Divergent beam microanalysis studies of bimetallic platinum catalysts supported on γ-AL2O3

Author(s):  
JR Fryer ◽  
Z Huang ◽  
D Stirling ◽  
G. Webb

Platinum dispersed on γ-alumina is used as a reforming catalyst to convert linear hydrocarbons to cyclic aromatic products. To improve selectivity and lifetime of the catalyst, other elements are included, and we have studied the distributions of Pt/Re, and Pt/Sn, bimetallic systems on the support both before and after use in octane reforming. Often, one or both of the components are not resolvable by HREM or microanalysis as individual particles because of small size and lack of contrast on the alumina, and divergent beam microanalysis has been used to establish the presence and relationship between the two elements.In the majority of catalysts the platinum is in the form of small panicles, some of which are large enough to be resolvable in the microscope. The ABT002B microscope with Link windowless Pentafet detector, used in this work, was able to obtain a resolvable signal from particles of 2nm diameter upwards. When the beam was concentrated on to such a particle the signal was at a maximum, and as the beam diameter was diverged - at the same total beam intensity and dead time - the signal decreased as shown in Figure 1.

2018 ◽  
Vol 4 (11) ◽  
pp. 134 ◽  
Author(s):  
Ilia Safonov ◽  
Ivan Yakimchuk ◽  
Vladimir Abashkin

We present image processing algorithms for a new technique of ceramic proppant crush resistance characterization. To obtain the images of the proppant material before and after the test we used X-ray microtomography. We propose a watershed-based unsupervised algorithm for segmentation of proppant particles, as well as a set of parameters for the characterization of 3D particle size, shape, and porosity. An effective approach based on central geometric moments is described. The approach is used for calculation of particles’ form factor, compactness, equivalent ellipsoid axes lengths, and lengths of projections to these axes. Obtained grain size distribution and crush resistance fit the results of conventional test measured by sieves. However, our technique has a remarkable advantage over traditional laboratory method since it allows to trace the destruction at the level of individual particles and their fragments; it grants to analyze morphological features of fines. We also provide an example describing how the approach can be used for verification of statistical hypotheses about the correlation between particles’ parameters and their crushing under load.


1985 ◽  
Vol 53 ◽  
Author(s):  
Li Xiqiang ◽  
Zhu Weiwen ◽  
Lin Chenglu ◽  
Wang Weiyuan ◽  
Tsou Shihchang

ABSTRACTThe InP films with thickness of 1-2 µm and resistivity of 10-10−3Ω-cm were sputtered on oxidized Si substrates heated at about 300°C to form as InP SOI. Using X-ray diffraction, ED, TEM, Hall and RBS, we have investigated the grain size, compositions, thermal stability and electrical characteristics of InP SOI before and after CW Ar+ laser recrystallization. The sputtered InP SOI films appear as polycrystalline and its grain size increases with increasing of irradiated laser power from 5.8 to 7.0 W at a beam diameter of 70 µm. After irradiation at 7 W the single crystal ED patterns are obtained, the mobility and carrier concentrations amount to 103cm2/Vs and 1017cm−3, respectively, and the compositions are stoichiometric.


2005 ◽  
Vol 38 (6) ◽  
pp. 1004-1011 ◽  
Author(s):  
J. G. Barker ◽  
C. J. Glinka ◽  
J. J. Moyer ◽  
M. H. Kim ◽  
A. R. Drews ◽  
...  

An ultra-high-resolution small-angle neutron scattering (USANS) double-crystal diffractometer (DCD) is now in operation at the NIST Center for Neutron Research (NCNR). The instrument uses multiple reflections from large silicon (220) perfect single crystals, before and after the sample, to produce both high beam intensity and a low instrument background suitable for small-angle scattering measurements. The minimum detector background to beam intensity ratio (noise-to-signal, N/S) forq≥ 5 × 10−4 Å−1is 4 × 10−7. The instrument uses 2.38 Å wavelength neutrons on a dedicated thermal neutron beam port, producing a peak flux on the sample of 17300 cm−2 s−1. The typical measurement range of the instrument extends from 3 × 10−5 Å−1to 5 × 10−3 Å−1in scattering wavevector (q), providing information on material structure over the size range from 0.1 µm to 20 µm. This paper describes the design and characteristics of the instrument, the mode of operation, and presents data that demonstrate the instrument's performance.


Author(s):  
J. Temple Black

Tool materials used in ultramicrotomy are glass, developed by Latta and Hartmann (1) and diamond, introduced by Fernandez-Moran (2). While diamonds produce more good sections per knife edge than glass, they are expensive; require careful mounting and handling; and are time consuming to clean before and after usage, purchase from vendors (3-6 months waiting time), and regrind. Glass offers an easily accessible, inexpensive material ($0.04 per knife) with very high compressive strength (3) that can be employed in microtomy of metals (4) as well as biological materials. When the orthogonal machining process is being studied, glass offers additional advantages. Sections of metal or plastic can be dried down on the rake face, coated with Au-Pd, and examined directly in the SEM with no additional handling (5). Figure 1 shows aluminum chips microtomed with a 75° glass knife at a cutting speed of 1 mm/sec with a depth of cut of 1000 Å lying on the rake face of the knife.


Author(s):  
R. F. Bils ◽  
W. F. Diller ◽  
F. Huth

Phosgene still plays an important role as a toxic substance in the chemical industry. Thiess (1968) recently reported observations on numerous cases of phosgene poisoning. A serious difficulty in the clinical handling of phosgene poisoning cases is a relatively long latent period, up to 12 hours, with no obvious signs of severity. At about 12 hours heavy lung edema appears suddenly, however changes can be seen in routine X-rays taken after only a few hours' exposure (Diller et al., 1969). This study was undertaken to correlate these early changes seen by the roengenologist with morphological alterations in the lungs seen in the'light and electron microscopes.Forty-two adult male and female Beagle dogs were selected for these exposure experiments. Treated animals were exposed to 94.5-107-5 ppm phosgene for 10 min. in a 15 m3 chamber. Roentgenograms were made of the thorax of each animal before and after exposure, up to 24 hrs.


Author(s):  
S. S. Sheinin ◽  
C. D. Cann

The effects of systematic reflections on the variation of diffracted beam intensity with depth in a crystal can only be taken into account by using the multi-beam dynamical theory. The results of calculations of this kind, which are presented here, indicate that the intensity profiles obtained are not periodic. Since extinction distance is a concept strictly applicable only when the diffracted beam intensity varies periodically with depth, its use as a parameter in describing multi-beam intensity profiles must be carefully considered.


Author(s):  
M. H. Wheeler ◽  
W. J. Tolmsoff ◽  
A. A. Bell

(+)-Scytalone [3,4-dihydro-3,6,8-trihydroxy-l-(2Hj-naphthalenone] and 1,8-di- hydroxynaphthalene (DHN) have been proposed as intermediates of melanin synthesis in the fungi Verticillium dahliae (1, 2, 3, 4) and Thielaviopsis basicola (4, 5). Scytalone is enzymatically dehydrated by V. dahliae to 1,3,8-trihydroxynaphthalene which is then reduced to (-)-vermelone [(-)-3,4- dihydro-3,8-dihydroxy-1(2H)-naphthalenone]. Vermelone is subsequently dehydrated to DHN which is enzymatically polymerized to melanin.Melanin formation in Curvularia sp., Alternaria sp., and Drechslera soro- kiniana was examined by light and electron-transmission microscopy. Wild-type isolates of each fungus were compared with albino mutants before and after treatment with 1 mM scytalone or 0.1 mM DHN in 50 mM potassium phosphate buffer, pH 7.0. Both chemicals were converted to dark pigments in the walls of hyphae and conidia of the albino mutants. The darkened cells were similar in appearance to corresponding cells of the wild types under the light microscope.


Author(s):  
P.J. Killingworth ◽  
M. Warren

Ultimate resolution in the scanning electron microscope is determined not only by the diameter of the incident electron beam, but by interaction of that beam with the specimen material. Generally, while minimum beam diameter diminishes with increasing voltage, due to the reduced effect of aberration component and magnetic interference, the excited volume within the sample increases with electron energy. Thus, for any given material and imaging signal, there is an optimum volt age to achieve best resolution.In the case of organic materials, which are in general of low density and electric ally non-conducting; and may in addition be susceptible to radiation and heat damage, the selection of correct operating parameters is extremely critical and is achiev ed by interative adjustment.


Author(s):  
Irwin Bendet ◽  
Nabil Rizk

Preliminary results reported last year on the ion etching of tobacco mosaic virus indicated that the diameter of the virus decreased more rapidly at 10KV than at 5KV, perhaps reaching a constant value before disappearing completely.In order to follow the effects of ion etching on TMV more quantitatively we have designed and built a second apparatus (Fig. 1), which incorporates monitoring devices for measuring ion current and vacuum as well as accelerating voltage. In addition, the beam diameter has been increased to approximately 1 cm., so that ten electron microscope grids can be exposed to the beam simultaneously.


Author(s):  
T. Gulik-Krzywicki ◽  
M.J. Costello

Freeze-etching electron microscopy is currently one of the best methods for studying molecular organization of biological materials. Its application, however, is still limited by our imprecise knowledge about the perturbations of the original organization which may occur during quenching and fracturing of the samples and during the replication of fractured surfaces. Although it is well known that the preservation of the molecular organization of biological materials is critically dependent on the rate of freezing of the samples, little information is presently available concerning the nature and the extent of freezing-rate dependent perturbations of the original organizations. In order to obtain this information, we have developed a method based on the comparison of x-ray diffraction patterns of samples before and after freezing, prior to fracturing and replication.Our experimental set-up is shown in Fig. 1. The sample to be quenched is placed on its holder which is then mounted on a small metal holder (O) fixed on a glass capillary (p), whose position is controlled by a micromanipulator.


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