. Chang ◽  
D. F. Parsons

The significance of dynamical scattering effects remains the major question in the structural analysis by electron diffraction of protein crystals preserved in the hydrated state. In the few cases (single layers of purple membrane and 400-600 Å thick catalase crystals examined at 100 kV acceleration voltage) where electron-diffraction patterns were used quantitatively, dynamical scattering effects were considered unimportant on the basis of a comparison with x-ray intensities. The kinematical treatment is usually justified by the thinness of the crystal. A theoretical investigation by Ho et al. using Cowley-Moodie multislice formulation of dynamical scattering theory and cytochrome b5as the test object2 suggests that kinematical analysis of electron diffraction data with 100-keV electrons would not likely be valid for specimen thickness of 300 Å or more. We have chosen to work with electron diffraction patterns obtained from actual wet protein crystals (rat hemoglobin crystals of thickness range 1000 to 2500 Å) at 200 and 1000 kV and to analyze these for dynamical effects.


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