Quantitative nano-characterization of heterogeneous catalysts

Author(s):  
P.A. Crozier ◽  
M. Pan

Heterogeneous catalysts can be of varying complexity ranging from single or double phase systems to complicated mixtures of metals and oxides with additives to help promote chemical reactions, extend the life of the catalysts, prevent poisoning etc. Although catalysis occurs on the surface of most systems, detailed descriptions of the microstructure and chemistry of catalysts can be helpful for developing an understanding of the mechanism by which a catalyst facilitates a reaction. Recent years have seen continued development and improvement of various TEM, STEM and AEM techniques for yielding information on the structure and chemistry of catalysts on the nanometer scale. Here we review some quantitative approaches to catalyst characterization that have resulted from new developments in instrumentation.HREM has been used to examine structural features of catalysts often by employing profile imaging techniques to study atomic details on the surface. Digital recording techniques employing slow-scan CCD cameras have facilitated the use of low-dose imaging in zeolite structure analysis and electron crystallography. Fig. la shows a low-dose image from SSZ-33 zeolite revealing the presence of a stacking fault.

2004 ◽  
Vol 10 (1) ◽  
pp. 55-76 ◽  
Author(s):  
Jingyue Liu

Heterogeneous catalysis is one of the oldest nanosciences. Although model catalysts can be designed, synthesized, and, to a certain degree, characterized, industrial heterogeneous catalysts are often chemically and physically complex systems that have been developed through many years of catalytic art, technology, and science. The preparation of commercial catalysts is generally not well controlled and is often based on accumulated experiences. Catalyst characterization is thus critical to developing new catalysts with better activity, selectivity, and/or stability. Advanced electron microscopy, among many characterization techniques, can provide useful information for the fundamental understanding of heterogeneous catalysis and for guiding the development of industrial catalysts. In this article, we discuss the recent developments in applying advanced electron microscopy techniques to characterizing model and industrial heterogeneous catalysts. The importance of understanding the catalyst nanostructure and the challenges and opportunities of advanced electron microscopy in developing nanostructured catalysts are also discussed.


Author(s):  
M. Pan ◽  
P.A. Crozier ◽  
I.Y. Chan ◽  
S.I. Zones

Zeolites constitute an important class of catalyst materials in the petrochemical industry. Zeolites are aluminosilicates with their framework structures made up of SiO4 (or AlO4) tetrahedra. The catalytic properties such as selectivity and activity are closely related to the structure sensitive properties of zeolites, e.g. shape selectivity, diffusivity, etc. Understanding these properties requires detailed structure characterization of the zeolites. High resolution electron microscopy (HREM) has been successfully applied to solve some zeolite structures when combined with experimental data from other techniques, e.g. absorption experiment. The connectivities of n-member rings in the zeolite frameworks can be directly deduced from the corresponding HREM images. However, radiation damage to the zeolite framework structures by the electron beam necessitates the use of low dose imaging techniques.


2022 ◽  
Vol 29 (1) ◽  
Author(s):  
Sebastian Kalbfleisch ◽  
Yuhe Zhang ◽  
Maik Kahnt ◽  
Khachiwan Buakor ◽  
Max Langer ◽  
...  

Coherent X-ray imaging techniques, such as in-line holography, exploit the high brilliance provided by diffraction-limited storage rings to perform imaging sensitive to the electron density through contrast due to the phase shift, rather than conventional attenuation contrast. Thus, coherent X-ray imaging techniques enable high-sensitivity and low-dose imaging, especially for low-atomic-number (Z) chemical elements and materials with similar attenuation contrast. Here, the first implementation of in-line holography at the NanoMAX beamline is presented, which benefits from the exceptional focusing capabilities and the high brilliance provided by MAX IV, the first operational diffraction-limited storage ring up to approximately 300 eV. It is demonstrated that in-line holography at NanoMAX can provide 2D diffraction-limited images, where the achievable resolution is only limited by the 70 nm focal spot at 13 keV X-ray energy. Also, the 3D capabilities of this instrument are demonstrated by performing holotomography on a chalk sample at a mesoscale resolution of around 155 nm. It is foreseen that in-line holography will broaden the spectra of capabilities of MAX IV by providing fast 2D and 3D electron density images from mesoscale down to nanoscale resolution.


2021 ◽  
Vol 10 (10) ◽  
pp. 2196
Author(s):  
Julie Finance ◽  
Laurent Zieleskewicz ◽  
Paul Habert ◽  
Alexis Jacquier ◽  
Philippe Parola ◽  
...  

Background: The COVID-19 pandemic has provided an opportunity to use low- and non-radiating chest imaging techniques on a large scale in the context of an infectious disease, which has never been done before. Previously, low-dose techniques were rarely used for infectious diseases, despite the recognised danger of ionising radiation. Method: To evaluate the role of low-dose computed tomography (LDCT) and lung ultrasound (LUS) in managing COVID-19 pneumonia, we performed a review of the literature including our cases. Results: Chest LDCT is now performed routinely when diagnosing and assessing the severity of COVID-19, allowing patients to be rapidly triaged. The extent of lung involvement assessed by LDCT is accurate in terms of predicting poor clinical outcomes in COVID-19-infected patients. Infectious disease specialists are less familiar with LUS, but this technique is also of great interest for a rapid diagnosis of patients with COVID-19 and is effective at assessing patient prognosis. Conclusions: COVID-19 is currently accelerating the transition to low-dose and “no-dose” imaging techniques to explore infectious pneumonia and their long-term consequences.


Dose-Response ◽  
2021 ◽  
Vol 19 (1) ◽  
pp. 155932582199565
Author(s):  
Paul A. Oakley ◽  
Deed E. Harrison

There are pressures to avoid use of radiological imaging throughout all healthcare due to the notion that all radiation is carcinogenic. This perception stems from the long-standing use of the linear no-threshold (LNT) assumption of risk associated with radiation exposures. This societal perception has led to relentless efforts to avoid and reduce radiation exposures to patients at great costs. Many radiation reduction campaigns have been launched to dissuade doctors from using radiation imaging. Lower-dose imaging techniques and practices are being advocated. Alternate imaging procedures are encouraged. Are these efforts warranted? Based on recent evidence, LNT ideology is shown to be defunct for risk assessment at low-dose exposure ranges which includes X-rays and CT scans. In fact, the best evidence that was once used to support LNT ideology, including the Life Span Study data, now indicates thresholds for cancer induction are high; therefore, low-dose X-rays cannot cause harm. Current practices are safe as exposures currently encountered are orders of magnitude below threshold levels shown to be harmful. As long as imaging is medically warranted, it is shown that efforts to reduce exposures that are within background radiation levels and that are also shown to enhance health by upregulating natural adaptive protection systems are definitively wasted resources.


Author(s):  
D. F. Blake ◽  
L. F. Allard ◽  
D. R. Peacor

Echinodermata is a phylum of marine invertebrates which has been extant since Cambrian time (c.a. 500 m.y. before the present). Modern examples of echinoderms include sea urchins, sea stars, and sea lilies (crinoids). The endoskeletons of echinoderms are composed of plates or ossicles (Fig. 1) which are with few exceptions, porous, single crystals of high-magnesian calcite. Despite their single crystal nature, fracture surfaces do not exhibit the near-perfect {10.4} cleavage characteristic of inorganic calcite. This paradoxical mix of biogenic and inorganic features has prompted much recent work on echinoderm skeletal crystallography. Furthermore, fossil echinoderm hard parts comprise a volumetrically significant portion of some marine limestones sequences. The ultrastructural and microchemical characterization of modern skeletal material should lend insight into: 1). The nature of the biogenic processes involved, for example, the relationship of Mg heterogeneity to morphological and structural features in modern echinoderm material, and 2). The nature of the diagenetic changes undergone by their ancient, fossilized counterparts. In this study, high resolution TEM (HRTEM), high voltage TEM (HVTEM), and STEM microanalysis are used to characterize tha ultrastructural and microchemical composition of skeletal elements of the modern crinoid Neocrinus blakei.


Author(s):  
A. V. Crewe ◽  
M. Ohtsuki

We have assembled an image processing system for use with our high resolution STEM for the particular purpose of working with low dose images of biological specimens. The system is quite flexible, however, and can be used for a wide variety of images.The original images are stored on magnetic tape at the microscope using the digitized signals from the detectors. For low dose imaging, these are “first scan” exposures using an automatic montage system. One Nova minicomputer and one tape drive are dedicated to this task.The principal component of the image analysis system is a Lexidata 3400 frame store memory. This memory is arranged in a 640 x 512 x 16 bit configuration. Images are displayed simultaneously on two high resolution monitors, one color and one black and white. Interaction with the memory is obtained using a Nova 4 (32K) computer and a trackball and switch unit provided by Lexidata.The language used is BASIC and uses a variety of assembly language Calls, some provided by Lexidata, but the majority written by students (D. Kopf and N. Townes).


Author(s):  
P. Pradère ◽  
J.F. Revol ◽  
R. St. John Manley

Although radiation damage is the limiting factor in HREM of polymers, new techniques based on low dose imaging at low magnification have permitted lattice images to be obtained from very radiation sensitive polymers such as polyethylene (PE). This paper describes the computer averaging of P4MP1 lattice images. P4MP1 is even more sensitive than PE (total end point dose of 27 C m-2 as compared to 100 C m-2 for PE at 120 kV). It does, however, have the advantage of forming flat crystals from dilute solution and no change in d-spacings is observed during irradiation.Crystals of P4MP1 were grown at 60°C in xylene (polymer concentration 0.05%). Electron microscopy was performed with a Philips EM 400 T microscope equipped with a Low Dose Unit and operated at 120 kV. Imaging conditions were the same as already described elsewhere. Enlarged micrographs were digitized and processed with the Spider image processing system.


Author(s):  
T. M. Weatherby ◽  
P.H. Lenz

Crustaceans, as well as other arthropods, are covered with sensory setae and hairs, including mechanoand chemosensory sensillae with a ciliary origin. Calanoid copepods are small planktonic crustaceans forming a major link in marine food webs. In conjunction with behavioral and physiological studies of the antennae of calanoids, we undertook the ultrastructural characterization of sensory setae on the antennae of Pleuromamma xiphias.Distal mechanoreceptive setae exhibit exceptional behavioral and physiological performance characteristics: high sensitivity (<10 nm displacements), fast reaction times (<1 msec latency) and phase locking to high frequencies (1-2 kHz). Unusual structural features of the mechanoreceptors are likely to be related to their physiological sensitivity. These features include a large number (up to 3000) of microtubules in each sensory cell dendrite, arising from or anchored to electron dense rods associated with the ciliary basal body microtubule doublets. The microtubules are arranged in a regular array, with bridges between and within rows. These bundles of microtubules extend far into each mechanoreceptive seta and terminate in a staggered fashion along the dendritic membrane, contacting a large membrane surface area and providing a large potential site of mechanotransduction.


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