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Title: Free-standing bilayered vanadium oxide films synthesized by liquid exfoliation of chemically preintercalated δ-Li x V 2 O 5 · n H 2 O

Abstract

A free-standing film composed of bilayered vanadium oxide nanoflakes is for the first time synthesized using a new low-energy process. The precursor powder, δ-LixV2O5·nH2O, was prepared using a simple sol–gel based chemical preintercalation synthesis procedure. δ-LixV2O5·nH2O was dispersed and probe sonicated in N-methyl pyrrolidone to exfoliate the bilayers followed by vacuum filtration resulting in the formation of a free-standing film with obsidian color. X-ray diffraction showed lamellar ordering of a single-phase material with a decreased interlayer distance compared to that of the precursor powder. Scanning electron microscopy images demonstrated stacking of the individual nanoflakes. This morphology was further confirmed with scanning transmission electron microscopy that showed highly malleable nanoflakes consisting of ~10–100 vanadium oxide bilayers. Furthermore, one of the most important consequences of this morphological rearrangement is that the electronic conductivity of the free-standing film, measured by the four-probe method, increased by an order of magnitude compared to conductivity of the pressed pellet made of precursor powder. X-ray photoelectron spectroscopy measurements showed the coexistence of both V5+ and V4+ oxidation states in the exfoliated sample, possibly contributing to the change in electronic conductivity. The developed approach provides the ability to maintain the phase purity and crystallographic order during the exfoliationmore » process, coupled with the formation of a free-standing film of enhanced conductivity. The produced bilayered vanadium oxide nanoflakes can be used as the building blocks for the synthesis of versatile two-dimensional heterostructures to create innovative electrodes for electrochemical energy storage applications.« less

Authors:
 [1];  [1]; ORCiD logo [1];  [2]; ORCiD logo [1]
  1. Department of Materials Science and Engineering, Drexel University, Philadelphia, USA
  2. Center for Nanophase Materials Sciences, Oak Ridge National Laboratory, Oak Ridge, USA
Publication Date:
Research Org.:
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES); National Science Foundation (NSF); National Research Foundation of Korea (NRF)
OSTI Identifier:
1772526
Alternate Identifier(s):
OSTI ID: 1822047
Grant/Contract Number:  
#DE-SC0012673; AC05-00OR22725; DMR-1752623; 2016K1A4A3945038; 2015K1A4A3047100
Resource Type:
Published Article
Journal Name:
Materials Advances
Additional Journal Information:
Journal Name: Materials Advances Journal Volume: 2 Journal Issue: 8; Journal ID: ISSN 2633-5409
Publisher:
Royal Society of Chemistry (RSC)
Country of Publication:
United Kingdom
Language:
English
Subject:
36 MATERIALS SCIENCE

Citation Formats

Houseman, Luke, Mukherjee, Santanu, Andris, Ryan, Zachman, Michael J., and Pomerantseva, Ekaterina. Free-standing bilayered vanadium oxide films synthesized by liquid exfoliation of chemically preintercalated δ-Li x V 2 O 5 · n H 2 O. United Kingdom: N. p., 2021. Web. doi:10.1039/D1MA00085C.
Houseman, Luke, Mukherjee, Santanu, Andris, Ryan, Zachman, Michael J., & Pomerantseva, Ekaterina. Free-standing bilayered vanadium oxide films synthesized by liquid exfoliation of chemically preintercalated δ-Li x V 2 O 5 · n H 2 O. United Kingdom. https://doi.org/10.1039/D1MA00085C
Houseman, Luke, Mukherjee, Santanu, Andris, Ryan, Zachman, Michael J., and Pomerantseva, Ekaterina. Mon . "Free-standing bilayered vanadium oxide films synthesized by liquid exfoliation of chemically preintercalated δ-Li x V 2 O 5 · n H 2 O". United Kingdom. https://doi.org/10.1039/D1MA00085C.
@article{osti_1772526,
title = {Free-standing bilayered vanadium oxide films synthesized by liquid exfoliation of chemically preintercalated δ-Li x V 2 O 5 · n H 2 O},
author = {Houseman, Luke and Mukherjee, Santanu and Andris, Ryan and Zachman, Michael J. and Pomerantseva, Ekaterina},
abstractNote = {A free-standing film composed of bilayered vanadium oxide nanoflakes is for the first time synthesized using a new low-energy process. The precursor powder, δ-LixV2O5·nH2O, was prepared using a simple sol–gel based chemical preintercalation synthesis procedure. δ-LixV2O5·nH2O was dispersed and probe sonicated in N-methyl pyrrolidone to exfoliate the bilayers followed by vacuum filtration resulting in the formation of a free-standing film with obsidian color. X-ray diffraction showed lamellar ordering of a single-phase material with a decreased interlayer distance compared to that of the precursor powder. Scanning electron microscopy images demonstrated stacking of the individual nanoflakes. This morphology was further confirmed with scanning transmission electron microscopy that showed highly malleable nanoflakes consisting of ~10–100 vanadium oxide bilayers. Furthermore, one of the most important consequences of this morphological rearrangement is that the electronic conductivity of the free-standing film, measured by the four-probe method, increased by an order of magnitude compared to conductivity of the pressed pellet made of precursor powder. X-ray photoelectron spectroscopy measurements showed the coexistence of both V5+ and V4+ oxidation states in the exfoliated sample, possibly contributing to the change in electronic conductivity. The developed approach provides the ability to maintain the phase purity and crystallographic order during the exfoliation process, coupled with the formation of a free-standing film of enhanced conductivity. The produced bilayered vanadium oxide nanoflakes can be used as the building blocks for the synthesis of versatile two-dimensional heterostructures to create innovative electrodes for electrochemical energy storage applications.},
doi = {10.1039/D1MA00085C},
journal = {Materials Advances},
number = 8,
volume = 2,
place = {United Kingdom},
year = {Mon Apr 26 00:00:00 EDT 2021},
month = {Mon Apr 26 00:00:00 EDT 2021}
}

Journal Article:
Free Publicly Available Full Text
Publisher's Version of Record
https://doi.org/10.1039/D1MA00085C

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