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Using SAXS for Determining the Sizes of Gold Nanoparticles in Au/C Catalysts: Advantages over Other Methods

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Abstract

The advantages of using SAXS along with the masking liquid technique for determining the sizes of supported metal particles over the standard TEM and XRD methods, usually used for these purposes, were shown in the case of Au/C catalysts. Particle size distributions of gold in a wide range (1–50 nm) were obtained from the SAXS data, including for all size fractions present in the samples. The mass fractions of X-ray amorphous gold particles smaller than 4 nm (WSAXS) were determined. The oxidative treatment of the carbon support before the deposition of the metallic gold precursor complexes has a significant effect on the size distribution of gold particles in the final catalyst. A comparison of the experimental rates of CO oxidation with an excess of moist air at 40°C on Au/C catalysts with the WSAXS values found for these catalysts showed that the catalytic activity increased exponentially as WSAXS increased. The Au/C catalysts with WSAXS ≥ 80% showed high activity in the oxidation of CO.

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ACKNOWLEDGMENTS

We are grateful to E.Yu. Gerasimov, D.A. Zyuzin, and M.S. Mel’gunov for help with performing this research. The SAXS measurements were performed using the equipment provided by the High Technologies and Analysis of Nanosystems (VTAN) Multiaccess Center of Novosibirsk State University.

Funding

This study was supported by the Ministry of Science and Higher Education of the Russian Federation (project FSUS-2020-0029) and was performed under the government contract at the Institute of Catalysis, Siberian Branch, Russian Academy of Sciences (project no. AAAA-A21-121011390053-4).

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Authors and Affiliations

  1. Boreskov Institute of Catalysis, Siberian Branch of the Russian Academy of Sciences, 630090, Novosibirsk, Russia

    Yu. V. Larichev, P. A. Pyrjaev & V. I. Bukhtiyarov

  2. Novosibirsk State University, 630090, Novosibirsk, Russia

    Yu. V. Larichev, B. L. Moroz & V. I. Bukhtiyarov

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  1. Yu. V. Larichev
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Translated by L. Smolina

Abbreviations and designations: SAXS, small-angle X-ray scattering; TEM, transmission electron microscopy; XRD, X-ray diffraction analysis; SCA, specific catalytic activity; CSR, coherent scattering region; PSD, metal particle size distribution; CS, carbon support; XRF, X-ray fluorescence analysis; SBET, specific surface area; VΣ, total volume of pores with sizes of 0.35–100 nm; BET, Brunauer–Emmett–Teller method; Dp, average pore diameter; Vμ, volume of micropores; D111, average size of the CSR of gold; IRM, initial reaction mixture; FRM, final reaction mixture; ХСО, CO conversion; A, catalytic activity; U, space velocity of IRM fed in the reactor; MAu, molar mass of gold; mAu, mass of gold in the catalyst sample; Vm, molar volume of the ideal gas; dl, dm, and dvs, the number-average, mass-average, and volume-surface diameters; DN(d) and DV(d), numerical and volume particle size distributions; WXRD and WSAXS, fractions of fine particles according to XRD and SAXS data; DSAXS, average particle size determined from the volumetric distribution according to the SAXS data; CA, cationic adsorption; and AA, anionic adsorption.

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Larichev, Y.V., Moroz, B.L., Pyrjaev, P.A. et al. Using SAXS for Determining the Sizes of Gold Nanoparticles in Au/C Catalysts: Advantages over Other Methods. Kinet Catal 64, 882–894 (2023). https://doi.org/10.1134/S0023158423060083

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