Transmission Electron Microscopy TEM Characterization

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... 

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... 

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). 

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)... 

Transition metal oxides, rare earth oxides and various metal complexes deposited on their surface are typical phases of DeNO catalysts that lead to redox properties. For each of these phases, complementary tools exist for a proper characterization of the metal coordination number, oxidation state or nuclearity. Among all the techniques such as EPR [80], UV-vis [81] and IR, Raman, transmission electron microscopy (TEM), X-ray absorption spectroscopy (XAS) and NMR, recently reviewed [82] for their application in the study of supported molecular metal complexes, Raman and IR spectroscopies are the only ones we will focus on. The major advantages offered by these spectroscopic techniques are that (1) they can detect XRD inactive amorphous surface metal oxide phases as well as crystalline nanophases and (2) they are able to collect information under various environmental conditions [83], We will describe their contributions to the study of both the support (oxide) and the deposited phase (metal complex). 

Ffirai and Toshima have published several reports on the synthesis of transition-metal nanoparticles by alcoholic reduction of metal salts in the presence of a polymer such as polyvinylalcohol (PVA) or polyvinylpyrrolidone (PVP). This simple and reproducible process can be applied for the preparation of monometallic [32, 33] or bimetallic [34—39] nanoparticles. In this series of articles, the nanoparticles are characterized by different techniques such as transmission electronic microscopy (TEM), UV-visible spectroscopy, electron diffraction (EDX), powder X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) or extended X-ray absorption fine structure (EXAFS, bimetallic systems). The great majority of the particles have a uniform size between 1 and 3 nm. These nanomaterials are efficient catalysts for olefin or diene hydrogenation under mild conditions (30°C, Ph2 = 1 bar)- In the case of bimetallic catalysts, the catalytic activity was seen to depend on their metal composition, and this may also have an influence on the selectivity of the partial hydrogenation of dienes. 

Transmission electron microscopy (TEM) is a powerful and mature microstructural characterization technique. The principles and applications of TEM have been described in many books [16 20]. The image formation in TEM is similar to that in optical microscopy, but the resolution of TEM is far superior to that of an optical microscope due to the enormous differences in the wavelengths of the sources used in these two microscopes. Today, most TEMs can be routinely operated at a resolution better than 0.2 nm, which provides the desired microstructural information about ultrathin layers and their interfaces in OLEDs. Electron beams can be focused to nanometer size, so nanochemical analysis of materials can be performed [21]. These unique abilities to provide structural and chemical information down to atomic-nanometer dimensions make it an indispensable technique in OLED development. However, TEM specimens need to be very thin to make them transparent to electrons. This is one of the most formidable obstacles in using TEM in this field. Current versions of OLEDs are composed of hard glass substrates, soft organic materials, and metal layers. Conventional TEM sample preparation techniques are no longer suitable for these samples [22-24], Recently, these difficulties have been overcome by using the advanced dual beam (DB) microscopy technique, which will be discussed later. 

Covering monometallic (Pd, Sn) and multimetallic (Pd-Sn, Pd-Ag) systems, several examples are presented in this chapter to illustrate the possibility offered by this chemistry to control the particle size distribution and the bimetallic interaction at a molecular level. This work is supported by a multitechnique characterization approachusing SnM6ssbauerspectroscopy,X-rayphotoelectron spectroscopy (XPS), low-energy ion spectroscopy (LEIS), and transmission electron microscopy (TEM). Catalytic performances in hydrogenation of different unsaturated hydrocarbons (phenylacetylene, butadiene) are finally discussed in order to establish structure-reactivity relationships. 

A fascinating study on the surface science of copper hydride on Si02, as well as on AI2O3, ceria (cerium oxide), and ZnO, has appeared [50]. Pure, yet thermally unstable, CuH can be precipitated as a red-brown solid from aqueous cupric sulfate and hypophosphorous acid in the presence of H2SO4, and has been characterized by powder X-ray diffraction (PXRD) (Eq. 5.25). Transmission electron microscopy (TEM) data suggest that it is most stable when deposited on acidic Si02. 

Transmission electron microscopy (TEM) can provide detailed stmcture of zeolites. I use the word characterize or characterization for stmctural study on a unit cell scale, such as various kind of stmctural defects and basic stmctural units, and determine or determination for obtaining atomic coordinates within the unit cell for all the atoms of a crystal. A simple text or reviews for stmctural characterization of porous materials can be found in a book or review articles [1-6]. Now, we are in a new era, that is, we can determine new stmctures of micro- and mesoporous materials only by electron microscopy(EM), an area called electron crystallography (EC) [7-11]. 

To characterize dendrimers, analytical methods used in synthetic organic chemistry as well as in macromolecular chemistry can be applied. Mass spectrometry and NMR spectroscopy are especially useful tools to estimate purity and structural perfection. To get an idea of the size of dendrimers, direct visualization methods such as atomic force microscopy (AFM) and transmission electron microscopy (TEM), or indirect methods such as size exclusion chromatography (SEC) or viscosimetry, are valuable. Computer aided simulation also became a very useful tool not only for the simulation of the geometry of a distinct molecule, but also for the estimation of the dynamics in a dendritic system, especially concerning mobility, shape-persistence, and end-group disposition. 

Transmission electron microscopy (TEM) can provide valuable information on particle size, shape, and structure, as well as on the presence of different types of colloidal structures within the dispersion. As a complication, however, all electron microscopic techniques applicable for solid lipid nanoparticles require more or less sophisticated specimen preparation procedures that may lead to artifacts. Considerable experience is often necessary to distinguish these artifacts from real structures and to decide whether the structures observed are representative of the sample. Moreover, most TEM techniques can give only a two-dimensional projection of the three-dimensional objects under investigation. Because it may be difficult to conclude the shape of the original object from electron micrographs, additional information derived from complementary characterization methods is often very helpful for the interpretation of electron microscopic data. 

In 2008 Shin et al. used lETS and transmission electron microscopy (TEM) to characterize the chemical integrity and morphology of rubrene (C40H24) layers after deposition of an Fe top electrode [57]. The lETS spectra were consistent with the known IR- and Raman-active normal modes, which led the authors to conclude there were no chemical reactions with Fe. Cross-sectional TEM images showed continuous rubrene layers between the bottom Co layer and top Fe layer, with no evidence for small particle formation. Similar to the study by Santos et al., they found that the presence of an AI2O3 layer had a profound effect on the tunneling... 

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