Electronic particle sizing

Figure 3. Pints of mean particle size versus standard deviation of two prepared mixtures of standards analyzed by selected automated electronic particle size analysers (from Syvitski et al 1991a). The expected value is shown with a black box. S SediGraph C. Coulter Counter M Malvern laser panicle. sizer G Galai CIS-1, L Lumosed photosedimentometer lA Image analysis (Syvitski et al.. 1991a).

One of the earliest electronic particle sizing devices available was developed in the late-1940 s and was originally designed to count blood cells (Coulter, 1956). The Coulter Counter rapidly gained immense popularity in many industry and research applications, including the Earth sciences, and is still a very commonly used instrument in sedimento-logical laboratories. The Coulter Principle is sufficiently well established to be included in many A.S.T.M. (American Society for Testing Materials) reference method standards. 

There is considerable technique required in appropriately interpreting the data from electronic particle size analyzers. Vendors can be quite helpful in the development of a measurement procedure, but some experimentation should be expected with each new system. 

Figure C2.17.2. Transmission electron micrograph of a gold nanoneedle. Inverse micelle environments allow for a great deal of control not only over particle size, but also particle shape. In this example, gold nanocrystals were prepared using a photolytic method in surfactant-rich solutions the surfactant interacts strongly with areas of low curvature, thus continued growth can occur only at the sharjD tips of nanocrystals, leading to the fonnation of high-aspect-ratio nanostmctures [52].

One of the most important uses of specific surface determination is for the estimation of the particles size of finely divided solids the inverse relationship between these two properties has already been dealt with at some length. The adsorption method is particularly relevant to powders having particle sizes below about 1 pm, where methods based on the optical microscope are inapplicable. If, as is usually the case, the powder has a raiige of particle sizes, the specific surface will lead to a mean particle size directly, whereas in any microscopic method, whether optical or electron-optical, a large number of particles, constituting a representative sample, would have to be examined and the mean size then calculated. 

Most tests of the validity of the BET area have been carried out with finely divided solids, where independent evaluation of the surface area can be made from optical microscopic or, more often, electron microscopic observations of particle size, provided the size distribution is fairly narrow. As already explained (Section 1.10) the specific surface obtained in this way is related to the mean projected diameter through the equation... 

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

Powder Preparation. The goal in powder preparation is to achieve a ceramic powder which yields a product satisfying specified performance standards. Examples of the most important powder preparation methods for electronic ceramics include mixing/calcination, coprecipitation from solvents, hydrothermal processing, and metal organic decomposition. The trend in powder synthesis is toward powders having particle sizes less than 1 p.m and Httie or no hard agglomerates for enhanced reactivity and uniformity. Examples of the four basic methods are presented in Table 2 for the preparation of BaTiO powder. Reviews of these synthesis techniques can be found in the Hterature (2,5). 

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. 

A = irnD ) where D is the atomic or molecular particle size. The number of electrons within a Debye sphere, A/, around an ion is then... 

Microscopic identification models ate similar to the CMB methods except that additional information is used to distinguish the source of the aerosol. Such chemical or morphological data include particle size and individual particle composition and are often obtained by electron or optical microscopy. 

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). 

To achieve low stress embedding material, low modulus material such as siUcones (elastomers or gels) and polyurethanes are usually used. Soft-domain elastomeric particles are usually incorporated into the hard (high modulus) materials such as epoxies and polyimides to reduce the stress of embedding materials. With the addition of the perfect particle size, distribution, and loading of soft domain particles, low stress epoxy mol ding compounds have been developed as excellent embedding materials for electronic appHcations. 

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