Scanning electron microscopy Imaging techniques

Scanning electron microscopy with an energy-dispersive x-ray system accessory has been used to identify the composition and nature of minerals in coals and to determine the associations of minerals with each other. Examinations can be made on samples resulting from ashing techniques or whole coal. With this technique it is possible to identify the elemental components and deduce the mineral types present in coal samples. Computerized systems to evaluate scanning electron microscopy images have been developed and are useful in characterizing the minerals in coal mine dusts and in coal. 

In scanning electron microscopy, images are obtained from the low-energy secondary electrons (< 50 eV) that are emitted from the sample in response to a narrow electron beam rastered across the surface. The intensity of the secondary electrons is sensitive to the orientation of the surface, so that the resulting image indicates its topography. The technique is widely used to determine... 

Figure 6 SEM (scanning electron microscopy) image of a test pattern prepared by direct-writing EBCL and surface initiated polymerization (SIPP) of styrene. On the left, line widths of 500 to to nm of the primary patterns were directly written onto the substrate by the e-beam. Below, some text and the biphenyl structure were inscribed to demonstrate that complex structures can easily be realized by this technique. The defects observable are due to adsorption of impurities aftCT the process was completed. (Reproduced from Ref. 34. WUey-VCH, 2007.)...

Optical (larger than 1 pm) and scanning electron microscopy (SEM) techniques literally give the clearest picture of a PSD. However, analyzing the images may be tedious without image analyzers. Nevertheless, this method can be used as a check or calibration on the indirect methods. 

In contrast to many other surface analytical techniques, like e. g. scanning electron microscopy, AFM does not require vacuum. Therefore, it can be operated under ambient conditions which enables direct observation of processes at solid-gas and solid-liquid interfaces. The latter can be accomplished by means of a liquid cell which is schematically shown in Fig. 5.6. The cell is formed by the sample at the bottom, a glass cover - holding the cantilever - at the top, and a silicone o-ring seal between. Studies with such a liquid cell can also be performed under potential control which opens up valuable opportunities for electrochemistry [5.11, 5.12]. Moreover, imaging under liquids opens up the possibility to protect sensitive surfaces by in-situ preparation and imaging under an inert fluid [5.13]. 

Core-shell colloidal crystal films were prepared in three steps as outlined in Table 4.2. First, spherical submicron polystyrene particles were prepared by known methods38 39. The size of isolated polystyrene beads was 326 5 nm as determined by analysis of scanning electron microscopy (SEM) images using standard techniques. 

Atomic force microscopy (AFM) is a commonly employed imaging technique for the characterization of the topography of material surfaces. In contrast to other microscopy techniques (e.g., scanning electron microscopy), AFM provides additional quantitative surface depth information and therefore yields a 3D profile of the material surface. AFM is routinely applied for the nanoscale surface characterization of materials and has been previously applied to determine surface heterogeneity of alkylsilane thin films prepared on planar surfaces [74,75,138]. 

For the detailed study of reaction-transport interactions in the porous catalytic layer, the spatially 3D model computer-reconstructed washcoat section can be employed (Koci et al., 2006, 2007a). The structure of porous catalyst support is controlled in the course of washcoat preparation on two levels (i) the level of macropores, influenced by mixing of wet supporting material particles with different sizes followed by specific thermal treatment and (ii) the level of meso-/ micropores, determined by the internal nanostructure of the used materials (e.g. alumina, zeolites) and sizes of noble metal crystallites. Information about the porous structure (pore size distribution, typical sizes of particles, etc.) on the micro- and nanoscale levels can be obtained from scanning electron microscopy (SEM), transmission electron microscopy ( ), or other high-resolution imaging techniques in combination with mercury porosimetry and BET adsorption isotherm data. This information can be used in computer reconstruction of porous catalytic medium. In the reconstructed catalyst, transport (diffusion, permeation, heat conduction) and combined reaction-transport processes can be simulated on detailed level (Kosek et al., 2005). 

Figure 13.11—Scanning electron microscopy (SEM) accompanied by X-ray fluorescence analysis. Secondary electron image of a cross-section of a supraconducting polycrystalline ceramic with oriented grains of oxide BiPbiSriCaiCurO, (Philips instrument, model XL30FEG). Energy emission spectra corresponding to the matrix and to a 5 pm-long inclusion (bottom). It should be noted that it is possible with this technique to obtain the composition at a precise point on the sample (Link-Oxford analyser) (study by V. Rouessac, reproduced by permission of CRISMAT. University of Caen).

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