Transmission electron microscopy development

The history of EM (for an overview see table Bl.17,1) can be interpreted as the development of two concepts the electron beam either illuminates a large area of tire sample ( flood-beam illumination , as in the typical transmission electron microscope (TEM) imaging using a spread-out beam) or just one point, i.e. focused to the smallest spot possible, which is then scaimed across the sample (scaiming transmission electron microscopy (STEM) or scaiming electron microscopy (SEM)). In both situations the electron beam is considered as a matter wave interacting with the sample and microscopy simply studies the interaction of the scattered electrons. 

Small needle-shaped single crystals were examined by transmission electron microscopy (TEM) and electron diffraction (ED) (see Fig. 16-17). The results show that the crystals are elongated along the b-axis, which is the direction of weak intermolecular n-n interactions, and have a well-developed (ab) top surface. It corresponds to the surface of aliphatic tails (direction of weak intermolecular interactions). There are indications of displacement of successive ( / )-laycrs along the fl-axis, in line with the other signs of disorder in the aliphatic layer. 

Recent demands for polymeric materials request them to be multifunctional and high performance. Therefore, the research and development of composite materials have become more important because single-polymeric materials can never satisfy such requests. Especially, nanocomposite materials where nanoscale fillers are incorporated with polymeric materials draw much more attention, which accelerates the development of evaluation techniques that have nanometer-scale resolution." To date, transmission electron microscopy (TEM) has been widely used for this purpose, while the technique never catches mechanical information of such materials in general. The realization of much-higher-performance materials requires the evaluation technique that enables us to investigate morphological and mechanical properties at the same time. AFM must be an appropriate candidate because it has almost comparable resolution with TEM. Furthermore, mechanical properties can be readily obtained by AFM due to the fact that the sharp probe tip attached to soft cantilever directly touches the surface of materials in question. Therefore, many of polymer researchers have started to use this novel technique." In this section, we introduce the results using the method described in Section 21.3.3 on CB-reinforced NR. 

There is great interest in developing molecular precursors for boron-nitrogen polymers and boron nitride solid state materials, and one general procedure is described in this report. Combinations of B-trichloroborazene and hexamethyldisilazane lead to formation of a gel which, upon thermolysis, gives hexagonal boron nitride. The BN has been characterized by infrared spectroscopy, x-ray powder diffraction and transmission electron microscopy. 

Many hydrogenation and polymerization reactions in the chemical industry are carried out with liquid-phase reactants. An example is the hydrogenation of aliphatic dinitriles to produce diamines (108,109), which are subsequently converted with adipic acid in solution and polymerized to produce linear polyamides, including nylon 6,6. Recently, the development of wet-environmental transmission electron microscopy (wet-ETEM) for direct nanoscale probing of... 

Transmission electron microscopy (TEM) is a powerful and mature microstructural characterization technique. The principles and applications of TEM have been described in many books [16 20]. The image formation in TEM is similar to that in optical microscopy, but the resolution of TEM is far superior to that of an optical microscope due to the enormous differences in the wavelengths of the sources used in these two microscopes. Today, most TEMs can be routinely operated at a resolution better than 0.2 nm, which provides the desired microstructural information about ultrathin layers and their interfaces in OLEDs. Electron beams can be focused to nanometer size, so nanochemical analysis of materials can be performed [21]. These unique abilities to provide structural and chemical information down to atomic-nanometer dimensions make it an indispensable technique in OLED development. However, TEM specimens need to be very thin to make them transparent to electrons. This is one of the most formidable obstacles in using TEM in this field. Current versions of OLEDs are composed of hard glass substrates, soft organic materials, and metal layers. Conventional TEM sample preparation techniques are no longer suitable for these samples [22-24], Recently, these difficulties have been overcome by using the advanced dual beam (DB) microscopy technique, which will be discussed later. 

The important role Transmission Electron Microscopy (TEM) can play in this process is demonstrated on the development of an oxidation catalyst for the production of acrylic acid. Acrylic acid is produced by BASF in quantities of several 100.000 tons per year in a two step gas phase oxidation process starting from propene, which is oxidised to acrolein in the first step and then further oxidised to acrylic acid in a second step, each step requiring a special developed catalyst. Acrylic acid is used as a base material for the production of superabsorbents for nappies, dispersions and emulsions for adhesives and construction materials. 

Roster, A.J., Ziese, U., Verkleij, A.J., Janssen, A.H., de Graaf J., Geus, J.W., and de Jong, K.P. (2000) Development and application of 3-dimensional transmission electron microscopy (3D-TEM) for the characterization of metal-zeolite catalyst systems. Stud. 

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