From colloidal particles to supported catalysts: a comprehensive study of palladium oxide hydrosols deposited on alumina.

Author(s):  
B. Didillon ◽  
E. Merlen ◽  
T. Pagès ◽  
D. Uzio
2008 ◽  
Vol 105 (40) ◽  
pp. 15241-15246 ◽  
Author(s):  
Ilkeun Lee ◽  
Ricardo Morales ◽  
Manuel A. Albiter ◽  
Francisco Zaera

Colloidal and sol-gel procedures have been used to prepare heterogeneous catalysts consisting of platinum metal particles with narrow size distributions and well defined shapes dispersed on high-surface-area silica supports. The overall procedure was developed in three stages. First, tetrahedral and cubic colloidal metal particles were prepared in solution by using a procedure derived from that reported by El-Sayed and coworkers [Ahmadi TS, Wang ZL, Green TC, Henglein A, El-Sayed MA (1996) Science 272:1924–1926]. This method allowed size and shape to be controlled independently. Next, the colloidal particles were dispersed onto high-surface-area solids. Three approaches were attempted: (i) in situ reduction of the colloidal mixture in the presence of the support, (ii) in situ sol-gel synthesis of the support in the presence of the colloidal particles, and (iii) direct impregnation of the particles onto the support. Finally, the resulting catalysts were activated and tested for the promotion of carbon–carbon double-bond cis-trans isomerization reactions in olefins. Our results indicate that the selectivity of the reaction may be controlled by using supported catalysts with appropriate metal particle shapes.


Author(s):  
F. A. Heckman ◽  
E. Redman ◽  
J.E. Connolly

In our initial publication on this subject1) we reported results demonstrating that contrast is the most important factor in producing the high image quality required for reliable image analysis. We also listed the factors which enhance contrast in order of the experimentally determined magnitude of their effect. The two most powerful factors affecting image contrast attainable with sheet film are beam intensity and KV. At that time we had only qualitative evidence for the ranking of enhancing factors. Later we carried out the densitometric measurements which led to the results outlined below.Meaningful evaluations of the cause-effect relationships among the considerable number of variables in preparing EM negatives depend on doing things in a systematic way, varying only one parameter at a time. Unless otherwise noted, we adhered to the following procedure evolved during our comprehensive study:Philips EM-300; 30μ objective aperature; magnification 7000- 12000X, exposure time 1 second, anti-contamination device operating.


Author(s):  
A. Singh ◽  
A. Dykeman ◽  
J. Jarrelf ◽  
D. C. Villeneuve

Hexachlorobenzene (HCB), a persistent and mobile organochlorine pesticide, occurs in environment. HCB has been shown to be present in human follicular fluid. An objective of the present report, which is part of a comprehensive study on reproductive toxicity of HCB, was to determine the cytologic effects of the compound on ovarian follicles in a primate model.Materials and Methods. Eight Cynomolgus monkeys were housed under controlled conditions at Animal facility of Health and Welfare, Ottawa. Animals were orally administered gelatin capsules containing HCB mixed with glucose in daily dosages of 0.0 or 10 mg/kg b.w. for 90 days; the former was the control group. On the menstrual period following completion of dosing, the monkeys underwent an induction cycle of superovulation. At necropsy, one-half of an ovary from each animal was diced into ca. 2- to 3-mm cubed specimens that were fixed by immersion in 2.5% glutaraldehyde in 0.1 M cacodylate buffer (pH 7.3). Subsequent procedures followed to obtain thin sections that were examined in a Hitachi H-7000 electron microscope have been described earlier.


Author(s):  
L. V. Leak ◽  
J. F. Burke

The vital role played by the lymphatic capillaries in the transfer of tissue fluids and particulate materials from the connective tissue area can be demonstrated by the rapid removal of injected vital dyes into the tissue areas. In order to ascertain the mechanisms involved in the transfer of substances from the connective tissue area at the ultrastructural level, we have injected colloidal particles of varying sizes which range from 80 A up to 900-mμ. These colloidal particles (colloidal ferritin 80-100A, thorium dioxide 100-200 A, biological carbon 200-300 and latex spheres 900-mμ) are injected directly into the interstitial spaces of the connective tissue with glass micro-needles mounted in a modified Chambers micromanipulator. The progress of the particles from the interstitial space into the lymphatic capillary lumen is followed by observing tissues from animals (skin of the guinea pig ear) that were injected at various time intervals ranging from 5 minutes up to 6 months.


Author(s):  
Michio Ashida ◽  
Yasukiyo Ueda

An anodic oxide film is formed on aluminum in an acidic elecrolyte during anodizing. The structure of the oxide film was observed directly by carbon replica method(l) and ultra-thin sectioning method(2). The oxide film consists of barrier layer and porous layer constructed with fine hexagonal cellular structure. The diameter of micro pores and the thickness of barrier layer depend on the applying voltage and electrolyte. Because the dimension of the pore corresponds to that of colloidal particles, many metals deposit in the pores. When the oxide film is treated as anode in emulsion of polyelectrolyte, the emulsion particles migrate onto the film and deposit on it. We investigated the behavior of the emulsion particles during electrodeposition.Aluminum foils (99.3%) were anodized in either 0.25M oxalic acid solution at 30°C or 3M sulfuric acid solution at 20°C. After washing with distilled water, the oxide films used as anode were coated with emulsion particles by applying voltage of 200V and then they were cured at 190°C for 30 minutes.


Author(s):  
D. L. Rohr ◽  
S. S. Hecker

As part of a comprehensive study of microstructural and mechanical response of metals to uniaxial and biaxial deformations, the development of substructure in 1100 A1 has been studied over a range of plastic strain for two stress states.Specimens of 1100 aluminum annealed at 350 C were tested in uniaxial (UT) and balanced biaxial tension (BBT) at room temperature to different strain levels. The biaxial specimens were produced by the in-plane punch stretching technique. Areas of known strain levels were prepared for TEM by lapping followed by jet electropolishing. All specimens were examined in a JEOL 200B run at 150 and 200 kV within 24 to 36 hours after testing.The development of the substructure with deformation is shown in Fig. 1 for both stress states. Initial deformation produces dislocation tangles, which form cell walls by 10% uniaxial deformation, and start to recover to form subgrains by 25%. The results of several hundred measurements of cell/subgrain sizes by a linear intercept technique are presented in Table I.


Author(s):  
F.E. Hossler ◽  
M.I. McKamey ◽  
F.C. Monson

A comprehensive study of the microvasculature of the normal rabbit bladder, revealed unusual "capillary glomeruli" along the lateral walls. Here they are characterized as hemal lymph nodes using light microscopy, SEM, TEM, ink injection, and vascular casting.Bladders were perfused via a cannula placed in the abdominal aorta with either 2% glutaraldehyde in 0.1M cacodylate buffer (pH 7.4) for fixation, 10% India ink in 0.9% saline and 0.1M phosphate (pH 7.4) for vessel tracing, or resin (Mercoximethylmethacrylate: catalyst, 4:1:0.3; Ladd Research Industries) for vascular corrosion casting. Infusion pressure was 100mm Hg. Fixed tissue was sectioned from epon-araldyte resin, and stained with toluidine blue for light microscopy, and lead and uranium for TEM. Ink injected tissue was photographed directly from saline-filled bladders illuminated from below. Resin-filled tissue was macerated in 5% KOH and distilled water. Casts were critical point dried, sputter coated with goldpalladium, and examined by routine SEM at 10 KV.


Author(s):  
J. Liu ◽  
M. Pan ◽  
G. E. Spinnler

Small metal particles have peculiar chemical and physical properties as compared to bulk materials. They are especially important in catalysis since metal particles are common constituents of supported catalysts. The structural characterization of small particles is of primary importance for the understanding of structure-catalytic activity relationships. The shape and size of metal particles larger than approximately 5 nm in diameter can be determined by several imaging techniques. It is difficult, however, to deduce the shape of smaller metal particles. Coherent electron nanodiffraction (CEND) patterns from nano particles contain information about the particle size, shape, structure and defects etc. As part of an on-going program of STEM characterization of supported catalysts we report some preliminary results of CEND study of Ag nano particles, deposited in situ in a UHV STEM instrument, and compare the experimental results with full dynamical simulations in order to extract information about the shape of Ag nano particles.


Author(s):  
R. L. Freed ◽  
M. J. Kelley

The commercial introduction of Pt-Re supported catalysts to replace Pt alone on Al2O3 has brought improvements to naphtha reforming. The bimetallic catalyst can be operated continuously under conditions which lead to deactivation of the single metal catalyst by coke formation. Much disagreement still exists as to the exact nature of the bimetallic catalyst at a microscopic level and how it functions in the process so successfully. The overall purpose of this study was to develop the materials characterization tools necessary to study supported catalysts. Specifically with the Pt-Re:Al2O3 catalyst, we sought to elucidate the elemental distribution on the catalyst.


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