Surface electron microscopy

Characterization of the Surfaces of Catalysts Measurements of the Density of Surface Faces for High Surface Area Supports. - It has always been a tenet of theories of catalysis that certain reactions will proceed at different rates on different surface planes of the same crystal. Experiments with metal single crystals have vindicated this view by showing that the rate of hydrogenolysis of ethane on a nickel surface will vary from one plane to another. In contrast the rate of methanation remains constant for the same planes.4 Because of this structure sensitivity of catalytic processes there is a requirement for methods of determining the number of each of the different planes which a catalyst and its support may expose at their surfaces. Electron microscopy studies of 5nm Pt particles supported upon graphite show them to be cubo-octahedra with surfaces bound by (111) and (100) planes.5 Similar studies of Pd and Pt prepared by evaporation reveal square pyramids of size 60-200 A bounded by incomplete (111) faces.6... 

Fig. 2 a Empty fruit bunch fiber before pretreatment, b Empty fruit bunch fiber after bleaching processes, c Surface Electron microscopy of empty fruit bunch fiber before pielieatment (x500 magnification), d Surface electron microscopy of treated fibre (x500 magnification)... 

Figire 43 Surface electron microscopy (left-hand side, 1 gm x 1 gm) and TEM (right-hand side) of the surface morphology of a block copolymer thin film with variable thickness. The thickness decreases from A to D. A scheme of the cross section of the film is presented at the bottom. Reprinted with permission from Fasolka, M. J. etal. Phys. Rev. Lett. 1997, 79(16), 3018. 8... 

SEM Scanning electron microscopy [7, 10, 14] A beam of electrons scattered from a surface is focused Surface morphology... 

Protein adsorption has been studied with a variety of techniques such as ellipsome-try [107,108], ESCA [109], surface forces measurements [102], total internal reflection fluorescence (TIRE) [103,110], electron microscopy [111], and electrokinetic measurement of latex particles [112,113] and capillaries [114], The TIRE technique has recently been adapted to observe surface diffusion [106] and orientation [IIS] in adsorbed layers. These experiments point toward the significant influence of the protein-surface interaction on the adsorption characteristics [105,108,110]. A very important interaction is due to the hydrophobic interaction between parts of the protein and polymeric surfaces [18], although often electrostatic interactions are also influential [ 116]. Protein desorption can be affected by altering the pH [117] or by the introduction of a complexing agent [118]. 

The specific surface area of a solid is one of the first things that must be determined if any detailed physical chemical interpretation of its behavior as an adsorbent is to be possible. Such a determination can be made through adsorption studies themselves, and this aspect is taken up in the next chapter there are a number of other methods, however, that are summarized in the following material. Space does not permit a full discussion, and, in particular, the methods that really amount to a particle or pore size determination, such as optical and electron microscopy, x-ray or neutron diffraction, and permeability studies are largely omitted. 

It has also been shown that sufiBcient surface self-diflfiision can occur so that entire step edges move in a concerted maimer. Although it does not achieve atomic resolution, the low-energy electron microscopy (LEEM) technique allows for the observation of the movement of step edges in real time [H]. LEEM has also been usefiil for studies of epitaxial growth and surface modifications due to chemical reactions. 

The most popular of the scanning probe tecimiques are STM and atomic force microscopy (AFM). STM and AFM provide images of the outemiost layer of a surface with atomic resolution. STM measures the spatial distribution of the surface electronic density by monitoring the tiumelling of electrons either from the sample to the tip or from the tip to the sample. This provides a map of the density of filled or empty electronic states, respectively. The variations in surface electron density are generally correlated with the atomic positions. 

Otlier fonns of microscopy have been used to evaluate nanocrystals. Scanning electron microscopy (SEM), while having lower resolution tlian TEM, is able to image nanoparticles on bulk surfaces, for direct visualization of... 

A completely new method of determining siufaces arises from the enormous developments in electron microscopy. In contrast to the above-mentioned methods where the surfaces were calculated, molecular surfaces can be determined experimentally through new technologies such as electron cryomicroscopy [188]. Here, the molecular surface is limited by the resolution of the experimental instruments. Current methods can reach resolutions down to about 10 A, which allows the visualization of protein structures and secondary structure elements [189]. The advantage of this method is that it can be apphed to derive molecular structures of maaomolecules in the native state. 

Specific surface area of carbon blacks before and after graphitization, determined by electron microscopy (A,) end by nitrogen adsorption (A ]t... 

Comparison of specific surface of anatase and zinc oxide determined by electron microscopy A ) and by nitrogen adsorption A )... 

The specific surface estimated from particle size determined by electron microscopy was I lOm g . 

Physical testing appHcations and methods for fibrous materials are reviewed in the Hterature (101—103) and are generally appHcable to polyester fibers. Microscopic analyses by optical or scanning electron microscopy are useful for evaluating fiber parameters including size, shape, uniformity, and surface characteristics. Computerized image analysis is often used to quantify and evaluate these parameters for quaUty control. 

Characterization. When siHca gel is used as an adsorbent, the pore stmcture determines the gel adsorption capacity. Pores are characterized by specific surface area, specific pore volume (total volume of pores per gram of solid), average pore diameter, pore size distribution, and the degree to which entrance to larger pores is restricted by smaller pores. These parameters are derived from measuring vapor adsorption isotherms, mercury intmsion, low angle x-ray scattering, electron microscopy, gas permeabiHty, ion or molecule exclusion, or the volume of imbibed Hquid (1). 

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