Transmission electron microscopy Characterization

Kleebe, H.-J. and Cinibulk, M.K., (1993), Transmission electron microscopy characterization of a ceria-fluxed silicon nitride , J. Mater. Sci. Lett., 12 (2), 70-72. 

Inductively coupled plasma-atomic emission spectrometry allows the determination of anionic surfactants (LAS and AS) and inorganic compounds (phosphate, silicate, zeolite, sulfate). Other techniques, such as X-ray fluorescence spectroscopy and X-ray powder diffraction, have been used for the qualitative analysis of inorganic detergents. For surface analysis, optical light microscopy, scanning electron microscopy, and transmission electron microscopy characterize particles, deposition of surfactant, or other detergent ingredients on fabric. 

Transmission electron microscopy (TEM) can resolve features down to about 1 nm and allows the use of electron diffraction to characterize the structure. Since electrons must pass through the sample however, the technique is limited to thin films. One cryoelectron microscopic study of fatty-acid Langmuir films on vitrified water [13] showed faceted crystals. The application of TEM to Langmuir-Blodgett films is discussed in Chapter XV. 

In many ways the nanocrystal characterization problem is an ideal one for transmission electron microscopy (TEM). Here, an electron beam is used to image a thin sample in transmission mode [119]. The resolution is a sensitive fimction of the beam voltage and electron optics a low-resolution microscope operating at 100 kV might... 

High-resolution transmission electron microscopy (HREM) is the technique best suited for the structural characterization of nanometer-sized graphitic particles. In-situ processing of fullerene-related structures may be performed, and it has been shown that carbonaceous materials transform themselves into quasi-spherical onion-like graphitic particles under the effect of intense electron irradiation[l 1],... 

Carr and his co-workers [86C01, 87C01] have shown that transmission electron microscopy is a powerful tool in characterizing linear and higher-order defect configurations and their densities on shock-modified rutile, alumina, aluminum nitride, and zirconia [84H02]. The principal impediment to detailed characterization of shock-formed defects is their very high concentrations, which prevent identification of specific deformation features except in... 

Four different material probes were used to characterize the shock-treated and shock-synthesized products. Of these, magnetization provided the most sensitive measure of yield, while x-ray diffraction provided the most explicit structural data. Mossbauer spectroscopy provided direct critical atomic level data, whereas transmission electron microscopy provided key information on shock-modified, but unreacted reactant mixtures. The results of determinations of product yield and identification of product are summarized in Fig. 8.2. What is shown in the figure is the location of pressure, mean-bulk temperature locations at which synthesis experiments were carried out. Beside each point are the measures of product yield as determined from the three probes. The yields vary from 1% to 75 % depending on the shock conditions. From a structural point of view a surprising result is that the product composition is apparently not changed with various shock conditions. The same product is apparently obtained under all conditions only the yield is changed. 

The nano-scale structures in polymer layered-silicate nano-composites can be thoroughly characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). XRD is used to identify intercalated structures. XRD allows quantification of changes in layer spacing and the most commonly used to probe the nano-composite structure and... 

In the matrix of PLA/ polycaprilactone (PCL)/OMMT nano-composites, the silicate layers of the organoclay were intercalated and randomly distributed (Zhenyang et at, 2007). The PLA/PCL blend significantly improved the tensile and other mechanical properties by addition of OMMT. Thermal stability of PLA/PCL blends was also explicitly improved when the OMMT content is less than 5%wt. Preparation of PLA/thermoplastic starch/MMT nano-composites have been investigated and the products have been characterized using X-Ray diffraction, transmission electron microscopy and tensile measurements. The results show improvement in the tensile and modulus, and reduction in fracture toughness (Arroyo et ah, 2010). 

The authors have characterized the graft polymer by solvent extraction, transmission electron microscopy, dynamic mechanical analysis, mechanical testing (including measurement of tensile, tear, and impact strength), and morphology by SEM. The reaction scheme is given in Figure 11.25. 

MgO-supported model Mo—Pd catalysts have been prepared from the bimetallic cluster [Mo2Pd2 /z3-CO)2(/r-CO)4(PPh3)2() -C2H )2 (Fig. 70) and monometallic precursors. Each supported sample was treated in H2 at various temperatures to form metallic palladium, and characterized by chemisorption of H2, CO, and O2, transmission electron microscopy, TPD of adsorbed CO, and EXAFS. The data showed that the presence of molybdenum in the bimetallic precursor helped to maintain the palladium in a highly dispersed form. In contrast, the sample prepared from the monometallie precursors was characterized by larger palladium particles and by weaker Mo—Pd interactions. ... 

Many years have passed since the early days of AFM, when adhesion was seen as a hindrance, and it is now regarded as a useful parameter for identification of material as well as a key to understanding many important processes in biological function. In this area, the ability of AFM to map spatial variations of adhesion has not yet been fully exploited but in future could prove to be particularly useful. At present, the chemical nature and interaction area of the AFM probe are still rarely characterized to a desirable level. This may be improved dramatically by the use of nanotubes, carbon or otherwise, with functionalized end groups. However, reliance on other measurement techniques, such as transmission electron microscopy and field ion microscopy, will probably be essential in order to fully evaluate the tip-sample systems under investigation. 

The feasibility of synthesizing oxovanadium phthalocyanine (VOPc) from vanadium oxide, dicyanobenzene, and ethylene ycol using the microwave synthesis was investigated by comparing reaction temperatures under the microwave irradiations with the same factors of conventional synthesis. The efficiency of microwave synthesis over the conventional synthesis was illustrated by the yield of crude VOPc. Polymorph of VOPc was obtained ttough the acid-treatment and recrystallization step. The VOPos synthesized in various conditions were characterized hy the means of an X-ray dif actometry (XRD), a scanning electron microscopy (SEM), and a transmission electron Microscopy (TEM). 

Transmission electron microscopy is one of the techniques most often used for the characterization of catalysts. In general, detection of supported particles is possible, provided that there is sufficient contrast between particles and support - a limitation that may impede applications of TEM on well-dispersed supported oxides. The determination of particle sizes or of distributions therein is now a routine matter, although it rests on the assumption that the size of the imaged particle is truly proportional to the size of the actual particle and that the detection probability is the same for all particles, independent of their dimensions. 

Fig. 4 Osmium clusters supported on MgO(OOl) a OssC/MgisOs and b OS5C at a surface point Vs defect site [33] these were represented by density functional theory, and the samples were characterized by EXAFS spectroscopy, transmission electron microscopy, and other techniques [15]...

Usually bimetallic nanoparticles as well as monometallic ones are characterized by many probing tools such as UV-visible (UV-Vis) spectroscopy, transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), EXAFS, infrared spectroscopy of adsorbed CO (CO-IR), and so on [1,2]. 

Nanoscale Characterization of Metal Nanoclusters by Means of X-Ray Diffraction (XRD) and Transmission Electron Microscopy (TEM)... 

One of the early questions raised on TUD-1 dealt with its pore structure did it have intersecting or nonintersecting pores At the University of Utrecht, one conclusive characterization was carried out with a silica TUD-1 with Pt inserted, which was analyzed by 3-D TEM (transmission electron microscopy) (9). The Pt anchors (not shown) were used as a focal point for maintaining the xyz orientation. As shown in Figure 41.2, the TUD-1 is clearly amorphous. While not quantitatively measured for this sample, the pores appear rather uniform, consistent with all porosimetry measurements on TUD-1 showing narrow pore size distributions. 

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