In this work, two groups of carbon supported Pt-Pd catalysts have been prepared in order to investigate the effect of Pd, as a second metal, and surfactants on the catalytic activity towards methanol and ethanol oxidation reactions used in the direct methanol and ethanol fuel cells. In the first group (group a), 1- hexanethiol was used as a stabilizing agent while in the second group (group b), 1,1 dimethyl hexanethiol was utilized. Cyclic voltammetry (CV), chronoamperometry (CA), X-ray diffraction (XRD), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS) were used in order to determine the nature of the catalysts. The average crystalline size of the metal particles in the catalysts was explored by XRD and TEM. TEM results revealed the uniform distribution of the metal nanoparticles on carbon support with a narrow size distribution in the range of 3.0 to 3.7 nm and the average crystalline sizes of metal particles for group &ldquo / b&rdquo / catalysts were larger than that of group &ldquo / a&rdquo / catalysts which can be explained by the surfactant effect. These results were in good agreement with XRD data. The oxidation states of platinum (Pt(0) and Pt(IV)) and palladium (Pd(0) and Pd(II)) and their ratios were investigated by XPS and for the most active catalyst, catalyst Ib, these ratios were found to be as 6.94 and 13.7, respectively. Electrochemical activities of the catalysts towards methanol and ethanol oxidation reactions were recorded and compared with that of Pt/C and the commercial Pt (ETEK 20 %wt) catalysts. The results indicated that the group &lsquo / b&rsquo / catalyst has greater catalytic activities than that of group &lsquo / a&rsquo / catalysts. Catalyst Ib comes into prominence as the most active catalyst due to its superior characteristics that it possess such as highest extent of alloying with respect to the palladium amount used, active surface area, CO-tolerance, stability and Pt (0) to Pt (IV) and Pd (0) to Pd (II) ratios.

Structural characterization is essential for the understanding of the magnetic properties of thin films and multilayers. In this thesis, both crystalline and amorphous thin films and multilayers were analyzed utilizing transmission electron microscopy (TEM). High resolution TEM and electron diffraction studies emphasize on the growth of amorphous Fe91Zr9 and Co68Fe24Zr8 on both Al2O3 and Al70Zr30 in multilayer structures by magnetron sputtering. The properties of the growth surfaces were found to strongly influence the formation of nano-crystallites of the magnetic material at interfaces. Field induced uniaxial magnetic anisotropy was found to be possible to imprint into both fully amorphous and partially crystallized Co68Fe24Zr8 layers, yielding similar magnetic characteristics regardless of the structure. These findings are important for the understanding of both growth and magnetic properties of these amorphous thin films. As magnetic systems become smaller, new analysis techniques need to be developed. One such important step was the realization of electron energy-loss magnetic circular dichroism (EMCD) in the TEM, where information about the ratio of the orbital to spin magnetic moment (mL/mS) of a sample can be obtained. EMCD makes use of angular dependent inelastic scattering, which is characterized using electron energy-loss spectroscopy. The work of this thesis contributes to the development of EMCD by performing quantitative measurements of the mL/mS ratio. Especially, methods for obtaining energy filtered diffraction patterns in the TEM together with analysis tools of the data were developed. It was found that plural inelastic scattering events modify the determination of the mL/mS ratio, wherefore a procedure to compensate for it was derived. Additionally, utilizing special settings of the electron gun it was shown that EMCD measurements becomes feasible on the nanometer level through real space maps of the EMCD signal.

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Surface Plasmons (SP) are elementary excitations mixing electrons and photons at metal surfaces,which can be seen in a classical electrodynamics framework as electromagnetic surface eigenmodesof a metal-dielectric system. The present work bases on the ability of mapping SP eigenmodes withnanometric spatial resolution over a broad spectral range using spatially resolved fast electron basedspectroscopies in a Scanning Transmission Electron Microscope (STEM). Such an ability has beenseparately demonstrated during the last few years by many spatially resolved experiments of ElectronEnergy Loss Spectroscopy (EELS), which measures the energy lost by fast electrons interactingwith the sample, and CathodoLuminescence (CL), which measures the energy released by subsequentlyemitted photons. In the case of EELS, the experimental results are today well accountedfor by strong theory elements which tend to show that the quantity measured in an experiment canbe safely interpreted in terms of the surface eigenmodes of the sample. In order to broaden thisinterpretation to fast electron based spectroscopies in general, I have performed combined spatiallyresolved EELS and CL experiments on a simple single nanoparticle (a gold nanoprism). I have shownthat EELS and CL results bear strong similarities but also slight differences, which is confirmed bynumerical simulations. I have extended the theoretical analysis of EELS to CL to show that CLmaps equally well than EELS the radiative surface eigenmodes, yet with slightly different spectralfeatures. This work is a proof of principle clarifiying the quantities measured in EELS and CL,which are shown to be respectively some nanometric equivalent of extinction and scattering spectroscopieswhen applied to metal-dielectric systems. Based on this interpretation, I have applied EELSto reveal the SP eigenmodes of random metallic media (in our case, semicontinuous metal films beforethe percolation threshold). These SP eigenmodes constitute a long standing issue in nanooptics.I have directly identified the eigenmodes from measurements and data processing. I havefully characterized these eigenmodes experimentally through an electric field intensity pattern, aneigenenergy and a relaxation rate. Doing so, I have shown that the fractal geometry of the medium,which grows towards the percolation, induces random-like eigenmodes in the system at low energies.Keywords: Surface plasmons, fast electron based spectroscopies, scanning transmission electronmicroscopy, disordered media

<p>The spectroscopic, SEM and Raman measurements on carbon nanotubes under the exact conditions of which OES analysis were made showed that at<br /> a pressure of 400 Torr and a flow rate of 200 sccm, the quality and quantity of single-walled carbon nanotubes was the highest.</p>

One of the oldest goals across the science is to watch atoms undergo reactions in real time. However, such observations are only meaningful if the object of interest is looked at in its natural environment. For most biological and materials sciences samples, this means in solution phase or dispersed in a liquid. Unfortunately, this restriction normally prohibits either reaching atomic spatial (10-10m) or ultrafast time (10-15sec) resolution. Here, two sample preparation techniques are shown providing a natural environment for experiments with high spatial and temporal resolution: a nanofluidic cell for electron microscopy, and a chip for serial time resolved x-ray crystallography. The nanofluidic cell was implemented into different transmission electron microscopes, and in initial experiments, the key features of the sample cell are shown, namely the ability to create stable ultrathin liquid layers of tuneable thickness within the harsh electron microscope vacuum. The option to directionally flow liquid through the sample cell opens the door to high throughput electron microscopy and on-the-fly sample exchanges with the option of triggering and influencing chemical reactions with external sample control. First applications highlight the impact of the nanocell: structural disintegration of gold nanorods exemplary for materials science, and amyloid fibrils, exemplary for biomedical applications. In future applications diffractive imaging with high time resolution is planned, and will complement the range of experiments within the fields of traditional transmission electron microscopy. The second half of this thesis presents a solid target for x-ray crystallography. The chip enables the arrangement of thousands of micrometer sized protein crystals in a regular array. The ability to prepare protein crystals in such a fashion is unique and permits serial in situ crystallography. Real time crystallography requires samples to be mounted in a saturated natural environment, i.e. under ambient pressure and temperature conditions. The crystallography chip fills this need while being easily integrated into a synchrotron beam line. In a first set of experiments, the chip design was refined and could prove functionality for static in situ structure analysis of protein systems. Based on this success, future time resolved experiments are under way and will show the full capability of this device.

In recent years, with the advance of computing equipment and image acquisition techniques, the sizes, dimensions and content of acquired images have increased considerably. Unfortunately as time passes there is a steadily increasing gap between the classical and parallel programming paradigms and their actual performance on modern computer hardware. In this thesis we consider in depth one particular algorithm, the continuous maximum flow computation. We review in detail why this algorithm is useful and interesting, and we propose efficient and portable implementations on various architectures. We also examine how it performs in the terms of segmentation quality on some recent problems of materials science and nano-scale biology