AVS 63rd International Symposium & Exhibition
    In-Situ and Operando Spectroscopy and Microscopy for Catalysts, Surfaces, & Materials Focus Topic Friday Sessions
       Session IS-FrM

Paper IS-FrM9
In situ Characterization of Green Rust Synthesized in Ionic Liquids by Liquid ToF-SIMS and SALVI

Friday, November 11, 2016, 11:00 am, Room 101C

Session: In situ Characterization of Nanomaterials
Presenter: Juan Yao, Pacific Northwest National Laboratory
Authors: J. Yao, Pacific Northwest National Laboratory
X. Sui, Pacific Northwest National Laboratory
D. Lao, Pacific Northwest National Laboratory
J. Weisenfeld, Pacific Northwest National Laboratory
Y. Zhou, Pacific Northwest National Laboratory
S. Nune, Pacific Northwest National Laboratory
D. Heldebrant, Pacific Northwest National Laboratory
Z. Zhu, Pacific Northwest National Laboratory
X.-Y. Yu, Pacific Northwest National Laboratory
Correspondent: Click to Email
Ionic liquids as green solvents have wide applications in material synthesis, catalysis, and separation. A model switchable ionic liquids (SWILs) consisting of 1,8-diazabicycloundec-7-ene (DBU) and 1-hexanol with carbon dioxide (CO2) gas was chosen to synthesize nanocrystalline green rust. Under anoxic conditions, a nanoparticulate green rust with carbonate (nano GR) was synthesized by the addition of methanol to the degassed switchable ionic liquid (SWIL) solution consisting of 1-hexanol, DBU, CO2 and iron (II) acetate (Fe(C2H3O2)2). The structure and oxidation state of nanocrystalline green rust were confirmed using SEM, TEM and Mössbauer spectroscopy. More importantly, the molecular structure change of the ionic liquid leading to green rust formation was characterized using in situ liquid using time-of-flight secondary ion mass spectrometry (ToF-SIMS) coupled with a vacuum compatible microfluidic reactor, SALVI (System for Analysis at the Liquid Vacuum Interface). Principal component analysis (PCA) was conducted to identify the key components of the solvated iron acetate in methanol and the green rust synthesized in the SWILs. Our results show that liquid SIMS can be a useful tool to study complex liquids at the molecular level providing insights in predicative synthesis of nanomaterials using environmentally friendly solvents.