In situ direct observation of photocorrosion in ZnO crystals in ionic liquid using a laser-equipped high-voltage electron microscope

ZnO photocatalysts in water react with environmental water molecules and corrode under illumination. ZnO nanorods in water can also grow because of water splitting induced by UV irradiation. To investigate their morphological behavior caused by crystal growth and corrosion, here we developed a new laser-equipped high-voltage electron microscope and observed crystal ZnO nanorods immersed in ionic liquid. Exposing the specimen holder to a laser with a wavelength of 325 nm, we observed the photocorrosion in situ at the atomic scale for the first time. This experiment revealed that Zn and O atoms near the interface between the ZnO nanorods and the ionic liquid tended to dissolve into the liquid. The polarity and facet of the nanorods were strongly related to photocorrosion and crystal growth.

[1]  L. Zhang,et al.  Tuning Optoelectrical Properties of ZnO Nanorods with Excitonic Defects via Submerged Illumination. , 2017, Nano letters.

[2]  Grant M. Rotskoff,et al.  Single-particle mapping of nonequilibrium nanocrystal transformations , 2016, Science.

[3]  S. Haigh,et al.  Molecular transport through capillaries made with atomic-scale precision , 2016, Nature.

[4]  Zhong Lin Wang,et al.  In situ transmission electron microscopy observation of ZnO polar and non-polar surfaces structure evolution under electron beam irradiation , 2016 .

[5]  S. Yatsu,et al.  Synthesis of stainless steel nanoballs via submerged glow-discharge plasma and its photocatalytic performance in methylene blue decomposition , 2015 .

[6]  Takahiko Kato,et al.  A pathway of nanocrystallite fabrication by photo-assisted growth in pure water , 2015, Scientific Reports.

[7]  S. Kuwabata,et al.  Single-step preparation of two-dimensionally organized gold particles via ionic liquid/metal sputter deposition. , 2015, Physical chemistry chemical physics : PCCP.

[8]  S. Kuwabata,et al.  Synthesis of alloy AuCu nanoparticles with the L1₀ structure in an ionic liquid using sputter deposition. , 2015, Dalton transactions.

[9]  S. Kuwabata,et al.  Atomic resolution imaging of gold nanoparticle generation and growth in ionic liquids. , 2014, Journal of the American Chemical Society.

[10]  S. Yatsu,et al.  Effects of nanosecond-pulsed laser irradiation on nanostructure formation on the surface of thin Au films on SiO2 glass substrates , 2014 .

[11]  James E. Evans,et al.  Direct observation of aggregative nanoparticle growth: kinetic modeling of the size distribution and growth rate. , 2014, Nano letters.

[12]  James E. Evans,et al.  Demonstration of an electrochemical liquid cell for operando transmission electron microscopy observation of the lithiation/delithiation behavior of Si nanowire battery anodes. , 2013, Nano letters.

[13]  T. Shibayama,et al.  Ion irradiation synthesis of Ag-Au bimetallic nanospheroids in SiO2 glass substrate with tunable surface plasmon resonance frequency , 2013 .

[14]  Takahiko Kato,et al.  The Irradiation Effect of a Simultaneous Laser and Electron Dual-beam on Void Formation , 2013, Scientific Reports.

[15]  S. Whitelam,et al.  Real-Time Imaging of Pt3Fe Nanorod Growth in Solution , 2012, Science.

[16]  J. Banfield,et al.  Direction-Specific Interactions Control Crystal Growth by Oriented Attachment , 2012, Science.

[17]  Daniel J. Hellebusch,et al.  High-Resolution EM of Colloidal Nanocrystal Growth Using Graphene Liquid Cells , 2012, Science.

[18]  S. Dahl,et al.  In situ transmission electron microscopy of light-induced photocatalytic reactions , 2012, Nanotechnology.

[19]  M. Kawai,et al.  Dislocation Loop Formation and Growth under In Situ Laser and/or Electron Irradiation , 2011, Scientific reports.

[20]  N. de Jonge,et al.  Electron microscopy of specimens in liquid. , 2011, Nature nanotechnology.

[21]  Shalendra Kumar,et al.  Growth and characterization of ZnO nanorods by microwave-assisted route: green chemistry approach , 2011 .

[22]  E. Boyden,et al.  Face-selective electrostatic control of hydrothermal zinc oxide nanowire synthesis. , 2011, Nature materials.

[23]  James E. Evans,et al.  Controlled growth of nanoparticles from solution with in situ liquid transmission electron microscopy. , 2011, Nano letters.

[24]  Keita Kobayashi,et al.  Direct HRTEM observation of ultrathin freestanding ionic liquid film on carbon nanotube grid. , 2011, ACS nano.

[25]  T. Kato,et al.  In situ observation of self-organizing nanodot formation under nanosecond-pulsed laser irradiation on Si surface , 2010 .

[26]  G. Jung,et al.  Polymer‐Templated Hydrothermal Growth of Vertically Aligned Single‐Crystal ZnO Nanorods and Morphological Transformations Using Structural Polarity , 2010 .

[27]  M. Rudneva,et al.  In situ High Resolution Electron Microscopy , 2010 .

[28]  Y. Qian,et al.  Sunlight-assisted fabrication of a hierarchical ZnO nanorod array structure , 2009 .

[29]  Lei Jin,et al.  ZnO with Different Morphologies Synthesized by Solvothermal Methods for Enhanced Photocatalytic Activity , 2009 .

[30]  N. Tanaka,et al.  In situ high-resolution transmission electron microscopy of photocatalytic reactions by excited electrons in ionic liquid. , 2007, Journal of electron microscopy.

[31]  S. Yatsu,et al.  Controlled formation of metallic nanoballs during plasma electrolysis , 2007 .

[32]  S. Kuwabata,et al.  Observation of Ionic Liquid by Scanning Electron Microscope , 2006 .

[33]  A. Zewail.  4D ultrafast electron diffraction, crystallography, and microscopy. , 2006, Annual review of physical chemistry.

[34]  Nobuo Tanaka,et al.  In situ high-resolution transmission electron microscopy observation of photodecomposition process of poly-hydrocarbons on catalytic TiO2 films , 2004 .