Transmission electron microscopy particles

Keywords carbon nanoparticles, carbon nanotubes electrochemical treatment transmission electron microscopy particle size. 

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. 

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]. 

Determined by inductively coupled plasma-mass spectrometry of acid digested catalyst samples Calculated from X-ray diffraction peak broadening at (101) foranatase and (110) formtile TiOa Mean particle diameter measured from transmission electron microscopy pictures of gold catalysts... 

The properties of titania particles were investigated using X-ray diffraction (XRD, Model D/MAX-RB, Rigaku Ltd.), scanning electron microscopy (SEM, Model 535M, Philips Ltd.), transmission electron microscopy (TEM, Model 2000EX, JEOL Ltd.). The crystallite sizes were estimated by Scherrer s equation and the composition of rutile phase in titania were estimated from the respective integrated XRD peak intensities. 

Thus, the interaction of the primary beam with the sample provides a wealth of information on morphology, crystallography and chemical composition. Using transmission electron microscopy to make a projection of the sample density is a routine way to study particle sizes in catalysts. 

Transmission electron microscopy is one of the techniques most often used for the characterization of catalysts. In general, detection of supported particles is possible, provided that there is sufficient contrast between particles and support - a limitation that may impede applications of TEM on well-dispersed supported oxides. The determination of particle sizes or of distributions therein is now a routine matter, although it rests on the assumption that the size of the imaged particle is truly proportional to the size of the actual particle and that the detection probability is the same for all particles, independent of their dimensions. 

Figure S.1S. Upper Equilibrium polyhedrons of metal particles on a support for different combinations of free energies of surfaces and interfaces. Lower Transmission electron microscopy of structures obtained by depositing 5-10 ML of Pd on a MgO surface. [Adapted from www.fysik.dtu.dk/CAMP, and C.R. Henry, Surf. Sci. Rep. 21 (1998) l.j...

However, in more recent times science has made rapid strides in this direction. It is now possible to use EXAFS in situ during a catalytic reaction to examine the average coordination of metal atoms in the small particles which often exist in precious metal catalysts [2]. High resolution transmission electron microscopy has evolved to the level of atomic resolution, but can only be used ex-situ, or in situ with moderate pressures when special cells are fitted [3]. 

The picture of cement microstructure that now emerges is of particles of partially degraded glass embedded in a matrix of calcium and aluminium polyalkenoates and sheathed in a layer of siliceous gel probably formed just outside the particle boundary. This structure (shown in Figure 5.17) was first proposed by Wilson Prosser (1982, 1984) and has since been confirmed by recent electron microscopic studies by Swift Dogan (1990) and Hatton Brook (1992). The latter used transmission electron microscopy with high resolution to confirm this model without ambiguity. 

Crystalline phases (truncated octahedra) of 5 nm silver particles, thiolate protected as well, have been detected by means of high-resolution transmission electron microscopy (HRTEM) [26-28]. Three-dimensional architectures of 5-6 nm thiolate-stabilized gold particles have also been described [29]. Several other reports on 3D superlattices of metal nanoparticles have become known during the last few years [30-33]. 

Lastly, gold supported on Mg(OH)2 is very active for CO oxidation even at 200 K [30]. However, it suddenly died after 4 months. Transmission electron microscopy could not clarify the reason because no appreciable change in particle diameter was observed. X-ray scattering due to gold clusters was measured experimentally. The... 

Transmission electron microscopy for [Pd/l]coii reveals the presence of small spherical but in some cases agglomerated particles of ca. 4 nm mean size, and wide angle X-ray scattering analyses evidence the fee structure of bulk palladium [44] (Figure 1). 

Figure 15.1 High resolution transmission electron microscopy images (HR-TEM) of 5 wt% Pd (a) and 50 wt% Pt-Ru (b) particles supported on carbon supports of the Sibunit family with surface areas of about 6m g (a) and 72m g (b). (c) Fourier-transformed image of (b). ((a) Reprinted from Pronkin et al. [2007], Copyright 2007, with permission from Elsevier, (b) and (c) reprinted from Gavrilov et al. [2007]—Reproduced by permission of the PCCP Owner Societies.)...

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