Revealing the Structural Evolution of Green Rust Synthesized in Ionic Liquids by In Situ Molecular Imaging

Shen, Yanjie; Fu, Yao; Yao, Jennifer; Lao, David; Nune, Satish; Zhu, Zihua; Heldebrant, David; Yao, Xiaohong; Yu, Xiao‐Ying

doi:10.1002/admi.202000452

Revealing the Structural Evolution of Green Rust Synthesized in Ionic Liquids by In Situ Molecular Imaging

Journal Article · Tue May 12 00:00:00 EDT 2020 · Advanced Materials Interfaces

DOI:https://doi.org/10.1002/admi.202000452· OSTI ID:1618336

Shen, Yanjie ^[1]; Fu, Yao ^[2]; Yao, Jennifer ^[2]; Lao, David ^[2]; Nune, Satish ^[2]; Zhu, Zihua ^[3]; Heldebrant, David ^[2]; Yao, Xiaohong ^[4]; ^[2]

Energy and Environment Directorate Pacific Northwest National Laboratory Richland WA 99354 USA, Key Lab of Marine Environmental Science and Ecology (MoE) Ocean University of China Qingdao 266100 China
Energy and Environment Directorate Pacific Northwest National Laboratory Richland WA 99354 USA
Environmental Molecular Sciences Laboratory Pacific Northwest National Laboratory Richland WA 99354 USA
Key Lab of Marine Environmental Science and Ecology (MoE) Ocean University of China Qingdao 266100 China

Abstract

Ionic liquids are green solvents that have wide applications in material synthesis, catalysis, and separation. A model switchable ionic liquid (SWIL) consisting of 1,8‐diazabicycloundec‐7‐ene (DBU) and 1‐hexanol with carbon dioxide (CO ₂ ) as the trigger gas is chosen to synthesize nanocrystalline green rust. Under anoxic conditions, by adding iron (II) acetate (Fe(C ₂ H ₃ O ₂ ) ₂ ) and methanol to the degassed SWIL, a nanoparticulate green rust with carbonate (nano‐GR) is synthesized. More importantly, the molecular structural change of the ionic liquid resulting in green rust crystallines is first characterized using in situ liquid using time‐of‐flight secondary ion mass spectrometry (ToF‐SIMS) coupled with the system for analysis at the liquid vacuum interface (SALVI), a vacuum compatible microfluidic reactor in this work. Dimers and ionic clusters consisting ferric and ferrous ions are identified in liquid ToF‐SIMS spectra. Spectral principal component analysis is used to confirm that these ion pairs including dimers and cluster ions are different from nonionic liquids. The results show that liquid ToF‐SIMS can be a useful tool to study complex liquids at the molecular level providing insights into predicative synthesis of nanomaterials using environmentally friendly green solvents and giving unique visualization of the evolving material interface due to nucleation.

View Accepted Manuscript (Publisher)

Sponsoring Organization:: USDOE

Grant/Contract Number:: AC05-76RL01830

OSTI ID:: 1618336

Journal Information:: Advanced Materials Interfaces, Journal Name: Advanced Materials Interfaces Journal Issue: 15 Vol. 7; ISSN 2196-7350

Publisher:: Wiley Blackwell (John Wiley & Sons)Copyright Statement

Country of Publication:: Germany

Language:: English

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