Elemental mass loss in silicate minerals during x-ray analysis

1990 ◽  
Vol 48 (4) ◽  
pp. 804-805
Author(s):  
P.E. Champness ◽  
R.W. Devenish
Keyword(s):  
Mass Loss ◽  
Current Density ◽  
Damage Mechanism ◽  
Beam Current ◽  
Single Chain ◽  
Plagioclase Feldspar ◽  
X Ray ◽  
Alkali Ions ◽  
Structural Order ◽  
Sheet Silicate

It has long been recognised that silicates can suffer extensive beam damage in electron-beam instruments. The predominant damage mechanism is radiolysis. For instance, damage in quartz, SiO2, results in loss of structural order without mass loss whereas feldspars (framework silicates containing Ca, Na, K) suffer loss of structural order with accompanying mass loss. In the latter case, the alkali ions, particularly Na, are found to migrate away from the area of the beam. The aim of the present study was to investigate the loss of various elements from the common silicate structures during electron irradiation at 100 kV over a range of current densities of 104 - 109 A m−2. (The current density is defined in terms of 50% of total current in the FWHM probe). The silicates so far ivestigated are:- olivine [(Mg, Fe)SiO4], a structure that has isolated Si-O tetrahedra, garnet [(Mg, Ca, Fe)3Al2Si3AO12 another silicate with isolated tetrahedra, pyroxene [-Ca(Mg, Fe)Si2O6 a single-chain silicate; mica [margarite, -Ca2Al4Si4Al4O2O(OH)4], a sheet silicate, and plagioclase feldspar [-NaCaAl3Si5O16]. Ion- thinned samples of each mineral were examined in a VG Microscopes UHV HB501 field- emission STEM. The beam current used was typically - 0.5 nA and the current density was varied by defocussing the electron probe. Energy-dispersive X-ray spectra were collected every 10 seconds for a total of 200 seconds using a Link Systems windowless detector. The thickness of the samples in the area of analysis was normally 50-150 nm.

Methods to quantify silver in autoradiographs

1980 ◽  
Vol 238 (3) ◽  
pp. H414-H422
Author(s):  
D. L. Fry ◽  
A. J. Tousimis ◽  
T. L. Talbot ◽  
S. J. Lewis
Keyword(s):  
Electron Beam ◽  
Current Density ◽  
Electron Probe ◽  
Beam Current ◽  
Silver Concentration ◽  
Electron Beam Current ◽  
Beam Size ◽  
X Ray ◽  
Small Variance ◽  
Arterial Tissue

The developed silver in specially prepared photographic films (PF) and autoradiographs (AR) of radiolabeled arterial tissue was quantified by direct grain counting (GC), microdensitometry (OD), and by electron probe X-ray microanalysis (EPA). The EPA data was proportional to the OD data with a very small variance. The GC data increased with the EPA data, but showed a large variance. The EPA signal was shown 1) to be reproducible even after multiple traverses across the specimen, 2) to be directly proportional to the electron beam current and emulsion silver concentration, and 3) to be insensitive to a) beam size, b) current density, c) energy above 17 keV, or d) nonuniformities in the thickness of the conductive coating on the specimen.

The Microstructure of Steatite (Protoenstatite)

1985 ◽  
Vol 43 ◽  
pp. 236-237
Author(s):  
W. E. Lee ◽  
A. H. Heuer
Keyword(s):  
High Frequency ◽  
Glass Ceramics ◽  
Magnesium Silicate ◽  
Beam Current ◽  
Glassy Matrix ◽  
Angle Of Incidence ◽  
X Ray ◽  
Mechanical And Electrical Properties ◽  
Argon Ions ◽  
High Temperature Polymorph

IntroductionTraditional steatite ceramics, made by firing (vitrifying) hydrous magnesium silicate, have long been used as insulators for high frequency applications due to their excellent mechanical and electrical properties. Early x-ray and optical analysis of steatites showed that they were composed largely of protoenstatite (MgSiO3) in a glassy matrix. Recent studies of enstatite-containing glass ceramics have revived interest in the polymorphism of enstatite. Three polymorphs exist, two with orthorhombic and one with monoclinic symmetry (ortho, proto and clino enstatite, respectively). Steatite ceramics are of particular interest a they contain the normally unstable high-temperature polymorph, protoenstatite.Experimental3mm diameter discs cut from steatite rods (∼10” long and 0.5” dia.) were ground, polished, dimpled, and ion-thinned to electron transparency using 6KV Argon ions at a beam current of 1 x 10-3 A and a 12° angle of incidence. The discs were coated with carbon prior to TEM examination to minimize charging effects.

Practical Importance of Spatial Resolution and Analytical Sensitivity in AEM X-ray Microanalysis

1990 ◽  
Vol 48 (2) ◽  
pp. 432-433
Author(s):  
J. Zhang ◽  
D.B. Williams ◽  
J.I. Goldstein
Keyword(s):  
Spatial Resolution ◽  
Practical Importance ◽  
Beam Current ◽  
Specimen Thickness ◽  
Analytical Sensitivity ◽  
Related Factors ◽  
X Ray ◽  
Probe Size ◽  
Excitation Volume ◽  
Two Parameters

Analytical sensitivity and spatial resolution are important and closely related factors in x-ray microanalysis using the AEM. Analytical sensitivity is the ability to distinguish, for a given element under given conditions, between two concentrations that are nearly equal. The analytical sensitivity is directly related to the number of x-ray counts collected and, therefore, to the probe current, specimen thickness and counting time. The spatial resolution in AEM analysis is determined by the probe size and beam broadening in the specimen. A finer probe and a thinner specimen give a higher spatial resolution. However, the resulting lower beam current and smaller X-ray excitation volume degrade analytical sensitivity. A compromise must be made between high spatial resolution and an acceptable analytical sensitivity. In this paper, we show the necessity of evaluating these two parameters in order to determine the low temperature Fe-Ni phase diagram.A Phillips EM400T AEM with an EDAX/TN2000 EDS/MCA system and a VG HB501 FEG STEM with a LINK AN10 EDS/MCA system were used.

Electron Beam-Induced Mass Loss in Freeze-Dried Tissue and Protein Samples

1985 ◽  
Vol 43 ◽  
pp. 470-471
Author(s):  
M.E. Cantino ◽  
M.K. Goddard ◽  
L.E. Wilkinson ◽  
D.E. Johnson
Keyword(s):  
Electron Beam ◽  
Salivary Gland ◽  
Mass Loss ◽  
Counting Rate ◽  
Dose Dependence ◽  
X Ray ◽  
Large Samples ◽  
Freeze Dried ◽  
Muscle Homogenate ◽  
Large Muscle

Quantification in biological x-ray microanalysis depends on accurate evaluation of mass loss. Although several studies have addressed the problem of electron beam induced mass loss from organic samples (eg., 1,2). uncertainty persists as to the dose dependence, the extent of loss, the elemental constituents affected, and the variation in loss for different materials and tissues. in the work described here, we used x-ray counting rate changes to measure mass loss in albumin (used as a quantification standard), salivary gland, and muscle.In order to measure mass loss at low doses (10-4 coul/cm2 ) large samples were needed. While freeze-dried salivary gland sections of the required dimensions were available, muscle sections of this size were difficult to obtain. To simulate large muscle sections, frog or rat muscle homogenate was injected between formvar films which were then stretched over slot grids and freeze-dried. Albumin samples were prepared by a similar procedure. using a solution of bovine serum albumin in water. Samples were irradiated in the STEM mode of a JEOL 100C.

Electron behavior in the gaseous environment of the ESEM chamber

1996 ◽  
Vol 54 ◽  
pp. 838-839 ◽  
Author(s):  
S.A. Wight
Keyword(s):  
Secondary Electron ◽  
High Vacuum ◽  
Beam Current ◽  
Chamber Pressure ◽  
Environmental Scanning ◽  
Carbon Block ◽  
Faraday Cup ◽  
X Ray ◽  
Gaseous Environment ◽  
Working Distance

Measurements of electrons striking the sample in the Environmental Scanning Electron Microscope (ESEM) are needed to begin to understand the effect of the presence of the gas on analytical measurements. Accurate beam current is important to x-ray microanalysis and it is typically measured with a faraday cup. A faraday cup (Figure 1) was constructed from a carbon block embedded in non-conductive epoxy with a 45 micrometer bore platinum aperture over the hole. Currents were measured with an electrometer and recorded as instrument parameters were varied.Instrument parameters investigated included working distance, chamber pressure, condenser percentage, and accelerating voltage. The conditions studied were low vacuum with gaseous secondary electron detector (GSED) voltage on; low vacuum with GSED voltage off; and high vacuum (GSED off). The base conditions were 30 kV, 667 Pa (5 Torr) water vapor, 100,000x magnification with the beam centered inside aperture, GSED voltage at 370 VDC, condenser at 50%, and working distance at 19.5 mm. All modifications of instrument parameters were made from these conditions.

scholarly journals Revisiting the Bøggild Intergrowth in Iridescent Labradorite Feldspars: Ordering, Kinetics, and Phase Equilibria

Minerals ◽  
2021 ◽  
Vol 11 (7) ◽  
pp. 727
Author(s):  
Shiyun Jin ◽  
Huifang Xu ◽  
Seungyeol Lee
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Atom Probe ◽  
Phase Region ◽  
Two Phase ◽  
Subsolidus Phase ◽  
Plagioclase Feldspar ◽  
X Ray ◽  
Transmission Electron ◽  
Scanning Transmission

The enigmatic Bøggild intergrowth in iridescent labradorite crystals was revisited in light of recent work on the incommensurately modulated structures in the intermediated plagioclase. Five igneous samples and one metamorphic labradorite sample with various compositions and lamellar thicknesses were studied in this paper. The lamellar textures were characterized with conventional transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM). The compositions of individual lamellae were analyzed with high-resolution energy-dispersive X-ray spectroscopy (EDS) mapping and atom probe tomography (APT). The average structure states of the studied samples were also compared with single-crystal X-ray diffraction data (SC-XRD). The Na-rich lamellae have a composition of An44–48, and the Ca-rich lamellae range from An56 to An63. Significant differences between the lamellar compositions of different samples were observed. The compositions of the Bøggild intergrowth do not only depend on the bulk compositions, but also on the thermal history of the host rock. The implications on the subsolidus phase relationships of the plagioclase feldspar solid solution are discussed. The results cannot be explained by a regular symmetrical solvus such as the Bøggild gap, but they support an inclined two-phase region that closes at low temperature.

scholarly journals The Texture of a Slate From Nantlle, Caernarvon, North Wales

Texture ◽  
1972 ◽  
Vol 1 (1) ◽  
pp. 1-8 ◽  
Author(s):  
Gerhard Oertel ◽  
Prem P. Phakey
Keyword(s):  
Ultrathin Section ◽  
Orthorhombic Symmetry ◽  
X Ray ◽  
Plane Normal ◽  
North Wales ◽  
Pole Figures ◽  
Sheet Silicate ◽  
Diffraction Patterns ◽  
Local Dissolution ◽  
Mechanical Rotation

A specimen of Cambrian slate from the slate belt in North Wales has been thinned by the ion bombardment technique to produce an ultrathin section with the specimen plane normal to the cleavage plane. This specimen has been investigated with the electron microscope by electron transmission. Selected area diffraction patterns allow identification of individual sheet silicate grains. The pole figures of the basal planes of two sheet silicate minerals, muscovite and chlorite, have been measured with an X-ray pole-figure goniometer and both show an elongated maximum normal to the slaty cleavage, with orthorhombic symmetry. While the preferred orientation could be the result of mechanical rotation of rigid flakes in a deforming matrix, the texture (the overall pattern due to the shapes and sizes of grains and their angular relations to each other) can only be explained if considerable recrystallization is assumed. It is tentatively proposed that local dissolution at points of stress-concentration with simultaneous redeposition of the dissolved material in less stressed regions may have allowed closely packed grains to act as if they were mechanically rotating rigid flakes, yet to accommodate their shapes enough to prevent interlocking.

scholarly journals Radio Supernovae as Direct Evidence of Stellar Evolution in Real Time

1998 ◽  
Vol 11 (1) ◽  
pp. 367-367
Author(s):  
S.D. Van Dyk ◽  
M.J. Montes ◽  
K.W. Weiler ◽  
R.A. Sramek ◽  
N. Panagia
Keyword(s):  
Mass Loss ◽  
Stellar Evolution ◽  
Loss Rate ◽  
Direct Evidence ◽  
Mass Loss Rate ◽  
X Ray ◽  
Stringent Constraint ◽  
Clear Change ◽  
Late Stages ◽  
Circumstellar Environment

The radio emission from supernovae provides a direct probe of a supernova’s circumstellar environment, which presumably was established by mass-loss episodes in the late stages of the progenitor’s presupernova evolution. The observed synchrotron emission is generated by the SN shock interacting with the relatively high-density circumstellar medium which has been fully ionized and heated by the initial UV/X-ray flash. The study of radio supernovae therefore provides many clues to and constraints on stellar evolution. We will present the recent results on several cases, including SN 1980K, whose recent abrupt decline provides us with a stringent constraint on the progenitor’s initial mass; SN 1993J, for which the profile of the wind matter supports the picture of the progenitor’s evolution in an interacting binary system; and SN 1979C, where a clear change in presupernova mass-loss rate occurred about 104 years before explosion. Other examples, such as SNe 19941 and 1996cb, will also be discussed.

Synergistic effect of Al2O3/TiO2 reinforcements on slurry erosion performance of nickel-based composite coatings

2017 ◽  
Vol 232 (8) ◽  
pp. 974-986 ◽  
Author(s):  
Rajeev Kumar ◽  
Sanjeev Bhandari ◽  
Atul Goyal
Keyword(s):  
Electron Microscope ◽  
Scanning Electron Microscope ◽  
Mass Loss ◽  
Erosion Resistance ◽  
Slurry Erosion ◽  
Specific Mass ◽  
Operational Parameter ◽  
X Ray ◽  
Specific Mass Loss ◽  
Scanning Electron

Various aspects such as development, experimentation, and analysis have been covered in the present work to examine the behavior of test coatings under slurry erosion. The primary objective of the present study was to establish the specific mass loss from the test coatings under various slurry environmental conditions and highlights the importance of the addition of alumina in improving the slurry erosion resistance of Ni-TiO2 coating. To attain this objective, two powder compositions, viz. Ni-20TiO2 and Ni-15TiO2-5Al2O3 were deposited onto the CA6NM grade hydro-turbine steel using high velocity frame spray process. The microstructural characterization of the coatings was done by employing surface roughness tester, scanning electron microscope/energy-dispersive X-ray spectroscopy, and X-ray diffraction techniques, whereas mechanical analysis was carried out using micro-hardness and bond strength tester. The slurry erosion tests were performed using an indigenously fabricated high speed slurry erosion test rig at different levels of rotational speed, average particle size of erodent, and slurry concentration in order to explore their effects on slurry erosion performance of test coatings. The slurry erosion results, as well as scanning electron microscope observations of eroded specimens, revealed higher slurry erosion resistance of Ni-15TiO2-5Al2O3 coating in comparison with Ni-20TiO2 coating. Furthermore, each operational parameter was found to have a proportional effect on specific mass loss in case of both the coatings.

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