Particles, transmission electron

FIG. 1.13 Spherical and cubic model particles with crystalline or amorphous microstructure (a) spherical zinc sulfide particles (transmission electron microscopy, TEM, see Section 1.6a.2a) x-ray diffraction studies show that the microstructure of these particles is crystalline (b) cubic lead sulfide particles (scanning electron microscopy, SEM, see Section 1.6a.2a) (c) amorphous spherical particles of manganese (II) phosphate (TEM) and (d) crystalline cubic cadmium carbonate particles (SEM). (Reprinted with permission of Matijevic 1993.)... 

As already discussed, the size, the shape and the dispersion are characteristic parameters of metal particles and will determine their properties. It is possible to characterize them as follows (i) The size of the metal particles (transmission electron microscopy, (TEM) [79-81], extended X-ray absorption fine structure (EXAFS) [82, 83]), (ii) their structures (X-ray diffraction (XRD), TEM), (iii) their chemical composition (TEM-EDX, elemental analysis), (iv) the chemical state of the surface and bulk metal atoms (X-ray photoelectron spectroscopy (XPS)), Mossbauer [84], thermo-programmed-reduction (TPR)), (v) chemisorption capacity toward probe molecules such as H2, O2, NO and CO (volumetric or dynamic measurements) [85-90]. 

Oxide layer thickness on particles (transmission electron microscopy (TEM)), a y. (nm) 2 18 20 22... 

Fig. Vni-3. (a) Atomic force microscope (AFM) and (b) transmission electron microscope (TEM) images of lead selenide particles grown under arachidic acid monolayers. (Pi Ref. 57.)...

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].

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.

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. 

Fig. 13. Transmission electron micrograph (tern) showing dislocations in aluminum in the region near a siUcon carbide particle, SiC. ...

Regarding a historical perspective on carbon nanotubes, very small diameter (less than 10 nm) carbon filaments were observed in the 1970 s through synthesis of vapor grown carbon fibers prepared by the decomposition of benzene at 1100°C in the presence of Fe catalyst particles of 10 nm diameter [11, 12]. However, no detailed systematic studies of such very thin filaments were reported in these early years, and it was not until lijima s observation of carbon nanotubes by high resolution transmission electron microscopy (HRTEM) that the carbon nanotube field was seriously launched. A direct stimulus to the systematic study of carbon filaments of very small diameters came from the discovery of fullerenes by Kroto, Smalley, and coworkers [1], The realization that the terminations of the carbon nanotubes were fullerene-like caps or hemispheres explained why the smallest diameter carbon nanotube observed would be the same as the diameter of the Ceo molecule, though theoretical predictions suggest that nanotubes arc more stable than fullerenes of the same radius [13]. The lijima observation heralded the entry of many scientists into the field of carbon nanotubes, stimulated especially by the un-... 

High-resolution transmission electron microscopy (HREM) is the technique best suited for the structural characterization of nanometer-sized graphitic particles. In-situ processing of fullerene-related structures may be performed, and it has been shown that carbonaceous materials transform themselves into quasi-spherical onion-like graphitic particles under the effect of intense electron irradiation[l 1],... 

Paine et al. [99] tried different stabilizers [i.e., hydroxy propylcellulose, poly(N-vinylpyrollidone), and poly(acrylic acid)] in the dispersion polymerization of styrene initiated with AIBN in the ethanol medium. The direct observation of the stained thin sections of the particles by transmission electron microscopy showed the existence of stabilizer layer in 10-20 nm thickness on the surface of the polystyrene particles. When the polystyrene latexes were dissolved in dioxane and precipitated with methanol, new latex particles with a similar surface stabilizer morphology were obtained. These results supported the grafting mechanism of stabilization during dispersion polymerization of styrene in polar solvents. 

MgO-supported model Mo—Pd catalysts have been prepared from the bimetallic cluster [Mo2Pd2 /z3-CO)2(/r-CO)4(PPh3)2() -C2H )2 (Fig. 70) and monometallic precursors. Each supported sample was treated in H2 at various temperatures to form metallic palladium, and characterized by chemisorption of H2, CO, and O2, transmission electron microscopy, TPD of adsorbed CO, and EXAFS. The data showed that the presence of molybdenum in the bimetallic precursor helped to maintain the palladium in a highly dispersed form. In contrast, the sample prepared from the monometallie precursors was characterized by larger palladium particles and by weaker Mo—Pd interactions. ... 

In 1997, a Chinese research group [78] used the colloidal solution of 70-nm-sized carboxylated latex particles as a subphase and spread mixtures of cationic and other surfactants at the air-solution interface. If the pH was sufficiently low (1.5-3.0), the electrostatic interaction between the polar headgroups of the monolayer and the surface groups of the latex particles was strong enough to attract the latex to the surface. A fairly densely packed array of particles could be obtained if a 2 1 mixture of octadecylamine and stearic acid was spread at the interface. The particle films could be transferred onto solid substrates using the LB technique. The structure was studied using transmission electron microscopy. 

Interestingly, this behavior of the reaction mixture can be prevented by employing another principle of particle stabilization steric protection. Inclusion of pegylated comonomer (PEG-AEPD) into the reaction mixture did enable the formation of nonaggregating DNA particles. It also caused the particles to form worm -like structures (as judged by transmission electron microscopy) that have previously been observed with DNA complexes formed from block copolymers of PEL and PEG [98]. 

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