Particle electron microscopy

To obtain more detailed information on the ultrastructure of lipid dispersions and the morphology of the particles, electron microscopy is usually performed on replicas of freeze fractured or on frozen hydrated samples. These techniques aim to preserve the liquid-like state of the sample and the organization of the dispersed structures during preparation. By using special devices, the sample is frozen so quickly that all liquid structures, including the dispersion medium, solidify in an amorphous state. 

The capability of FFF to produce high-resolution (and thus detailed) size distribution curves in the submicrometer-size range is particularly important. Submicrometer-size distributions extending down to 5-nm diameter, as obtained from flow FFF, are generally very difficult to obtain by other techniques. For such small particles, electron microscopy is a primary tool, but electron microscopy can be used even more beneficially in combination with FFF, particularly if aggregation or other morphological features of the sample materials must be examined. 

Several techniques are commonly used to measure the size distributions of metal colloid particles. Electron microscopy. X-ray diffi ction, and small angle X-ray scattering are the most commonly used, although dassical methods such as sedimentation rates are sometimes reported. The techniques whidi have been extensively applied to the sizing of polymer colloids and emulsions, [183] such as light scattering and neutron scattering, have been only rarely applied to the characterization of metal sols. [103, 151, 153, 184]... 

In order to get information on wear mechanisms, it is necessary to complement the determination of wear volume by a structural characterization of the worn surface. Friction and wear cause characteristic changes of surface topography and of the microstructure in a thin zone below the rubbing surface, which can give information on prevailing wear mechanisms. Additional information is obtained by an analysis of the size and composition of the wear particles. Electron microscopy (SEM, TEM) and surface analysis methods (AES, XPS, etc) are generally used for this purpose. 

Shape of particle Electronic microscopy Mostly spherical but others... 

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. 

Electron microscopy (see section B1.18) is very valuable in characterizing particles (see, for instance, figure C2.6.1). The suspension stmcture is, of course, not represented well because of tire vacuum conditions in tire microscope. This can be overcome using environmental SEM [241. 

Figure C2.17.4. Transmission electron micrograph of a field of Zr02 (tetragonal) nanocrystals. Lower-resolution electron microscopy is useful for characterizing tire size distribution of a collection of nanocrystals. This image is an example of a typical particle field used for sizing puriDoses. Here, tire nanocrystalline zirconia has an average diameter of 3.6 nm witli a polydispersity of only 5% 1801.

Flueli M, Buffat P A and Borel J P 1988 Real time observation by high resolution electron microscopy (HREM) of the coalescence of small gold particles in the electron beam Surf. Sc/. 202 343... 

Pocza J F, Barna A and Barna P B 1969 Formation processes of vacuum deposited indium films and thermodynamical properties of submicroscopic particles observed by in situ electron microscopy J. Vac. Sc/. Techno . 6 472... 

Comparison of particle diameter of colloidal silica by electron microscopy (cf,). by nitrogen adsorption (d ) and by light scattering (d,)... 

The slit-shaped model has come into prominence in recent years, as electron microscopy has revealed the prevalence of solids composed of platelike particles the technique, indeed, has now developed to the point where it is possible to identify the presence of slit-shaped pores, and even to measure their width. In the ideal case where the sides of the slit are truly planar and parallel, the hysteresis takes an extreme form since the mean radius of curva-... 

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

Additional information on elastomer and SAN microstmcture is provided by C-nmr analysis (100). Rubber particle composition may be inferred from glass-transition data provided by thermal or mechanochemical analysis. Rubber particle morphology as obtained by transmission or scanning electron microscopy (101) is indicative of the ABS manufacturing process (77). (See Figs. 1 and 2.)... 

Particle Size. Wet sieve analyses are commonly used in the 20 )J.m (using microsieves) to 150 )J.m size range. Sizes in the 1—10 )J.m range are analyzed by light-transmission Hquid-phase sedimentation, laser beam diffraction, or potentiometric variation methods. Electron microscopy is the only rehable procedure for characterizing submicrometer particles. Scanning electron microscopy is useful for characterizing particle shape, and the relation of particle shape to slurry stabiUty. 

The mechanism for coercivity in the Cr—Co—Fe alloys appears to be pinning of domain walls. The magnetic domains extend through particles of both phases. The evidence from transmission electron microscopy studies and measurement of JT, and anisotropy vs T is that the walls are trapped locally by fluctuations in saturation magnetization. 

These primary particles also contain smaller internal stmctures. Electron microscopy reveals a domain stmcture at about 0.1-p.m dia (8,15,16). The origin and consequences of this stmcture is not weU understood. PVC polymerized in the water phase and deposited on the skin may be the source of some of the domain-sized stmctures. Also, domain-sized flow units may be generated by certain unusual and severe processing conditions, such as high temperature melting at 205°C followed by lower temperature mechanical work at 140—150°C (17), which break down the primary particles further. 

In order to define the extent of emissions from automotive brakes and clutches, a study was carried out in which specially designed wear debris collectors were built for the dmm brake, the disk brake, and the clutch of a popular U.S. vehicle (1). The vehicle was driven through various test cycles to determine the extent and type of brake emissions generated under all driving conditions. Typical original equipment and aftermarket friction materials were evaluated. Brake relines were made to simulate consumer practices. The wear debris was analyzed by a combination of optical and electron microscopy to ascertain the asbestos content and its particle size distribution. It was found that more than 99.7% of the asbestos was converted to a nonfibrous form and... 

Surface Area and Permeability or Porosity. Gas or solute adsorption is typicaUy used to evaluate surface area (74,75), and mercury porosimetry is used, ia coajuactioa with at least oae other particle-size analysis, eg, electron microscopy, to assess permeabUity (76). Experimental techniques and theoretical models have been developed to elucidate the nature and quantity of pores (74,77). These iaclude the kinetic approach to gas adsorptioa of Bmaauer, Emmett, and TeUer (78), known as the BET method and which is based on Langmuir s adsorption model (79), the potential theory of Polanyi (25,80) for gas adsorption, the experimental aspects of solute adsorption (25,81), and the principles of mercury porosimetry, based on the Young-Duprn expression (24,25). 

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