The Effect of Specimen Thickness and Probe Size on Aem Analysis of Cr-Depletion Profiles in Sensitized Stainless Steel

1982 ◽  
Vol 40 ◽  
pp. 518-519
Author(s):  
E. L. Hall
Keyword(s):  
Grain Boundaries ◽  
Boundary Region ◽  
Chromium Concentration ◽  
Foil Thickness ◽  
Specimen Thickness ◽  
Probe Size ◽  
Analytical Electron ◽  
Analytical Electron Microscope ◽  
Sensitization Process ◽  
Compositional Gradients

Sensitization in stainless steels is caused by the formation of chromium-rich M23C6 carbides at grain boundaries, which depletes the adjacent matrix and boundary region of chromium, and hence leads to rapid intergranular attack. To fully understand the sensitization process, and to test the accuracy of theories proposed to model this process, it is necessary to obtain very accurate measurements of the chromium concentration at grain boundaries in sensitized specimens. Quantitative X-ray spectroscopy in the analytical electron microscope (AEM) enables the chromium concentration profile across these boundaries to be studied directly; however, it has been shown that a strong effect of foil thickness and electron probe size may be present in the analysis of rapidly-changing compositional gradients. The goal of this work is to examine these effects.

Resolution of a Transmitted Electron Image Formed by A Scanning Electron Microscope

1970 ◽  
Vol 28 ◽  
pp. 386-387
Author(s):  
S. Takashima ◽  
H. Hashimoto ◽  
S. Kimoto
Keyword(s):  
Electron Microscope ◽  
Scanning Electron Microscope ◽  
Chromatic Aberration ◽  
Objective Lens ◽  
Specimen Thickness ◽  
Probe Diameter ◽  
Transmission Electron ◽  
Electron Image ◽  
Conventional Transmission Electron Microscope ◽  
Scanning Electron

The resolution of a conventional transmission electron microscope (TEM) deteriorates as the specimen thickness increases, because chromatic aberration of the objective lens is caused by the energy loss of electrons). In the case of a scanning electron microscope (SEM), chromatic aberration does not exist as the restrictive factor for the resolution of the transmitted electron image, for the SEM has no imageforming lens. It is not sure, however, that the equal resolution to the probe diameter can be obtained in the case of a thick specimen. To study the relation between the specimen thickness and the resolution of the trans-mitted electron image obtained by the SEM, the following experiment was carried out.

A New 1000kv Electron Microscope

1969 ◽  
Vol 27 ◽  
pp. 100-101
Author(s):  
J.L. Williams ◽  
K. Heathcote ◽  
E.J. Greer
Keyword(s):  
Electron Microscope ◽  
Direct Observation ◽  
High Voltage ◽  
Three Dimensional ◽  
Dimensional Structure ◽  
Specimen Thickness ◽  
Voltage Electron ◽  
High Voltage Electron Microscope ◽  
Dynamic Experiments ◽  
Conventional Instrument

High Voltage Electron Microscope already offers exciting experimental possibilities to Biologists and Materials Scientists because the increased specimen thickness allows direct observation of three dimensional structure and dynamic experiments on effectively bulk specimens. This microscope is designed to give maximum accessibility and space in the specimen region for the special stages which are required. At the same time it provides an ease of operation similar to a conventional instrument.

Spatial resolution of X-ray microanalysis in thin foils

1978 ◽  
Vol 36 (1) ◽  
pp. 544-545
Author(s):  
R. Hutchings ◽  
I.P. Jones ◽  
M.H. Loretto ◽  
R.E. Smallman
Keyword(s):  
Spatial Resolution ◽  
Electron Probe ◽  
Beam Divergence ◽  
Inelastic Interaction ◽  
Specimen Thickness ◽  
High Current ◽  
Beam Spreading ◽  
X Ray ◽  
Thin Foils ◽  
Complex Calculation

There is increasing interest in X-ray microanalysis of thin specimens and the present paper attempts to define some of the factors which govern the spatial resolution of this type of microanalysis. One of these factors is the spreading of the electron probe as it is transmitted through the specimen. There will always be some beam-spreading with small electron probes, because of the inevitable beam divergence associated with small, high current probes; a lower limit to the spatial resolution is thus 2αst where 2αs is the beam divergence and t the specimen thickness.In addition there will of course be beam spreading caused by elastic and inelastic interaction between the electron beam and the specimen. The angle through which electrons are scattered by the various scattering processes can vary from zero to 180° and it is clearly a very complex calculation to determine the effective size of the beam as it propagates through the specimen.

Absolute inner-shell cross section determination for EELS analysis

1988 ◽  
Vol 46 ◽  
pp. 534-535
Author(s):  
P.A. Crozier
Keyword(s):  
Cross Section ◽  
Cross Sections ◽  
Absolute Cross Section ◽  
Specimen Thickness ◽  
Mass Thickness ◽  
Scattering Cross ◽  
Before And After ◽  
Estimated Error ◽  
Scattering Cross Sections ◽  
Electron Microscopist

Absolute inelastic scattering cross sections or mean free paths are often used in EELS analysis for determining elemental concentrations and specimen thickness. In most instances, theoretical values must be used because there have been few attempts to determine experimental scattering cross sections from solids under the conditions of interest to electron microscopist. In addition to providing data for spectral quantitation, absolute cross section measurements yields useful information on many of the approximations which are frequently involved in EELS analysis procedures. In this paper, experimental cross sections are presented for some inner-shell edges of Al, Cu, Ag and Au.Uniform thin films of the previously mentioned materials were prepared by vacuum evaporation onto microscope cover slips. The cover slips were weighed before and after evaporation to determine the mass thickness of the films. The estimated error in this method of determining mass thickness was ±7 x 107g/cm2. The films were floated off in water and mounted on Cu grids.

Experimental Determination of the Effective Resolution Limit in Thick Specimens at High Voltages

1975 ◽  
Vol 33 ◽  
pp. 664-665
Author(s):  
Mircea Fotino
Keyword(s):  
Experimental Approach ◽  
Chromatic Aberration ◽  
Resolving Power ◽  
Biological Research ◽  
Specimen Thickness ◽  
Resolution Limit ◽  
High Voltage Electron Microscopy ◽  
Voltage Electron ◽  
Resolution Level

The use of thick specimens (0.5 μm to 5.0 μm or more) is one of the most resourceful applications of high-voltage electron microscopy in biological research. However, the energy loss experienced by the electron beam in the specimen results in chromatic aberration and thus in a deterioration of the effective resolving power. This sets a limit to the maximum usable specimen thickness when investigating structures requiring a certain resolution level.An experimental approach is here described in which the deterioration of the resolving power as a function of specimen thickness is determined. In a manner similar to the Rayleigh criterion in which two image points are considered resolved at the resolution limit when their profiles overlap such that the minimum of one coincides with the maximum of the other, the resolution attainable in thick sections can be measured by the distance from minimum to maximum (or, equivalently, from 10% to 90% maximum) of the broadened profile of a well-defined step-like object placed on the specimen.

The effect of temperature on high-resolution TEM image contrast

1995 ◽  
Vol 53 ◽  
pp. 640-641
Author(s):  
T. Geipel ◽  
W. Mader ◽  
P. Pirouz
Keyword(s):  
Form Factor ◽  
Inelastic Scattering ◽  
Accurate Method ◽  
Waller Factor ◽  
Effect Of Temperature ◽  
Specimen Thickness ◽  
Influence Of Temperature ◽  
Debye Waller Factor ◽  
Influence Of Temperature On ◽  
Atomic Form Factor

Temperature affects both elastic and inelastic scattering of electrons in a crystal. The Debye-Waller factor, B, describes the influence of temperature on the elastic scattering of electrons, whereas the imaginary part of the (complex) atomic form factor, fc = fr + ifi, describes the influence of temperature on the inelastic scattering of electrons (i.e. absorption). In HRTEM simulations, two possible ways to include absorption are: (i) an approximate method in which absorption is described by a phenomenological constant, μ, i.e. fi; - μfr, with the real part of the atomic form factor, fr, obtained from Hartree-Fock calculations, (ii) a more accurate method in which the absorptive components, fi of the atomic form factor are explicitly calculated. In this contribution, the inclusion of both the Debye-Waller factor and absorption on HRTEM images of a (Oll)-oriented GaAs crystal are presented (using the EMS software.Fig. 1 shows the the amplitudes and phases of the dominant 111 beams as a function of the specimen thickness, t, for the cases when μ = 0 (i.e. no absorption, solid line) and μ = 0.1 (with absorption, dashed line).

Comparison of Calculated and Recorded Electron Energy-Loss Spectra of Aluminium and Carbon

1990 ◽  
Vol 48 (2) ◽  
pp. 64-65
Author(s):  
L. Reimer ◽  
R. Oelgeklaus
Keyword(s):  
Fourier Transform ◽  
Energy Loss ◽  
Electron Energy ◽  
Rotational Symmetry ◽  
Mean Free Path ◽  
Single Scattering ◽  
Specimen Thickness ◽  
Two Dimensional ◽  
Image Position ◽  
Electron Energy Loss

Quantitative electron energy-loss spectroscopy (EELS) needs a correction for the limited collection aperture α and a deconvolution of recorded spectra for eliminating the influence of multiple inelastic scattering. Reversely, it is of interest to calculate the influence of multiple scattering on EELS. The distribution f(w,θ,z) of scattered electrons as a function of energy loss w, scattering angle θ and reduced specimen thickness z=t/Λ (Λ=total mean-free-path) can either be recorded by angular-resolved EELS or calculated by a convolution of a normalized single-scattering function ϕ(w,θ). For rotational symmetry in angle (amorphous or polycrystalline specimens) this can be realised by the following sequence of operations :(1)where the two-dimensional distribution in angle is reduced to a one-dimensional function by a projection P, T is a two-dimensional Fourier transform in angle θ and energy loss w and the exponent -1 indicates a deprojection and inverse Fourier transform, respectively.

Thickness Measurement in the AEM by Macintosh-Based Analysis of Two-Beam Convergent Beam Patterns

1990 ◽  
Vol 48 (2) ◽  
pp. 504-505
Author(s):  
John F. Mansfield ◽  
Douglas C. Crawford
Keyword(s):  
Electron Microscope ◽  
Video Camera ◽  
Thickness Measurement ◽  
Specimen Thickness ◽  
Crystalline Materials ◽  
Beam Dynamic ◽  
Line Measurement ◽  
On Line ◽  
Image Position ◽  
Convergent Beam

A method has been developed that allows on-line measurement of the thickness of crystalline materials in the analytical electron microscope. Two-beam convergent beam electron diffraction (CBED) patterns are digitized from a JEOL 2000FX electron microscope into an Apple Macintosh II microcomputer via a Gatan #673 CCD Video Camera and an Imaging Systems Technology Video 1000 frame-capture board. It is necessary to know the lattice parameters of the sample since measurements are made of the spacing of the diffraction discs in order to calibrate the pattern. The sample thickness is calculated from measurements of the spacings of the fringes that are seen in the diffraction discs. This technique was pioneered by Kelly et al, who used the two-beam dynamic theory of MacGillavry relate the deviation parameter (Si) of the ith fringe from the exact Bragg condition to the specimen thickness (t) with the equation:Where ξg, is the extinction distance for that reflection and ni is an integer.

Problems in Thin-Film X-ray Quantification

1990 ◽  
Vol 48 (2) ◽  
pp. 458-459
Author(s):  
J N Chapman ◽  
W A P Nicholson
Keyword(s):  
Thin Film ◽  
Specimen Thickness ◽  
X Rays ◽  
Characteristic Peak ◽  
Local Composition ◽  
X Ray ◽  
Measured Ratio ◽  
Path Lengths ◽  
Composition Changes

Energy dispersive x-ray microanalysis (EDX) is widely used for the quantitative determination of local composition in thin film specimens. Extraction of quantitative data is usually accomplished by relating the ratio of the number of atoms of two species A and B in the volume excited by the electron beam (nA/nB) to the corresponding ratio of detected characteristic photons (NA/NB) through the use of a k-factor. This leads to an expression of the form nA/nB = kAB NA/NB where kAB is a measure of the relative efficiency with which x-rays are generated and detected from the two species.Errors in thin film x-ray quantification can arise from uncertainties in both NA/NB and kAB. In addition to the inevitable statistical errors, particularly severe problems arise in accurately determining the former if (i) mass loss occurs during spectrum acquisition so that the composition changes as irradiation proceeds, (ii) the characteristic peak from one of the minority components of interest is overlapped by the much larger peak from a majority component, (iii) the measured ratio varies significantly with specimen thickness as a result of electron channeling, or (iv) varying absorption corrections are required due to photons generated at different points having to traverse different path lengths through specimens of irregular and unknown topography on their way to the detector.

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