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Universidad Nacional Autónoma de México - CNyN

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1st International Symposium on Nanoscience and Nanomaterials<br />

Keywords: inhomogeneous thin film, optical spectroscopy.<br />

Optical spectroscopy applied to thin film growth, is a noninvasive technique, which allows us, to<br />

monitor emission lines and control the refractive in<strong>de</strong>x of the film. In this work we established the connection<br />

between plasma spectra and resulting inhomogeneous thin film ma<strong>de</strong> by reactive sputtering. Our goal is to get<br />

prescribed in<strong>de</strong>x profile of oxynitri<strong>de</strong> inhomogeneous thin films, monitoring the emission spectra of the<br />

plasma. We growth films with variation in refractive in<strong>de</strong>x, by controlling the flux rate between two gases,<br />

oxygen and nitrogen in or<strong>de</strong>r to change the film stoichiometry. The plasma was monitored with a<br />

spectrometer in the entire visible spectrum. By analyzing the spectral lines of Ar, N and O we observed their<br />

temporal evolution during the growth of the layers. In-situ spectroscopic ellipsometry is used to characterize<br />

the resulting coating, to obtain refractive in<strong>de</strong>x and thickness. We are able to grow films with 1.46 to 2.1<br />

refractive in<strong>de</strong>x, <strong>de</strong>pending the concentration of Si 3 N 4 or SiO 2 . The mixture is simulated with effective<br />

medium approximation (EMA) mo<strong>de</strong>l. We present results of inhomogeneous thin films with their<br />

corresponding line spectra evolution, to emphasize the possibility of monitoring stoichiometry during the<br />

<strong>de</strong>position process. Partial support from the Conacyt-Mexico project 60351 and DGAPA-UNAM projects<br />

IN100910 is acknowledged, Miss Abundiz thanks Conacyt for her scholarship.<br />

O-018<br />

MICROSTRUCTURAL STUDIES THROUGH HIGH RESOLUTION TRANSMISSION ELECTRON<br />

MICROSCOPY AND X - RAY DIFFRACTOMETRY OF HDS CATALYTIC NANOMATERIALS<br />

E. M. Rivera-Muñoz 1,a , R. Huirache-Acuña 2,b , R. Nava 3,c , C.V. Loricera 4,d , B. Pawelec 4,e<br />

1 Centro <strong>de</strong> Física Aplicada y Tecnología Avanzada, <strong>Universidad</strong> <strong>Nacional</strong> Autónoma <strong>de</strong> México, A.P. 1-<br />

1010 Querétaro, Qro. C.P. 76000, Mexico<br />

2 Facultad <strong>de</strong> Ingeniería Química, <strong>Universidad</strong> Michoacana <strong>de</strong> San Nicolás <strong>de</strong> Hidalgo, Ciudad Universitaria,<br />

Morelia, 58060, México.<br />

3 Facultad <strong>de</strong> Ingeniería, <strong>Universidad</strong> Autónoma <strong>de</strong> Querétaro, Centro Universitario, Cerro <strong>de</strong> las campanas,<br />

76000, Querétaro, Mexico<br />

4 Instituto <strong>de</strong> Catálisis y Petroleoquímica, CSIC, c/ Marie Curie, 2, Cantoblanco, 28049 Madrid, Spain<br />

a emrivera@fata.unam.mx, b rafael_huirache@yahoo.it, c rufino@uaq.mx, d cristinavalero@icp.csic.es,<br />

e bgarcia@icp.csic.es<br />

Keywords: HRTEM, HDS catalysts, SBA-15, SBA-16.<br />

Mesoporous SBA-15 and SBA-16 materials were used as supports of novel ternary Co(Ni)-Mo-W<br />

hydro<strong>de</strong>sulphurization (HDS) catalysts. These materials have shown a high catalytic activity in HDS of<br />

dibenzothiophene (DBT) reactions, even much higher compared with commercial catalysts. An exploration<br />

was ma<strong>de</strong> on structure of both the supports as well as on tri-metallic sulfi<strong>de</strong> HDS catalysts prepared by<br />

simultaneous impregnation via incipient wetness method. Prior to the catalytic test, the catalytic materials<br />

were sulfi<strong>de</strong>d ex situ at atmospheric pressure in a tubular furnace heated up 673 K un<strong>de</strong>r a flow of H 2 S in<br />

hydrogen (15%) and kept un<strong>de</strong>r those conditions for 4 h. The sulfi<strong>de</strong>d catalysts were tested in the HDS of<br />

DBT performed in a batch reactor at 623 K and total pressure of 3.1 MPa. The calcined and fresh sulfi<strong>de</strong><br />

catalysts were characterized by a variety of techniques, such as N 2 adsorption-<strong>de</strong>sorption isotherms, TPD of<br />

NH 3 , XRD and HRTEM. It has been found that both the morphology of the supports as its modification with<br />

20

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