Transmission electron microscopic procedure

FIGURE 19.2 Procedure for three-dimensional-transmission electron microscopic (3D-TEM) observation, composed of TEM measurements and computerized tomography to reconstruct a 3D image. (From Kohjiya, S., Kato, A., Shimanuki, J., Hasegawa, T., and Ikeda, Y., Polymer, 46, 4440, 2005. With permission.)... 

The Fe-B nanocomposite was synthesized by the so-called pillaring technique using layered bentonite clay as the starting material. The detailed procedures were described in our previous study [4]. X-ray diffraction (XRD) analysis revealed that the Fe-B nanocomposite mainly consists of Fc203 (hematite) and Si02 (quartz). The bulk Fe concentration of the Fe-B nanocomposite measured by a JOEL X-ray Reflective Fluorescence spectrometer (Model JSX 3201Z) is 31.8%. The Fe surface atomic concentration of Fe-B nanocomposite determined by an X-ray photoelectron spectrometer (Model PHI5600) is 12.25 (at%). The BET specific surface area is 280 m /g. The particle size determined by a transmission electron microscope (JOEL 2010) is from 20 to 200 nm. 

To etch away silica, carbonization product samples were treated with a mixture of concentrated sulfuric and hydrofluoric acids (5 drops of H2S04 and 1 mL of HF), boiled dry and washed with water. From the precipitate obtained were prepared dispersions in acetone, which were used to determine the size and shape of particles on a JEM100CX-II transmission electron microscope by a commonly used procedure[10]. 

Fig. 9.2. High Resolution Transmission Electron Microscopic (HRTEM) image of Au nanoparticles stabilized by dodecanethiol ligand molecules after SMAD and digestive ripening procedure. (Reprinted from Stoeva, S. et al J. Phys. Chem. B, 2003,107,7441-7448, Fig. 11(c), by permission of the American Chemical Society, copyright 2002, American Chemical Society.)...

This paper describes chemical analyses at points across individual zeolite crystals in the size range 0.1-2.0pm. The technique employed was x-ray emission spectroscopy in the scanning transmission electron microscope (STEM). Two ZSM-5 preparations were made with Si Al ratios about 10 and 40. Many particles were examined carefully to detect chemical segregation. To check the analysis procedure, particles of NaA zeolite were examined as a control. 

Morphology was studied by AFM (Solver P47) in semicontact mode using a 10 nm radius tip. Philips CM 20 transmission electron microscope operating at 200 keV was used to analyze the surface and cross-section of the samples thinned by our standard ion beam milling procedure [4]. 

Transmission Electron Microscope images were obtained on a JEOL 2010 EX instrument operated at 200 kV. This microscope provides a point resolution of 0.19 nm with the LaBe electron emitter that was used during these experiments. Sample preparation involved grinding the catalyst in a mortar and pestle, suspending it in ethanol and dipping a Cu TEM grid into the supernatant. This procedure allowed a very thin layer of the catalyst sample to... 

In considering surfaces and modified surfaces, the techniques and procedures usually used to characterize solid and surfaces are of prominent importance, such as Brunauei>-Emmett-Teller (BET) isotherms, nuclear magnetic resonance (NMR) of solids (in our case, generally Si and P), scanning electron microscope (SEM), and transmission electron microscope (TEM). 

Computer Simulation of Crack Propagation. A typical experimental procedure for investigating fracture consists in looking at the fracture surface with a scanning electron microscope (SEM) or a transmission electron microscope (TEM) (49,50). This provides us with the morphology at the time of fracture, which is useful information. However, the microscopic techniques do not tell us where and how the crack(s) which eventually led to fracture had started. 

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