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Title: Final Technical Report: Application of in situ Neutron Diffraction to Understand the Mechanism of Phase Transitions

Abstract

In this research, phase transitions in the bulk electrodes for Li-ion batteries were investigated using neutron diffraction (ND) as well as neutron imaging techniques. The objectives of this research is to design of a novel in situ electrochemical cell to obtain Rietveld refinable neutron diffraction experiments using small volume electrodes of various laboratory/research-scale electrodes intended for Li-ion batteries. This cell is also to be used to investigate the complexity of phase transitions in Li(Mg) alloy electrodes, either by diffraction or by neutron imaging, which occur under electrochemical lithiation and delithiation, and to determine aspects of phase transition that enable/limit energy storage capacity. Additional objective is to investigate the phase transitions in electrodes made of etched micro-columns of silicon and investigate the effect of particle/column size on phase transitions and nonequilibrium structures. An in situ electrochemical cell was designed successfully and was used to study the phase transitions under in-situ neutron diffraction in both the electrodes (anode/cathode) simultaneously in graphite/LiCoO 2 and in graphite/LiMn 2O 4 cells each with two cells. The diffraction patterns fully validated the working of the in situ cell. Additional experimental were performed using the Si micro-columnar electrodes. The results revealed new lithiation phenomena, as evidenced bymore » mosaicity formation in silicon electrode. These experiments were performed in Vulcan diffractometer at SNS, Oak Ridge National Laboratory. In parallel, the spatial distribution of Li during lithiation and delithiation processes in Li-battery electrodes were investigated. For this purpose, neutron tomographic imaging technique has been used for 3D mapping of Li distribution in bulk Li(Mg) alloy electrodes. It was possible to observe the phase boundary of Li(Mg) alloy indicating phase transition from Li-rich BCC β-phase to Li-lean α-phase. These experiments have been performed at CG-1D Neutron Imaging Prototype Station at SNS.« less

Authors:
ORCiD logo [1]
  1. Univ. of Utah, Salt Lake City, UT (United States). Dept. of Metallurgical Engineering
Publication Date:
Research Org.:
Univ. of Utah, Salt Lake City, UT (United States)
Sponsoring Org.:
USDOE Office of Science (SC)
Contributing Org.:
Oak Ridge National Laboratory (ORNL)
OSTI Identifier:
1419943
Report Number(s):
DE-Utah-SC-0008681
DOE Contract Number:  
SC0008681
Resource Type:
Technical Report
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; 25 ENERGY STORAGE; Neutron diffraction; neutron imaging; electro-chemical; lithium; magnesium; silicon; electrode; battery

Citation Formats

Chandran, Ravi. Final Technical Report: Application of in situ Neutron Diffraction to Understand the Mechanism of Phase Transitions. United States: N. p., 2018. Web. doi:10.2172/1419943.
Chandran, Ravi. Final Technical Report: Application of in situ Neutron Diffraction to Understand the Mechanism of Phase Transitions. United States. doi:10.2172/1419943.
Chandran, Ravi. Fri . "Final Technical Report: Application of in situ Neutron Diffraction to Understand the Mechanism of Phase Transitions". United States. doi:10.2172/1419943. https://www.osti.gov/servlets/purl/1419943.
@article{osti_1419943,
title = {Final Technical Report: Application of in situ Neutron Diffraction to Understand the Mechanism of Phase Transitions},
author = {Chandran, Ravi},
abstractNote = {In this research, phase transitions in the bulk electrodes for Li-ion batteries were investigated using neutron diffraction (ND) as well as neutron imaging techniques. The objectives of this research is to design of a novel in situ electrochemical cell to obtain Rietveld refinable neutron diffraction experiments using small volume electrodes of various laboratory/research-scale electrodes intended for Li-ion batteries. This cell is also to be used to investigate the complexity of phase transitions in Li(Mg) alloy electrodes, either by diffraction or by neutron imaging, which occur under electrochemical lithiation and delithiation, and to determine aspects of phase transition that enable/limit energy storage capacity. Additional objective is to investigate the phase transitions in electrodes made of etched micro-columns of silicon and investigate the effect of particle/column size on phase transitions and nonequilibrium structures. An in situ electrochemical cell was designed successfully and was used to study the phase transitions under in-situ neutron diffraction in both the electrodes (anode/cathode) simultaneously in graphite/LiCoO2 and in graphite/LiMn2O4 cells each with two cells. The diffraction patterns fully validated the working of the in situ cell. Additional experimental were performed using the Si micro-columnar electrodes. The results revealed new lithiation phenomena, as evidenced by mosaicity formation in silicon electrode. These experiments were performed in Vulcan diffractometer at SNS, Oak Ridge National Laboratory. In parallel, the spatial distribution of Li during lithiation and delithiation processes in Li-battery electrodes were investigated. For this purpose, neutron tomographic imaging technique has been used for 3D mapping of Li distribution in bulk Li(Mg) alloy electrodes. It was possible to observe the phase boundary of Li(Mg) alloy indicating phase transition from Li-rich BCC β-phase to Li-lean α-phase. These experiments have been performed at CG-1D Neutron Imaging Prototype Station at SNS.},
doi = {10.2172/1419943},
journal = {},
number = ,
volume = ,
place = {United States},
year = {Fri Feb 09 00:00:00 EST 2018},
month = {Fri Feb 09 00:00:00 EST 2018}
}

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