High-resolution transmission electron microscopic measurement

The transmission electron microscopy (TEM) images of a two-layer Tl-1223 film are shown in Fig. 7.12, which confirms the epitaxial nature of the annealed electrodeposited films. All films showed a significant amount of intergrowth, as shown by a high-resolution transmission electron microscopic (HRTEM) measurement in Figs. 7.12c and d of a representative two-layer... 

High Resolution Transmission Electron microscopy (HR-TEM) images were recorded on a Philips CM-30 microscope operated at 250 kV. The films were scratched from the substrate. The collected powders and flakes were grinded and dispersed in ethanol. Then the suspensions were dropped gently to a holey amorphous carbon film on a Ni or Cu grid. The Particle size distribution (PSD) was obtained by measuring 100 particles from the TEM micrographs. The mean... 

The gold content in catalysts was analyzed by Atomic absorption method and made by the Analytical Center of the CNRS, Lyon, France. The XRD patterns were obtained with a Philips PW 170 diffiactometer, using Cu Ka (1.54178 A) radiation. High resolution transmission electron microscopy (HRTEM) analysis was performed on a Jeol JEM-3010 microscope at 300 kV. Nitrogen adsorption-desorption isotherms and specific surface areas were measured at -196 °C over a wide relative pressure range from 0.01 to 0.995 with a volumetric adsorption analyzer TRISTAR 3000 manufactured by Micromeritics. The pore diameter and the pore size distribution were determined by the Barret-Joyner-Halenda (BJH) method using the adsorption branch of isotherms [15]. 

The details of the structural characteristics of individual constituents in the various carbon deposits were obtained by examination of a number of specimens from each experiment in a JEOL 100 CX transmission electron microscope that was fitted with a high resolution pole piece, capable of 0.18 nm lattice resolution. Suitable transmission specimens were prepared by applying a drop of an ultrasonic dispersion of the deposit in iso-butanol to a carbon support film. In many cases the solid carbon product was found to consist entirely of filamentous structures. Variations in the width of the filaments as a function of both catalyst composition and growth conditions were determined from the measurements of over 300 such structures in each specimen. In certain samples evidence was found for the existence of another type of ca naceous solid, a shell-like deposit in which metal particles appeared to be encapsulated by graphitic platelet structures. Selected area electron diffraction studies were performed to ascertain the overall crystalline order of the carbon filaments and the shell-like materials produced from the various catalyst systems. 

Atomic Force Microscopy measurements were carried out on a Topometrix 2010 TMX Microscope under ambient conditions. High Resolution Scanning Electron Microscopy was done with a Jeol JSM-6000F scanning microscope. Transmission Electron Microscopy was performed on a Philips CM-30 FEG microscope to prove the presence of metal oxide after crystallization of the silicalite-1 layer. 

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