Transmission electron microscopy films

Transmission Electron Microscopy. Films of all samples designated R were obtained by evaporation of toluene from solutions of the block copolymers and were observed without staining using a Hitachi Hu-125 or a JEOL JEM 100 S electron microscope. Methods of preparing the films have been described previously (24). So far, we have obtained evidence for microphase separation in only the four highest molecular-weight samples by TEM. We have not obtained continuous films of the lower molecular-weight samples we plan to examine sections of these samples later. Because of the very small compatibility of styrene and polydimethylsiloxane, however, we expect phase separation in all of these samples. 

Transmission electron microscopy (TEM) can resolve features down to about 1 nm and allows the use of electron diffraction to characterize the structure. Since electrons must pass through the sample however, the technique is limited to thin films. One cryoelectron microscopic study of fatty-acid Langmuir films on vitrified water [13] showed faceted crystals. The application of TEM to Langmuir-Blodgett films is discussed in Chapter XV. 

Figure 6 High-resolution transmission electron microscopy image of an epitaxial thin film of Y Ba2Cu307 j, grown on LaAI03, shown in cross section. (Courtesy of T. E. MKchell, Los Alamos National Laboratory)...

Alternatives to XRD include transmission electron microscopy (TEM) and diffraction, Low-Energy and Reflection High-Energy Electron Diffraction (LEED and RHEED), extended X-ray Absorption Fine Structure (EXAFS), and neutron diffraction. LEED and RHEED are limited to surfaces and do not probe the bulk of thin films. The elemental sensitivity in neutron diffraction is quite different from XRD, but neutron sources are much weaker than X-ray sources. Neutrons are, however, sensitive to magnetic moments. If adequately large specimens are available, neutron diffraction is a good alternative for low-Z materials and for materials where the magnetic structure is of interest. 

Usually, the molecular strands are coiled in the glassy polymer. They become stretched when a crack arrives and starts to build up the deformation zone. Presumably, strain softened polymer molecules from the bulk material are drawn into the deformation zone. This microscopic surface drawing mechanism may be considered to be analogous to that observed in lateral craze growth or in necking of thermoplastics. Chan, Donald and Kramer [87] observed by transmission electron microscopy how polymer chains were drawn into the fibrils at the craze-matrix-interface in PS films [92]. One explanation, the hypothesis of devitrification by Gent and Thomas [89] was set forth as early as 1972. 

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. 

Khmenkov M, Nepijko S, Kuhlenbeck H, Baiimer M, Schldgl R, Ereund H-J. 1997. The structure of Pt-aggregates on a supported thin aluminum oxide film in comparison with unsupported alumina a transmission electron microscopy study. Surf Sci 391 27-36. 

It has been found that various material properties are thickness-dependent. Raman experiments show a dependence on the type of substrate (glass, c-Si, stainless steel, ITO on glass) and on the thickness (up to 1 /nm) of the films [392,393]. Recent transmission electron microscopy (TEM) results also show this [394]. This is in contrast to other results, where these effects are negligible for thicknesses larger than 10 nm [395, 396], as is also confirmed by ellipsometry [397] and IR absorption [398] studies. 

The use of lightly crosslinked polymers did result in hydrophilic surfaces (contact angle 50°, c-PI, 0.2 M PhTD). However, the surfaces displayed severe cracking after 5 days. Although qualitatively they appeared to remain hydrophilic, reliable contact angle measurements on these surfaces were impossible. Also, the use of a styrene-butadiene-styrene triblock copolymer thermoplastic elastomer did not show improved permanence of the hydrophilicity over other polydienes treated with PhTD. The block copolymer film was cast from toluene, and transmission electron microscopy showed that the continuous phase was the polybutadiene portion of the copolymer. Both polystyrene and polybutadiene domains are present at the surface. This would probably limit the maximum hydrophilicity obtainable since the RTD reagents are not expected to modify the polystyrene domains. 

High Resolution Transmission Electron Microscopy (HRTEM, Philips CM20, 200 kV) was applied to get structural and nanotextural information on the fibers, by imaging the profile of the aromatic carbon layers in the 002-lattice fringe mode. A carbon fiber coated with pyrolytic carbon was incorporated in epoxy resin and a transverse section obtained by ultramicrotomy was deposited on a holey carbon film. An in-house made image analysis procedure was used to get quantitative data on the composite. 

Reaney, I. M. Brooks, K. Klissurka, R. Pawlaczyk, C. Setter, N. 1994. Use of transmission electron microscopy for the characterization of rapid thermally annealed solution-gel, lead zirconate titanate films. /. Am. Ceram. Soc. 77 1209-1216. 

The transmission electron microscopy (TEM) images of a two-layer Tl-1223 film are shown in Fig. 7.12, which confirms the epitaxial nature of the annealed electrodeposited films. All films showed a significant amount of intergrowth, as shown by a high-resolution transmission electron microscopic (HRTEM) measurement in Figs. 7.12c and d of a representative two-layer... 

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