Effective fabrication of porous Au-Ag alloy nanorods for in situ Raman monitoring catalytic oxidation and reduction reactions

doi:10.1016/j.jmst.2021.01.095

Abstract

Abstract:

Porous metal nanostructures exhibit excellent catalytic properties due to their high surface-to-volume ratios and abundant catalytic active sites. However, it is still challenging to control nanopores density and structural features in a facile route and the preparation of porous alloy nanorods for catalytic application has not been well explored. In this work, we demonstrate a synthetic strategy to fabricate highly porous Au-Ag alloy nanorods (P-AuAgNRs) by critically dealloying Ag atoms from homogeneous solid Au-Ag alloy nanorods (AuAgNRs). Combining the merits of the tunable plasmonic properties of noble metal nanorods, excellent stabilities of alloys, and superior catalytic activities of porous structures, we use the P-AuAgNRs as a Raman probe for the in situ monitoring of the catalytic oxidation of 3,3’,5,5’ tetramethylbenzidine (TMB) and reduction of 4-nitrothiophenol (4-NTP). We also compare their composition-dependent catalytic activities. The results show that P-AuAgNRs possess superior chemical stability and higher catalytic activity than those of core-shell structures due to synergistic structural and chemical mechanisms. This strategy provides a predictive design approach for the next-generation alloy catalysts with high-performance.

Key words: Catalysis, Porous Au-Ag alloy nanorod, High-index facets, Raman monitoring, Oxidation and reduction

Shanlin Ke, Caixia Kan, Xingzhong Zhu, Changshun Wang, Weijian Gao, Zhaosheng Li, Xiaoguang Zhu, Daning Shi. Effective fabrication of porous Au-Ag alloy nanorods for in situ Raman monitoring catalytic oxidation and reduction reactions[J]. J. Mater. Sci. Technol., 2021, 91: 262-269.

Figures/Tables 5

Fig. 1. (a) Extinction spectra of Au@AgNRs (A) and UT-AuAgNRs (B) and T-AuAgNRs (C). Insets show the corresponding colloidal solution colors. (b) Extinction spectra of P-AuAgNRs as a function of dealloying time. Insets indicate the color changes of P-AuAgNRs during dealloying. (c-f) Representative TEM images of P-AuAgNRs obtained after etching with Fe(NO3)3 for different times: (c) 5 min, (d) 10 min, (e) 30 min, and (f) 120 min.

Fig. 2. (a) Low-magnification HAADF-STEM image of P-AuAgNRs. (b) High-magnification HAADF-STEM image of a single P-AuAgNR, and (c-e) their corresponding elemental maps. (f, g) EDX line scans along and perpendicular to the long axis of P-AuAgNR, respectively.

Fig. 3. (a) Aberration-corrected HAADF-STEM image of P-AuAgNRs at low magnification. The diffraction pattern (inset) shows that P-AuAgNRs are single-crystalline. The marked squares denote the areas resolved by HAADF-STEM in the following observing. (b-f) Surface planes with monatomic terraces, steps, kinks, and vacancies were observed. The schematics illustration atomic-scale structural characterization of the corresponding high-index or low-index faceting are exhibited in each graph inset. (g) Schematics illustration of various catalytic sites.

Fig. 4. Extinction spectra of (a) AuAgNR and (c) Au@AgNR exposed to an aqueous etching solution, H2O2 (1.5 vol.%) and NH3·H2O (1 vol.%) in the presence of CTAC, and using 120 µL Fe(NO3)3 as the etchant for (b) AuAgNR and (d) Au@AgNR. Colloidal SERS spectra of 4-NTP on (e) Au@AgNR and (f) AuAgNR dispersed in an aqueous etching solution, H2O2 (1.5 vol.%) and NH3·H2O (1 vol.%) in the presence of CTAC for 10 min.

Fig. 5. (a) Chematic illustrating of the oxidation of TMB by H2O2 and the reduction of 4-NTP by NaBH4 using P-AuAgNRs nanocatalysts. (b, c) The SERS spectra of TMB recorded at different time intervals during the peroxidase-like catalytic reaction in the presence of H2O2 and (d) the corresponding SERS intensities at 1611 cm-1 versus reaction time. (e) Color-coded intensity map of time-dependent SERS signals obtained from 4-NTP adsorbed on the surfaces of P-AuAgNRs (etching time=30 min) at different reaction times. (f) Representative SERS signals acquired from 4-NTP functionalized on P-AuAgNRs at different reaction times. (g) Fraction of reactant (4-NTP) as a function of reaction time during the reduction catalyzed by P-AuAgNRs, and the rate constant (blue line) obtained via plotting the logarithm of the Raman intensity at 1340 cm-1 versus reaction time. The error bars denote the standard deviations accomplished from 3 measurements.

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