Optimizing conditions for x-ray microchemical analysis in analytical electron microscopy

1978 ◽  
Vol 36 (1) ◽  
pp. 548-549 ◽  
Author(s):  
N. J. Zaluzec
Keyword(s):  
Solid Angle ◽  
Analytical Electron Microscopy ◽  
Incident Beam ◽  
Thin Foil ◽  
Experimental Conditions ◽  
X Ray ◽  
Microchemical Analysis ◽  
Analytical Electron ◽  
Image Position ◽  
Incident Beam Energy

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

Analytical Formulae for Calculation of X-Ray Detector Solid Angles in the Scanning and Scanning/Transmission Analytical Electron Microscope

2014 ◽  
Vol 20 (4) ◽  
pp. 1318-1326 ◽  
Author(s):  
Nestor J. Zaluzec
Keyword(s):  
Electron Microscopy ◽  
Electron Microscope ◽  
Solid Angle ◽  
Analytical Electron Microscopy ◽  
X Ray ◽  
Analytical Electron ◽  
Analytical Electron Microscope ◽  
Scanning Transmission ◽  
Analytical Formulae ◽  
Detector Configurations

AbstractClosed form analytical equations used to calculate the collection solid angle of six common geometries of solid-state X-ray detectors in scanning and scanning/transmission analytical electron microscopy are presented. Using these formulae one can make realistic comparisons of the merits of the different detector geometries in modern electron column instruments. This work updates earlier formulations and adds new detector configurations.

Diffusion Measurements by Analytical Electron Microscopy

1985 ◽  
Vol 62 ◽  
Author(s):  
A. D. Romig
Keyword(s):  
Electron Microprobe ◽  
Analytical Electron Microscopy ◽  
Thin Foil ◽  
Diffusion Couples ◽  
Concentration Gradients ◽  
X Ray ◽  
Analytical Electron ◽  
Multiphase Diffusion ◽  
Better Than

ABSTRACTThe analytical electron microscope (AEM) has been used to measure the concentration gradients which form in single and multiphase diffusion couples. The procedures used to collect x-ray microanalytical data and reduce that data to elemental compositions are typical of those used to quantify x-ray data generated in thin films. The primary difficulty in analyzing diffusion couples with the AEM is sample preparation. The principle advantage of the AEM as a tool to measure diffusion induced concentration gradients is its high spatial resolution, approximately 20 to 100 times better than that of the electron microprobe which has been traditionally used to measure these concentration profiles. As a consequence, the AEM data can yield diffusivities as much as 5 orders of magnitude smaller than those obtained from electron microprobe data. This paper will review the fundamental principles of the determination of diffusion coefficients from the concentration gradients measured in single and multiphase diffusion couples and the basic considerations of thin foil x-ray microanalysis. With this understanding of the basic concepts, recent studies of diffusion in Ta-W and U-Nb will be discussed.

The standard hole-count test: A progress report

1991 ◽  
Vol 49 ◽  
pp. 720-721
Author(s):  
C. E. Lyman ◽  
D. W. Ackland
Keyword(s):  
Standard Specimen ◽  
Analytical Electron Microscopy ◽  
Thin Foil ◽  
X Rays ◽  
Absolute Value ◽  
X Ray ◽  
Disk Specimen ◽  
Illumination System ◽  
Analytical Electron ◽  
Order Of Magnitude

Analytical electron microscopy (AEM) was well served by the original hole count test that prompted microscope manufacturers to reduce, by an order of magnitude, spurious x-ray generation in the specimen. This spurious x-ray signal is caused by hard x-rays or uncollimated electrons from the illumination system and is typically generated over the entire specimen regardless of where the electron probe is placed for analysis. The original test was performed on an ion-milled thin foil disk specimen of Ag or Mo, but the absolute value of hole count was dependent upon both specimen and operator. To make progress in die reduction of spurious xrays at intermediate voltages (if the problem is present), a hole-count test on a standard specimen that does not require operator judgement would be useful. The ultimate goal would be to reduce spurious x-rays to a level that would not affect any experiment on any specimen.

Analytical Electron Microscopy (AEM) of Meningeal Cells Exposed to Particulate Cobalt During Studies of Experimental Epilepsy

1982 ◽  
Vol 40 ◽  
pp. 186-187
Author(s):  
R.G. Frederickson ◽  
R.G. Ulrich ◽  
J.L. Culberson
Keyword(s):  
Electron Microscopy ◽  
Analytical Electron Microscopy ◽  
Experimental Epilepsy ◽  
Metallic Cobalt ◽  
Experimental Animals ◽  
X Ray ◽  
Brain Surface ◽  
Meningeal Cells ◽  
Analytical Electron ◽  
The Brain

Metallic cobalt acts as an epileptogenic agent when placed on the brain surface of some experimental animals. The mechanism by which this substance produces abnormal neuronal discharge is unknown. One potentially useful approach to this problem is to study the cellular and extracellular distribution of elemental cobalt in the meninges and adjacent cerebral cortex. Since it is possible to demonstrate the morphological localization and distribution of heavy metals, such as cobalt, by correlative x-ray analysis and electron microscopy (i.e., by AEM), we are using AEM to locate and identify elemental cobalt in phagocytic meningeal cells of young 80-day postnatal opossums following a subdural injection of cobalt particles.

High-resolution x-ray analysis of dislocation networks nn tilt boundaries

1988 ◽  
Vol 46 ◽  
pp. 612-613
Author(s):  
J. R. Michael ◽  
C. H. Lin ◽  
S. L. Sass
Keyword(s):  
Grain Boundaries ◽  
Analytical Electron Microscopy ◽  
Solute Segregation ◽  
X Ray ◽  
Periodic Arrays ◽  
Analytical Electron ◽  
Primary Dislocation ◽  
Tilt Boundaries ◽  
Polycrystalline Solids ◽  
Twist Boundaries

The segregation of solute atoms to grain boundaries in polycrystalline solids can be responsible for embrittlement of the grain boundaries. Although Auger electron spectroscopy (AES) and analytical electron microscopy (AEM) have verified the occurrence of solute segregation to grain boundaries, there has been little experimental evidence concerning the distribution of the solute within the plane of the interface. Sickafus and Sass showed that Au segregation causes a change in the primary dislocation structure of small angle [001] twist boundaries in Fe. The bicrystal specimens used in their work, which contain periodic arrays of dislocations to which Au is segregated, provide an excellent opportunity to study the distribution of Au within the boundary by AEM.The thin film Fe-0.8 at% Au bicrystals (composition determined by Rutherford backscattering spectroscopy), ∼60 nm thick, containing [001] twist boundaries were prepared as described previously. The bicrystals were analyzed in a Vacuum Generators HB-501 AEM with a field emission electron source and a Link Analytical windowless x-ray detector.

LACBED with Quantitative Anomalous Absorption Corrections

1990 ◽  
Vol 48 (2) ◽  
pp. 528-529
Author(s):  
C.J. Rossouw ◽  
L.J. Allen ◽  
P.R. Miller
Keyword(s):  
Momentum Transfer ◽  
Scattering Amplitude ◽  
Incident Beam ◽  
Waller Factor ◽  
Beam Momentum ◽  
Anomalous Absorption ◽  
Quantitative Calculation ◽  
Ewald Sphere ◽  
Image Position ◽  
Incident Beam Energy

An Einstein model for thermal diffuse scattering (TDS) has enabled quantitative calculation of the absorptive potential V'(r). This allows anomalous absorption to be accounted for in LACBED contrast. Fourier coefficients Vg-h of the absorptive component from each atom α are calculated from integrals of the formwhere fα is the scattering amplitude and M(Q) the Debye-Waller factor. Integration over the Ewald sphere (dΩ) requires the momentum transfer q to have values up to 2ko (the incident beam momentum). Dynamical ‘dechannelling’ is accounted for by the terms g ≠ h. The crystal absorptive potential is obtained by coherently summing over these atomic absorptive potentials within the unit cell. Unlike the elastic potential, the absorptive potential is a strong function of incident beam energy Eo, since the range of momentum transfer q and associated solid angles dΩ change with the Ewald sphere radius.Fig. 1 shows a LACBED pattern of the zeroth order beam from Si aligned along a <001> zone axis.

Phase identification in SiC whisker reinforced Al2O3-R2O3-based composites

1992 ◽  
Vol 50 (1) ◽  
pp. 152-153
Author(s):  
C.M. Sung ◽  
K.J. Ostreicher ◽  
M.L. Huckabee ◽  
S.T. Buljan
Keyword(s):  
Analytical Electron Microscopy ◽  
Phase Identification ◽  
Reinforced Composites ◽  
Ion Milling ◽  
X Ray ◽  
Binary Oxides ◽  
Analytical Electron ◽  
The Matrix ◽  
Second Phases ◽  
Convergent Beam

A series of binary oxides and SiC whisker reinforced composites both having a matrix composed of an α-(Al, R)2O3 solid solution (R: rare earth) have been studied by analytical electron microscopy (AEM). The mechanical properties of the composites as well as crystal structure, composition, and defects of both second phases and the matrix were investigated. The formation of various second phases, e.g. garnet, β-Alumina, or perovskite structures in the binary Al2O3-R2O3 and the ternary Al2O3-R2O3-SiC(w) systems are discussed.Sections of the materials having thicknesses of 100 μm - 300 μm were first diamond core drilled. The discs were then polished and dimpled. The final step was ion milling with Ar+ until breakthrough occurred. Samples prepared in this manner were then analyzed using the Philips EM400T AEM. The low-Z energy dispersive X-ray spectroscopy (EDXS) data were obtained and correlated with convergent beam electron diffraction (CBED) patterns to identify phase compositions and structures. The following EDXS parameters were maintained in the analyzed areas: accelerating voltage of 120 keV, sample tilt of 12° and 20% dead time.

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.

Some Aspects of Exelfs Analysis in the Electron Microscope

1980 ◽  
Vol 38 ◽  
pp. 118-119
Author(s):  
D. E. Johnson ◽  
S. Csillag
Keyword(s):  
Fine Structure ◽  
Electron Microscope ◽  
Energy Loss ◽  
Analytical Electron Microscopy ◽  
Interference Effects ◽  
Interatomic Distances ◽  
X Ray ◽  
Structure Information ◽  
Microanalytical Technique ◽  
Analytical Electron

Recently, the applications area of analytical electron microscopy has been extended to include the study of Extended Energy Loss Fine Structure (EXELFS). Modulations past an ionization edge in the energy loss spectrum (EXELFS), contain atomic fine structure information similar to Extended X-ray Absorbtion Fine Structure (EXAFS). At low momentum transfer the main contribution to these modulations comes from interference effects between the outgoing excited inner shell electron waves and electron waves backscattered from the surrounding atoms. The ability to obtain atomic fine structure information (such as interatomic distances) combined with the spatial resolution of an electron microscope is unique and makes EXELFS an important microanalytical technique.

scholarly journals Analytical electron microscopic evaluation of the effects of paraformaldehyde pretreatment on the reaction of glutaraldehyde with biogenic amines.

1982 ◽  
Vol 30 (5) ◽  
pp. 481-486 ◽  
Author(s):  
R E McClung ◽  
J Wood
Keyword(s):  
Electron Microscopy ◽  
Analytical Electron Microscopy ◽  
Microscopic Level ◽  
Electron Microscopic Level ◽  
Spectrographic Analysis ◽  
Electron Microscopic ◽  
X Ray ◽  
Microscopic Evaluation ◽  
Analytical Electron ◽  
Dense Product

Analytical electron microscopy was used to determine the quantitative effects of paraformaldehyde pretreatment on the formation of the biogenic amine-glutaraldehyde-chrome complex. Pretreatment with paraformaldehyde prevented the glutaraldehyde-chrome reaction with norepinephrine in the rat adrenal medulla. In contrast to the effect of paraformaldehyde on norepinephrine, pretreatment did not prevent the chrome reaction in serotonin-containing argentaffin cells of the gut. X-Ray energy spectrographic analysis revealed a significant decrease in chrome content in the paraformaldehyde treated tissue, but sufficient chrome did react to produce an electron-dense product. Thus by treating tissue with paraformaldehyde prior to the glutaraldehyde chrome procedure, serotonergic sites may be differentiated from catecholaminergic areas at the electron microscopic level.

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