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Title: Direct observation of the redistribution of sulfur and polysufides in Li-S batteries during first cycle by in situ X-Ray fluorescence microscopy

Journal Article · · Advanced Energy Materials
 [1];  [2];  [1];  [1];  [2];  [1];  [1];  [3];  [4];  [2];  [5];  [1]
  1. Brookhaven National Laboratory (BNL), Upton, NY (United States)
  2. Pacific Northwest National Laboratory, Joint Center for Energy Storage Research, Richland, WA (United States)
  3. Dongguk University-Seoul, Department of Energy and Materials Engineering, (Republic of Korea)
  4. Univ. of Massachusetts at Boston, Dept. of Chemistry, MA (United States)
  5. Argonne National Laboratory, X-ray Science Division, Lemont, IL (United States)

The demands on low cost and high energy density rechargeable batteries for both transportation and large-scale stationary energy storage are stimulating more and more research toward new battery systems. Since sulfur is an earth-abundant material with low cost, research on the high energy density Li–S batteries (2600 W h kg⁻¹) are getting more and more attention. The reactions between sulfur and lithium during charge–discharge cycling are quite complicated, going through multiple electron transfer process associated with chemical and electrochemical equilibrium between long- and short-chain polysulfide Li₂Sx intermediates (1 < x ≤ 8). It is reported that the long-chain polysulfides can be dissolved into electrolyte with aprotic organic solvents and migrated to the Li anode side. This so-called “shuttle effect” is believed to be the main reason for capacity loss and low columbic efficiency of the Li–S batteries. In the past few years, a great deal of efforts have been made on how to overcome the problem of polysulfide dissolution through new sulfur electrode construction and cell designs, as well as the modification of the electrolyte. Although it has been reported by several publications that some Li–S cells can sustain more than a thousand cycles based on the thin film electrode configurations, the long-term cycling stability is still one of the major barriers for the real application of Li–S batteries. More in-depth studies on the fundamental understanding of the sulfur reaction mechanism and interactions among the different polysulfide species, the electrolyte and the electrodes are still greatly needed. Various in situ techniques have been developed and applied to study the mechanism of the sulfur chemistry in Li–S batteries during electrochemical cycling, such as transmission X-ray microscopy (TXM), X-ray absorption spectroscopy (XAS), X-ray diffraction (XRD), UV–visible spectroscopy, and electron paramagnetic resonance (EPR). The applications of these characterization techniques have demonstrated their power in probing the structure changes, morphology evolutions, and coordination of sulfur and polysulfides with the electrolyte in Li–S cells, providing complementary information to each other thus enhancing the understanding in Li–S battery systems. In this communication, in situ X-ray fluorescence (XRF) microscopy was combined with XAS to directly probe the morphology changes of Li–S batteries during first cycle. The morphology changes of the sulfur electrode and the redistribution of sulfur and polysulfides were monitored in real time through the XRF images, while the changes of the sulfur containing compounds were characterized through the XAS spectra simultaneously. In contrast to other studies using ex situ or single characterization technique as reported in the literatures, the in situ technique used in this work has the unique feature of probing the Li–S cell under operating conditions, as well as the combination of XRF imaging with spectroscopy data. By doing this, the morphology evolution and redistribution of specific sulfur particles during cycling can be tracked and identified at certain locations in a real time. In addition, this technique allows us to select the field-of-view (FOV) area from micrometer to centimeter size, providing the capability to study the Li–S reactions not just at the material level, but also at the electrode level. This is very important for both understanding Li–S chemistry and designing effective strategies for Li–S batteries.

Research Organization:
Brookhaven National Laboratory (BNL), Upton, NY (United States)
Sponsoring Organization:
USDOE Office of Energy Efficiency and Renewable Energy (EERE)
Grant/Contract Number:
SC00112704
OSTI ID:
1177848
Report Number(s):
BNL-107699-2015-JA; R&D Project: MA453MAEA; VT1201000
Journal Information:
Advanced Energy Materials, Vol. 5, Issue 16; ISSN 1614-6832
Publisher:
WileyCopyright Statement
Country of Publication:
United States
Language:
English
Citation Metrics:
Cited by: 67 works
Citation information provided by
Web of Science

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A Comprehensive Understanding of Lithium–Sulfur Battery Technology journal June 2019
Structure-Property Relationships of Organic Electrolytes and Their Effects on Li/S Battery Performance journal June 2017
Revisiting the Role of Polysulfides in Lithium-Sulfur Batteries journal March 2018
Review on High-Loading and High-Energy Lithium-Sulfur Batteries journal May 2017
Deciphering the Reaction Mechanism of Lithium–Sulfur Batteries by In Situ/Operando Synchrotron‐Based Characterization Techniques journal March 2019
Activating Inert Metallic Compounds for High‐Rate Lithium–Sulfur Batteries Through In Situ Etching of Extrinsic Metal journal March 2019
A Toolbox for Lithium-Sulfur Battery Research: Methods and Protocols journal June 2017
In Situ Probing Multiple-Scale Structures of Energy Materials for Li-Ion Batteries journal May 2019
High-performance Li–S battery cathode with catalyst-like carbon nanotube-MoP promoting polysulfide redox journal June 2017
Understanding the Reaction Mechanism of Lithium–Sulfur Batteries by In Situ/Operando X-ray Absorption Spectroscopy journal March 2019
Toward Better Lithium–Sulfur Batteries: Functional Non-aqueous Liquid Electrolytes journal August 2018
Using in situ and operando methods to characterize phase changes in charged lithium nickel cobalt aluminum oxide cathode materials journal January 2020
Review—Solid Electrolytes for Safe and High Energy Density Lithium-Sulfur Batteries: Promises and Challenges journal June 2017
Activating Inert Metallic Compounds for High‐Rate Lithium–Sulfur Batteries Through In Situ Etching of Extrinsic Metal journal January 2019
Review : Solid Electrolytes for Safe and High Energy Density Lithium-Sulfur Batteries : Promises and Challenges text January 2018
Directing the Lithium–Sulfur Reaction Pathway via Sparingly Solvating Electrolytes for High Energy Density Batteries journal May 2017
High sulfur-containing carbon polysulfide polymer as a novel cathode material for lithium-sulfur battery journal September 2017