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Palladium–zinc catalysts on mesoporous titania prepared by colloid synthesis. II. Synthesis and characterization of PdZn/TiO2 coating on inner surface of fused silica capillary

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Abstract

Nanoparticle-doped mesoporous titania coating was synthesized by incorporation of PdZn nanoparticles into TiO2 sol followed by dip coating of the sol on inner surface of fused silica capillary. Monodispersed PdZn bimetallic colloidal particles with average particle diameters of approximately 2 nm have been prepared by an ethylene glycol reduction of ZnCl2 and Pd(CH3COO)2 in the presence of polyvinylpyrrolidone. The textural properties, surface structure, chemical composition, and morphology of the samples were investigated by means of N2 sorption measurements, TEM, and X-ray diffraction. PdZn/TiO2 coating has been further analyzed by quantitative analysis of the SAXS data in combination with the density contrast method, providing direct structural-dispersion information about the active component and support. Calcination conditions suitable for surfactant removal have been optimized to obtain PdZn/TiO2 coatings with required metal particle size and composition. The high dispersion and chemical composition of the nanoparticles embedded in mesoporous titania coating have been retained with no modification after thermal treatment in vacuum at 300 °C. Results suggest how porous structure of the PdZn coating may be fine-tuned to improve the accessibility of the pores to reactants. The control of the pore size in the range of 4.9–6.8 nm of the mesoporous titania was achieved by adding co-surfactants, such as n-butanol.

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Abbreviations

PVP:

Polyvinylpyrrolidone

TEM:

Transmission electron microscopy

SAXS:

Small angle X-ray scattering

XRD:

X-ray diffraction

EDS:

Energy dispersive spectroscopy

ICP-AES:

Inductively coupled plasma atomic emission spectroscopy

XRF:

X-ray fluorescence spectroscopy

HRTEM:

High resolution TEM

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Acknowledgments

The authors wish to thank E. Yu. Gerasimov for the investigation of the catalysts by TEM, Dr. V. A. Ushakov for XRD analysis of the samples. We also thank Mrs. I.L. Kraevskaya for X-ray Fluorescence analysis of the samples. The support of this work by Presidium of SB RAS (Interdisciplinary Integration Project N76) and Russian Foundation for Basic Research (Project N12-03-00722) is gratefully acknowledged.

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Authors and Affiliations

  1. Boreskov Institute of Catalysis, Lavrentyeva pr. 5, Novosibirsk, 630090, Russia

    Lyudmila B. Okhlopkova, Michail A. Kerzhentsev, Fedor V. Tuzikov, Yurii V. Larichev & Zinfer R. Ismagilov

  2. Novosibirsk State University, Pirogova St. 2, Novosibirsk, 630090, Russia

    Fedor V. Tuzikov

  3. Institute of Coal Chemistry and Material Science, Sovetsky Ave. 18, Kemerovo, 650000, Russia

    Zinfer R. Ismagilov

Authors
  1. Lyudmila B. Okhlopkova
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  2. Michail A. Kerzhentsev
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  3. Fedor V. Tuzikov
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  4. Yurii V. Larichev
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  5. Zinfer R. Ismagilov
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Correspondence to Lyudmila B. Okhlopkova.

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Okhlopkova, L.B., Kerzhentsev, M.A., Tuzikov, F.V. et al. Palladium–zinc catalysts on mesoporous titania prepared by colloid synthesis. II. Synthesis and characterization of PdZn/TiO2 coating on inner surface of fused silica capillary. J Nanopart Res 14, 1088 (2012). https://doi.org/10.1007/s11051-012-1088-x

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