Synthesis and characterization of Pd-MCM-TYPE mesoporous nanocomposite materials

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Tezin Türü: Yüksek Lisans

Tezin Yürütüldüğü Kurum: Orta Doğu Teknik Üniversitesi, Fen Bilimleri Enstitüsü, Fen Bilimleri Enstitüsü, Türkiye

Tezin Onay Tarihi: 2006

Öğrenci: CANAN ŞENER

Danışman: TİMUR DOĞU

Özet:

Noble metal incorporated MCM-41 based nanostructured mesoporous materials have attracted the attention of material researchers in recent years. Sorption characteristics of MCM materials can be improved by surface modification techniques. Besides surface modification, metal nanoparticles can also be produced within the pores of mesoporous materials. MCM-41 can act as host for several metal nanoparticles such as palladium. The present study is focused on the synthesis of Pd-MCM-41 nanocomposite catalytic materials by using different direct synthesis procedures, as well as an impregnation method. Impregnated samples were used to synthesize Pd nanoparticles inside the pores of MCM-41. In the direct hydrothermal synthesis of Pd-MCM-41, incorporation of the Pd metal was achieved by adding PdCl2, K2PdCl4 and Pd(NH3)4(NO2)3 solutions into the synthesis mixture. Syntheses were performed in acidic and basic routes. Hydrothermal synthesis was carried out in an autoclave at 120 oC. The solid product was filtered, washed, dried, calcined at 550 oC in a stream of dry air and reduced in a stream of hydrogen at 200 oC. In the case of impregnation, PdCl2 solution was added to a suspension of MCM-41. The product was evaporated to dryness, dried under vacuum and reduced with H2 gas at 200 oC. Physical and chemical properties and surface morphology of Pd-MCM-41 nanomaterials were characterized by using XRD, XPS, EDS, BET, SEM, TEM and TPR techniques. Very high Pd/Si ratios, as high as 0.45 and 0.18 were obtained in the mesoporous materials produced by the basic and acidic direct synthesis routes, respectively. The BET surface areas of these materials were found as 999 m2/g and 694 m2/g, respectively. These results showed that the basic direct synthesis procedure was highly successful for the incorporation of Pd into the mesoporous Si structure. In addition, EDS analysis of the Pd-MCM-41