Transmission electron microscopy sample preparation

Samples for transmission electron microscopy were prepared in the following manner. Films were grown with different current rates up to various thicknesses on platinum working electrodes. The film thickness was controlled by the period of current flow. The films were transferred onto carbon coated electron microscope grids by stripping with formvar and subsequently removing the formvar with methylene chloride. As-synthesized films were directly used for scanning electron microscopy. 

Samples for transmission electron microscopy were prepared in the following manner. A 50/50 blend was potted in an acrylic resin (London Resin Co. Ltd.) and subsequently microtomed in thin films of approximately 600 angstrom thickness and transferred onto electron microscope grids. These sections were then doped with iodine vapor (stained) and were ready for transmission electron microscopy. The blends of other compositions were not examined in this manner for reasons discussed later. 

Our research on these subjects began more than 25 years ago with Yeh s examination of the morphology and properties of amorphous poly(ethylene terephthalate) (PET) and the effect thereon of crystallization and deformation. Both thick and thin (i.e., > 10 i and ca. 1,000 A, suitable for transmission electron microscopy) samples were used, the samples being either quenched from the melt or cast from solution into the amorphous state. The films, as prepared, were amorphous by x-ray or electron diffraction. 

Also a good interface resolution is obtained with transmission electron microscopy (TEM), where, however, a dedicated sample preparation and treatment are necessary to achieve nanometer resolution and suitable contrast [64]. Thus the... 

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. ... 

In order to obtain Pt nanoparticles, aqueous solution of 10 M K2PtCl4, which contained 10 M (as monomer unit) of poly-NIPA or poly-NEA, was bubbled with Ar gas and then H2 gas. Then the reaction vessel was sealed tightly and kept in a water bath at a suitable temperature. At given reaction times, the vessels were opened and the samples for transmission electron microscopy (TEM) were prepared by soaking a grid (carbon substrate, Oken) in the colloidal solution and then drying it in the air. The TEM (Hitachi H-8100) was operated at 200 kV. 

Sample Preparation for Transmission Electron Microscopy Analysis... 

Tomography was applied during Transmission Electron Microscopy (TEM) analysis of various reduced Au/zeolite samples. The size and location of the gold nanoparticles as a function of the support characteristics and preparation method are discussed. 

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. 

If the sample is thin enough, for example a specially prepared thin section, electrons may go straight through and be detected, as well as elastically and inelastically scattered electrons which are scattered in a forward direction. These form the basis of transmission electron microscopy (TEM). 

Samples prepared with stirring and poured into test tubes at different times (stopping the stirring) showed the sequence illustrated schematically in Fig. 2. The two layers were distinguishable because of dullness and hardness differences. At a reaction temperature of 80°C, the volume of the upper layer (elastomer continuous) decreases slowly and finally disappears at about 90 min. Samples of both top and bottom layers were studied by transmission electron microscopy techniques, and micrographs for a 10/90 COPE/PSN are shown in Fig. 3. Up to 90 min, samples exhibit elastomer continuous top and plastic continuous bottoms. 

Transmission electron microscopy micrographs (Fig. 13.24) also indicate an important characteristic of the supported particles. As in the case of suspensions, they are either aggregated or isolated. Support surface properties may he an important factor governing this aggregation. After deposition on the support, we observed that samples prepared from acidic hydrosols are characterized by the presence of aggregated particles constituting flocculates ranging from 10 to 200 nm, whereas samples prepared via basic hydrosols contain only isolated particles. The opposite was observed when hydrosols were concerned. These final states of the supported particles may be controlled... 

Nanocrystalline iron-doped Ti02 samples (as-prepared S2 and annealed at 500°C S4 [7]) and undoped samples (Si and S3 [8]) were S5mthesised by a modified sol-gel method. The details of preparation were reported earlier [7, 8]. The X-ray diffiaction of the samples was carried out at room temperature using a Philips powder diffractometer (PW 1820) with monochromatized CuXa radiation. Transmission electron microscopy (TEM) and SAED investigations were carried out by using a JEOL JEM 2010 200 kV microscope, Cs=0.5 mm, point resolution 0.19 nm. 

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). 

The use of [RUO4] as a reagent for the preparation of epidermal samples for transmission electron microscopy has been investigated." ... 

In transmission electron microscopy (TEM), a beam of highly focused and highly energetic electrons is directed toward a thin sample (< 200 nm) which might be prepared from solution as thin film (often cast on water) or by cryocutting of a solid sample. The incident electrons interact with the atoms in the sample, producing characteristic radiation. Information is obtained from both deflected and nondeflected transmitted electrons, backscattered and secondary electrons, and emitted photons. 

The basal spacing (d 001) (DRX-Kristalloflex-805 Siemens) and the surface area (Micromeritics ASAP 2400) was obtained on the solids calcined at different temperatures. X-Ray diffraction patterns have also been obtained after ethylenglycol saturation of selected samples. High resolution transmission electron microscopy (HREM) was performed (Jeol 100 CX Temscan) on ultrathin preparations (LKB Ultratome type 8802A). TPD (NH3) and infrared spectroscopy (pyridine) allowed to evaluate the acid properties of the solid calcined at 4(X) and 600°C. 

Recently, we reported that an Fe supported zeolite (FeHY-1) shows high activity for acidic reactions such as toluene disproportionation and resid hydrocracking in the presence of H2S [1,2]. Investigations using electron spin resonance (ESR), Fourier transform infrared spectroscopy (FT-IR), MiJssbauer and transmission electron microscopy (TEM) revealed that superfine ferric oxide cluster interacts with the zeolite framework in the super-cage of Y-type zeolites [3,4]. Furthermore, we reported change in physicochemical properties and catalytic activities for toluene disproportionation during the sample preparation period[5]. It was revealed that the activation of the catalyst was closely related with interaction between the iron cluster and the zeolite framework. In this work, we will report the effect of preparation conditions on the physicochemical properties and activity for toluene disproportionation in the presence of 82. ... 

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. 

The consolidated titanate waste pellets are similar in appearance to their glass counterparts, i.e., both are dense, black and apparently homogeneous. Microscopic analyses, however, reveal important differences between these two waste forms. While little definitive work has been done with glassy waste forms, it is apparent that several readily soluble oxide particulates of various nuclides are simply encapsulated in the glass matrix. The titanate waste form has undergone extensive analyses which includes optical microscopy, x-ray, scanning electron microscopy, microprobe, and transmission electron microscopy (l ) The samples of titanate examined were prepared by pressure sintering and consisted of material from a fully loaded titanate column. Zeolite and silicon additions were also present in the samples. 

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