Spectroscopy Scanning Transmission Electron

The scanning transmission electron microscope (STEM) was used to directly observe nm size crystallites of supported platinum, palladium and first row transition metals. The objective of these studies was to determine the uniformity of size and mass of these crystallites and when feasible structural features. STEM analysis and temperature programmed desorption (TPD) of hydrogen Indicate that the 2 nm platinum crystallites supported on alumina are uniform In size and mass while platinum crystallites 3 to 4 nm in size vary by a factor of three-fold In mass. Analysis by STEM of platinum-palladium dn alumina established the segregation of platinum and palladium for the majority of crystallites analyzed even after exposure to elevated temperatures. Direct observation of nickel, cobalt, or iron crystallites on alumina was very difficult, however, the use of direct elemental analysis of 4-6 nm areas and real time Imaging capabilities of up to 20 Mx enabled direct analyses of these transition metals to be made. Additional analyses by TPD of hydrogen and photoacoustic spectroscopy (PAS) were made to support the STEM observations. 

There are two types of electron energy loss spectroscopy currently in use. The first of these is found in scanning transmission electron microscopes. As indicated in Figure 5.1, compositional information may be obtained in the TEM by measuring the energy loss of the inelastically scattered electrons transmitted through a thin specimen. 

Analytical electron microscopy of individual catalyst particles provides much more information than just particle size and shape. The scanning transmission electron microscope (STEM) with analytical facilities allows chemical analysis and electron diffraction patterns to be obtained from areas on the order of lOnm in diameter. In this paper, examples of high spatial resolution chemical analysis by x-ray emission spectroscopy are drawn from supported Pd, bismuth and ferric molybdates, and ZSM-5 zeolite. 

Substrate Characterization. Test coupons and panels of 7075-T6 aluminum, an alloy used extensively for aircraft structures, were degreased In a commercial alkaline cleaning solution and rinsed In distilled, deionized water. The samples were then subjected to either a standard Forest Products Laboratories (FPL) treatment ( 0 or to a sulfuric acid anodization (SAA) process (10% H2SO4, v/v 15V 20 min), two methods used for surface preparation of aircraft structural components. The metal surfaces were examined by scanning transmission electron microscopy (STEM) In the SEM mode and by X-ray photoelectron spectroscopy (XPS). 

To find the distribution of iron within the nanotube walls an energy dispersive x-ray spectroscopy (EDS) line scan was performed via scanning transmission electron microscopy (STEM), see Fig. 5. 55. The intensity of both the TiK and FeKa lines are maximum at the center of the wall due to its torus shape. Despite the presence of isolated hematite crystallites, a more or less uniform distribution of iron relative to the titanium can be seen across the wall. STEM line scans were performed across a number of walls, and while the average relative intensity of the TiK and FeKa lines varied from wall to wall the relative distribution across a single wall remained uniform. It appears that some of the iron goes into the titanium lattice substituting titanium ions, and the rest either forms hematite crystallites or remains in the amorphous state. 

PA6 phase of the blends. This approach was further extended to PA6 based ternary and quaternary blends in an attempt to find the applicability of this strategy. Raman spectroscopy and transmission electron microscopy (TEM) have been performed to get more insights into the role of these modifiers in debundling the MWNTs. AC electrical conductivity measurements have been carried out to assess the state of dispersion of MWNTs in the blends. Further, the phase microstructures and the localization of MWNTs in the blends have been investigated using scanning electron microscopy (SEM). 

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. 

In addition to its power of directly imaging atomic structures of crystals, H RTEM is often equipped with several other powerful devices for characterization of solids, such as electron diffraction (ED), EDX, electron energy loss spectroscopy (EELS), scanning transmission electron microscopy (STEM) and so on. In this chapter, only the most commonly used supporting techniques for HRTEM, ED and EDX, are discussed in detail. 

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