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Frontiers of Optoelectronics

Front. Optoelectron.    2015, Vol. 8 Issue (4) : 379-393     DOI: 10.1007/s12200-014-0423-5
Optical approaches in study of nanocatalysis with single-molecule and single-particle resolution
Kun LI,Weiwei QIN,Yan XU,Tianhuan PENG,Di LI()
Division of Physical Biology & Bioimaging Center, Shanghai Synchrotron Radiation Facility, Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800, China
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Studying the activity of individual nanocatalysts, especially with high spatiotemporal resolution of single-molecule and single-turnover scale, is essential for the understanding of catalytic mechanism and the designing of effective catalysts. Several approaches have been developed to monitor the catalytic reaction on single catalysts. In this review, we summarized the updated progresses of several new spectroscopic and microscopic approaches, including single-molecule fluorescence microscopy, surface-enhanced Raman spectroscopy, surface plasmon resonance microscopy and X-ray microscopy, for the study of single-molecule and single-particle catalysis.

Keywords nanocatalysis      single-molecule fluorescence      surface-enhanced Raman      localized surface plasmon resonance      X-ray     
Corresponding Authors: Di LI   
Online First Date: 11 April 2014    Issue Date: 24 November 2015
 Cite this article:   
Kun LI,Weiwei QIN,Yan XU, et al. Optical approaches in study of nanocatalysis with single-molecule and single-particle resolution[J]. Front. Optoelectron., 2015, 8(4): 379-393.
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Kun LI
Weiwei QIN
Yan XU
Tianhuan PENG

Chemical imaging methods that are available or will become available in the future (in italics), for the investigation of catalysts at the single-particle level. The abbreviations of the included characterization techniques are as follows. Vibrational spectroscopy methods (green): DORS, diagonally offset Raman spectroscopy; IRM, infrared microscopy; CRM, confocal Raman microscopy, CARS, coherent anti-Stokes Raman spectroscopy; SRS, stimulated Raman scattering microscopy; SNIM, scanning near-field infrared microscopy; TERS, tip-enhanced Raman spectroscopy. X-ray spectroscopy methods (blue): μ-XAFS, microbeam X-ray absorption fine structure spectroscopy; XRM, X-ray microscopy; XMT, X-ray microtomography; XAS-SNOM, X-ray absorption spectroscopy/scanning near-field optical microscopy. Electronic spectroscopy methods (red): UV-VIS, ultraviolet–visible microscopy; CFM, confocal fluorescence microscopy; 2PFM, two-photon fluorescence microscopy; CLM, chemiluminescence microscopy; PR-DFM, plasmon resonance dark field microscopy; STED, stimulated emission depletion microscopy; STORM, stochastic optical reconstruction microscopy; FPALM, fluorescence photo-activated localization microscopy; SSIM, saturated structured illumination microscopy. X-ray diffraction methods (black): TEDDI, tomographic energy-dispersive diffraction imaging; XRD-CT, X-ray diffraction-computed tomography; μ-XRD/AFM, microbeam X-ray diffraction/atomic force microscopy. Miscellaneous (orange): MRI, magnetic resonance imaging; IFM, interference microscopy; MSI, mass spectrometry imaging; SHG, second-harmonic generation microscopy; MS-SNOM, mass spectrometry/scanning near-field optical microscopy. Adapted with permission from Ref. [4], copyright 2012 Nature Publishing Group


Single-molecule detection of fluorogenic catalytic reactions on single Au nanoparticles. (a) Experimental design using fluorogenic catalytic reaction, surface immobilized catalysts, and total internal reflection fluorescence microscopy; (b) schematic of a prism-based TIRFM and a microfluidic reactor cell made between a slide and a coverslip; (c) a typical image (~18 μm× 18 μm) of fluorescent products on 6 nm pseudospherical Au nanoparticles during catalysis taken at 100 ms per frame; (d) a segment of the fluorescence trajectory from the fluorescence spot marked by the arrow in (c); (e) schematic diagram of the kinetic mechanism of catalysis. Aum: Au nanoparticle; S: resazurin; P: resorufin. Aum–Sn represents an Au nanoparticle having n adsorbed substrate molecules. The fluorescence state (on or off) of the nanoparticle is indicated at each reaction stage. Figures 2(a) to 2(d) were reproduced with permission from Ref. [23], copyright 2008 Nature Publishing Group. Figure 2(e) was reproduced with permission from Ref. [29], copyright 2010 American Chemical Society


Super-resolution imaging of single particle nanocatalysis. (a) Fluorogenic reaction converts a nonfluorescent molecule (Amplex Red) to a fluorescent molecule (resorufin) catalyzed by individual Au@mSiO2 nanorods; (b) fluorescence intensity versus time trajectory for a single Au@mSiO2 nanorod under catalysis, and wide-field fluorescence pattern during one burst (red circled); (c) subparticle distribution of reactivity map obtained for a gold nanorod. Segmentation of the nanorods clearly shows substrate concentration-dependent turnover rate in different regions; (d) spatially resolved activity quantitation on single Au@mSiO2 nanoplates; (e) and (f) spatial distributions of fluorescence spots collected from TiO2 (e) and 14 nm Au/TiO2 particles (f); (g) super-resolution reaction map showing a single needle like ZSM-22 particle; (h) reconstructed fluorescence maps showing the location of the active intergrowth region on a ZSM-5 crystal; (i) turnover mapping on Ti-MCM-41 particles. Figures 3(a), 3(b), and 3(c) were reproduced with permission from Ref. [34], copyright 2012 Nature Publishing Group. Figure 3(d) was reproduced with permission from Ref. [35], Figs. 3(e) and 3(f) were reproduced with permission from Ref. [40], copyright 2013 American Chemical Society. Figures 3(g), 3(h), and 3(i) were reproduced with permission from Refs. [41,42], copyright 2009, 2010 Wiley


Surface/tip-enhanced Raman spectroscopy for single particle nanocatalysis. (a) Scanning electron microscopy (SEM) image of a single roughened Ag microsphere with nanostructured surface; (b) photo of the gas flow cell for monitoring the surface plasmon assisted catalysis reaction under controlled gas atmosphere; (c) structure schematic of the designed reaction station; (d) time-dependent SERS spectra of 4ATP under continuous 633 nm laser excitation taken every 1 min, and series shown as a color-coded intensity map; (e) schematic overview of the experimental setup for TERS combining confocal Raman and atomic force microscope; (f) time-dependent SERS spectra acquired with the setup for TERS of the photocatalytic reduction of pNTP (top spectrum) to DMAB, and series shown as a color-coded intensity map. Figures 4(a), 4(b), and 4(c) were reproduced with permission from Ref. [54], copyright 2013 Nature Publishing Group. Figures 4(d) and 4(e) were reproduced with permission from Ref. [55], copyright 2012 Nature Publishing Group


Direct localized surface plasmon resonance monitoring of single plasmonic particle nanocatalysis. (a) Scanning electron microscopy (SEM) image of gold decahedron; (b) scattering spectra of nanoparticle vs. time after electron injection by ascorbate ions; (c) spectral shift as a function of time for the catalysis reaction and for the control experiment; (d) evolution of the scattering spectrum of a gold nanorod (aspect ratio 2.87) after a growth solution is added; (e) spectral shift as a function of time for a growth experiment and for a control experiment; (f) predicted surface plasmon position versus aspect ratio for hemispherically capped rods based on DDA results; (g) scheme for the reduction of 4-nitrophenol, catalyzed by gold nanoparticles with ammonia borane as the reducing agent. AB: ammonia borane; 4-NIP: 4-nitrophenol; 4-AMP: 4-aminophenol; (h) and (i) evolution of the scattering spectrum and surface plasmon band position of a gold nanorod (h) and an elongated tetrahexahedral gold nanoparticle (i) as a function of time after introducing water, 10 mM1)<FootNote>

1 mM= 1 mmol?L–6

</FootNote> AB, and 0.1 mM 4-NIP, sequentially. Figures 5(a) to 5(f) were reproduced with permission from Ref. [67], copyright 2008 Nature Publishing Group. Figures 5(g), 5(h), and 5(i) were reproduced with permission from Ref. [69], copyright 2013 Royal Society of Chemistry


Indirect localized surface plasmon resonance monitoring of single particle nanocatalysis. (a) Hydrogen adsorption on a Pd nanoparticle induces minimal wavelength shift in its scattering spectrum; (b) hydrogen sensing with a plasmonic Au nanostructure-antenna enhanced single Pd nanoparticle; (c) maximum scattering wavelength from the Au antenna depends on hydrogen partial pressure; (d) surface plasmon resonance electrochemical current density images of a single Pt nanoparticle at different potentials; (e) cyclic voltammogram of the same single nanoparticle obtained by integrating the current density over the images in (d); (f) typical cyclic voltammograms of three different single Pt nanoparticles. Figures 6(a) to 6(c) were reproduced with permission from Ref. [72], Figs. 6(d) to 6(f) were reproduced with permission from Ref. [77], copyright 2011, 2012 Nature Publishing Group


Indirect localized surface plasmon resonance monitoring of single particle nanocatalysis. (a) Hydrogen adsorption on a Pd nanoparticle induces minimal wavelength shift in its scattering spectrum; (b) hydrogen sensing with a plasmonic Au nanostructure-antenna enhanced single Pd nanoparticle; (c) maximum scattering wavelength from the Au antenna depends on hydrogen partial pressure; (d) surface plasmon resonance electrochemical current density images of a single Pt nanoparticle at different potentials; (e) cyclic voltammogram of the same single nanoparticle obtained by integrating the current density over the images in (d); (f) typical cyclic voltammograms of three different single Pt nanoparticles. Figures 6(a) to 6(c) were reproduced with permission from Ref. [72], Figs. 6(d) to 6(f) were reproduced with permission from Ref. [77], copyright 2011, 2012 Nature Publishing Group

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