Scanning transmission electron microscope analyses

Analysis of individual catalyst particles less than IMm in size requires an analytical tool that focuses electrons to a small probe on the specimen. Analytical electron microscopy is usually performed with either a dedicated scanning transmission electron microscope (STEM) or a conventional transmission electron microscope (TEM) with a STEM attachment. These instruments produce 1 to 50nm diameter electron probes that can be scanned across a thin specimen to form an image or stopped on an image feature to perform an analysis. In most cases, an electron beam current of about 1 nanoampere is required to produce an analytical signal in a reasonable time. 

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. 

Figure 5 shows the Z-contrast scanning transmission electron microscope (STEM) image of a Ru/Sn02 nanocomposite catalyst prepared by the assembly process [18]. A combined EDX analysis, using an electron beam of... 

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. 

Powder X-ray diffraction (XRD) data were collected via a Siemens D5005 diffractometer with CuKa radiation (A. = 1.5418 A). Routine transmission electron microscopy (TEM) and Z-contrast microscopy were carried out using an HITACH HD-2000 scanning transmission electron microscope (STEM) operated at 200 kV. Nitrogen gas adsorption measurements (Micromeritics Gemini) were used to determine the surface area and porosity of the catalyst supports. Inductively coupled plasma (ICP) analysis was performed via an IRIS Intrepid II XSP spectrometer (Thermo Electron Corporation). 

Arsenic Oxidation States. A solution sample was taken 257 hr after initiation of the 300°C basalt + arsenic-doped deionized water experiment (Run D2-8, Table II). The data from arsenic oxidation state AAS analysis of the initial As(V)-doped water (0-hr sample) and of the 257-hr solution sample are given in Table HI. All detectable arsenic was in the +3 oxidation state [As(V) <15pg/L] in the 257-hr sample. Standard additions of AsGD) and As(V) to the 257-hr sample were quantitatively recovered. To desorb arsenic from particulates in this sample, an aliquot of the solution was treated with 5% hydrofluoric acid. The higher As(III) content of the treated 257-hr sample aliquot (110 vs. 61pg/L, Table HI) demonstrates that sorption occurred. Scanning transmission electron microscopic (STEM) analysis of the particulates indicated the presence of poorly crystallized high-iron illite . 

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. 

Browning, N.D. Chisholm, M.F. Pennycook, S.J. Atomic-resolution chemical analysis using a scanning transmission electron microscope. Nature 1993, 366, 143-146. 

It is now possible to obtain scanning transmission electron microscopes (STEMs). With a STEM, the electrons pass through the specimen but, as in SEM, the electron optics focus the beam into a narrow spot that is scanned over the sample in a raster. This makes these microscopes suitable for analysis techniques such as mapping by energy dispersive X-ray (EDX) spectroscopy among others. Also, the resolution on the latest STEM instruments is less than one Angstrom. 

Mosesson, M. W.. Church, W. R., DiOrio, J. P., Krishnaswamy, S., Mann, K. G., Hainfeld, J. F and Wall, J. S. (1990a). Structural model of factors V and Va based on scanning transmission electron microscope (STEM) images and STEM mass analysis. J. Biol. Chem. 265, 8863-8868. 

Recent progress in scanning transmission electron microscope imaging and analysis application to nanoparticles and 2D nanomaterials... 

STEM Scanning transmission electron microscope TEM Transmission electron microscope TGA Thermogravimetric analysis... 

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