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Title: Synchrotron X-ray Analytical Techniques for Studying Materials Electrochemistry in Rechargeable Batteries

Abstract

Rechargeable battery technologies have ignited major breakthroughs in contemporary society, including but not limited to revolutions in transportation, electronics, and grid energy storage. The remarkable development of rechargeable batteries is largely attributed to in-depth efforts to improve battery electrode and electrolyte materials. There are, however, still intimidating challenges of lower cost, longer cycle and calendar life, higher energy density, and better safety for large scale energy storage and vehicular applications. Further progress with rechargeable batteries may require new chemistries (lithium ion batteries and beyond) and better understanding of materials electrochemistry in the various battery technologies. In the past decade, advancement of battery materials has been complemented by new analytical techniques that are capable of probing battery chemistries at various length and time scales. Synchrotron X-ray techniques stand out as one of the most effective methods that allows for nearly nondestructive probing of materials characteristics such as electronic and geometric structures with various depth sensitivities through spectroscopy, scattering, and imaging capabilities. This article begins with the discussion of various rechargeable batteries and associated important scientific questions in the field, followed by a review of synchrotron X-ray based analytical tools (scattering, spectroscopy and imaging) and their successful applications (ex situ, in situ,more » and in operando) in gaining fundamental insights into these scientific questions. Furthermore, electron microscopy and spectroscopy complement the detection length scales of synchrotron X-ray tools, and are also discussed towards the end. We highlight the importance of studying battery materials by combining analytical techniques with complementary length sensitivities, such as the combination of X-ray absorption spectroscopy and electron spectroscopy with spatial resolution, because a sole technique may lead to biased and inaccurate conclusions. We then discuss the current progress of experimental design for synchrotron experiments and methods to mitigate beam effects. Finally, a perspective is provided to elaborate how synchrotron techniques can impact the development of next-generation battery chemistries.« less

Authors:
 [1];  [2];  [3];  [4];  [5];  [5];  [6];  [7];  [4];  [8];  [9];  [10];  [2];  [7];  [4]
  1. Virginia Polytechnic Inst. and State Univ. (Virginia Tech), Blacksburg, VA (United States). Dept. of Chemistry
  2. SLAC National Accelerator Lab., Menlo Park, CA (United States). Stanford Synchrotron Radiation Lightsource (SSRL)
  3. Brookhaven National Lab. (BNL), Upton, NY (United States). Dept. of Chemistry; Chinese Academy of Sciences (CAS), Beijing (China). Inst. of Physics. Beijing National Lab. for Condensed Matter Physics (BNLCP-CAS)
  4. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Energy Storage and Distributed Resources Division
  5. Univ. of California, San Diego, CA (United States). Dept. of Physics
  6. Brookhaven National Lab. (BNL), Upton, NY (United States). Center for Functional Nanomaterials (CFN)
  7. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Advanced Light Source (ALS)
  8. Center for High Pressure Science & Technology Advanced Research, Shanghai (China)
  9. Brookhaven National Lab. (BNL), Upton, NY (United States). Dept. of Chemistry
  10. Univ. of California, San Diego, CA (United States). Dept. of NanoEngineering
Publication Date:
Research Org.:
Brookhaven National Lab. (BNL), Upton, NY (United States). National Synchrotron Light Source II (NSLS-II); Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)
Sponsoring Org.:
USDOE Office of Energy Efficiency and Renewable Energy (EERE), Vehicle Technologies Office (EE-3V); USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22); Chinese Academy of Sciences (CAS)
OSTI Identifier:
1437973
Alternate Identifier(s):
OSTI ID: 1377367
Report Number(s):
BNL-114217-2017-JA
Journal ID: ISSN 0009-2665; R&D Project: MA453MAEA; VT1201000
Grant/Contract Number:
SC0012704; SC0001805; AC02-76SF00515; 2016YFA0202500; AC02-05CH11231
Resource Type:
Journal Article: Accepted Manuscript
Journal Name:
Chemical Reviews
Additional Journal Information:
Journal Volume: 117; Journal Issue: 21; Journal ID: ISSN 0009-2665
Publisher:
American Chemical Society
Country of Publication:
United States
Language:
English
Subject:
25 ENERGY STORAGE; National Synchrotron Light Source II; 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY

Citation Formats

Lin, Feng, Liu, Yijin, Yu, Xiqian, Cheng, Lei, Singer, Andrej, Shpryko, Oleg G., Xin, Huolin L., Tamura, Nobumichi, Tian, Chixia, Weng, Tsu-Chien, Yang, Xiao-Qing, Meng, Ying Shirley, Nordlund, Dennis, Yang, Wanli, and Doeff, Marca M. Synchrotron X-ray Analytical Techniques for Studying Materials Electrochemistry in Rechargeable Batteries. United States: N. p., 2017. Web. doi:10.1021/acs.chemrev.7b00007.
Lin, Feng, Liu, Yijin, Yu, Xiqian, Cheng, Lei, Singer, Andrej, Shpryko, Oleg G., Xin, Huolin L., Tamura, Nobumichi, Tian, Chixia, Weng, Tsu-Chien, Yang, Xiao-Qing, Meng, Ying Shirley, Nordlund, Dennis, Yang, Wanli, & Doeff, Marca M. Synchrotron X-ray Analytical Techniques for Studying Materials Electrochemistry in Rechargeable Batteries. United States. doi:10.1021/acs.chemrev.7b00007.
Lin, Feng, Liu, Yijin, Yu, Xiqian, Cheng, Lei, Singer, Andrej, Shpryko, Oleg G., Xin, Huolin L., Tamura, Nobumichi, Tian, Chixia, Weng, Tsu-Chien, Yang, Xiao-Qing, Meng, Ying Shirley, Nordlund, Dennis, Yang, Wanli, and Doeff, Marca M. Wed . "Synchrotron X-ray Analytical Techniques for Studying Materials Electrochemistry in Rechargeable Batteries". United States. doi:10.1021/acs.chemrev.7b00007.
@article{osti_1437973,
title = {Synchrotron X-ray Analytical Techniques for Studying Materials Electrochemistry in Rechargeable Batteries},
author = {Lin, Feng and Liu, Yijin and Yu, Xiqian and Cheng, Lei and Singer, Andrej and Shpryko, Oleg G. and Xin, Huolin L. and Tamura, Nobumichi and Tian, Chixia and Weng, Tsu-Chien and Yang, Xiao-Qing and Meng, Ying Shirley and Nordlund, Dennis and Yang, Wanli and Doeff, Marca M.},
abstractNote = {Rechargeable battery technologies have ignited major breakthroughs in contemporary society, including but not limited to revolutions in transportation, electronics, and grid energy storage. The remarkable development of rechargeable batteries is largely attributed to in-depth efforts to improve battery electrode and electrolyte materials. There are, however, still intimidating challenges of lower cost, longer cycle and calendar life, higher energy density, and better safety for large scale energy storage and vehicular applications. Further progress with rechargeable batteries may require new chemistries (lithium ion batteries and beyond) and better understanding of materials electrochemistry in the various battery technologies. In the past decade, advancement of battery materials has been complemented by new analytical techniques that are capable of probing battery chemistries at various length and time scales. Synchrotron X-ray techniques stand out as one of the most effective methods that allows for nearly nondestructive probing of materials characteristics such as electronic and geometric structures with various depth sensitivities through spectroscopy, scattering, and imaging capabilities. This article begins with the discussion of various rechargeable batteries and associated important scientific questions in the field, followed by a review of synchrotron X-ray based analytical tools (scattering, spectroscopy and imaging) and their successful applications (ex situ, in situ, and in operando) in gaining fundamental insights into these scientific questions. Furthermore, electron microscopy and spectroscopy complement the detection length scales of synchrotron X-ray tools, and are also discussed towards the end. We highlight the importance of studying battery materials by combining analytical techniques with complementary length sensitivities, such as the combination of X-ray absorption spectroscopy and electron spectroscopy with spatial resolution, because a sole technique may lead to biased and inaccurate conclusions. We then discuss the current progress of experimental design for synchrotron experiments and methods to mitigate beam effects. Finally, a perspective is provided to elaborate how synchrotron techniques can impact the development of next-generation battery chemistries.},
doi = {10.1021/acs.chemrev.7b00007},
journal = {Chemical Reviews},
number = 21,
volume = 117,
place = {United States},
year = {Wed Aug 30 00:00:00 EDT 2017},
month = {Wed Aug 30 00:00:00 EDT 2017}
}

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  • Rechargeable battery technologies have ignited major breakthroughs in contemporary society, including but not limited to revolutions in transportation, electronics, and grid energy storage. The remarkable development of rechargeable batteries is largely attributed to in-depth efforts to improve battery electrode and electrolyte materials. There are, however, still intimidating challenges of lower cost, longer cycle and calendar life, higher energy density, and better safety for large scale energy storage and vehicular applications. Further progress with rechargeable batteries may require new chemistries (lithium ion batteries and beyond) and better understanding of materials electrochemistry in the various battery technologies. In the past decade, advancementmore » of battery materials has been complemented by new analytical techniques that are capable of probing battery chemistries at various length and time scales. Synchrotron X-ray techniques stand out as one of the most effective methods that allows for nearly nondestructive probing of materials characteristics such as electronic and geometric structures with various depth sensitivities through spectroscopy, scattering, and imaging capabilities. This article begins with the discussion of various rechargeable batteries and associated important scientific questions in the field, followed by a review of synchrotron X-ray based analytical tools (scattering, spectroscopy and imaging) and their successful applications (ex situ, in situ, and in operando) in gaining fundamental insights into these scientific questions. Furthermore, electron microscopy and spectroscopy complement the detection length scales of synchrotron X-ray tools, and are also discussed towards the end. We highlight the importance of studying battery materials by combining analytical techniques with complementary length sensitivities, such as the combination of X-ray absorption spectroscopy and electron spectroscopy with spatial resolution, because a sole technique may lead to biased and inaccurate conclusions. We then discuss the current progress of experimental design for synchrotron experiments and methods to mitigate beam effects. Finally, a perspective is provided to elaborate how synchrotron techniques can impact the development of next-generation battery chemistries.« less
    Cited by 3
  • The emergence of portable telecommunication, computer equipment and ultimately hybrid electric vehicles has created a substantial interest in manufacturing rechargeable batteries that are less expensive, non-toxic, operate for longer time, small in size and weigh less. Li-ion batteries are taking an increasing share of the rechargeable battery market. The present commercial battery is based on a layered LiCoO{sub 2} cathode and a graphitized carbon anode. LiCoO{sub 2} is expensive but it has the advantage being easily manufactured in a reproducible manner. Other low cost layered compounds such as LiNiO{sub 2}, LiNi{sub 0.85}Co{sub 0.15}O{sub 2} or cubic spinels such as LiMn{submore » 2}O{sub 4} have been considered. However, these suffer from cycle life and thermal stability problems. Recently, some battery companies have demonstrated a new concept of mixing two different types of insertion compounds to make a composite cathode, aimed at reducing cost and improving self-discharge. Reports clearly showed that this blending technique can prevent the decline in ·capacity caused by cycling or storage at elevated temperatures. However, not much work has been reported on the charge-discharge characteristics and phase transitions for these composite cathodes. Understanding the structure and structural changes of electrode materials during the electrochemical cycling is the key to develop better .lithium ion batteries. The successful commercialization of the· lithium-ion battery is mainly built on the advances in solid state chemistry of the intercalation compounds. Most of the progress in understanding the lithium ion battery materials has been obtained from x-ray diffraction studies. Up to now, most XRD studies on lithium-ion battery materials have been done ex situ. Although these ex situ XRD studies have provided important information· about the structures of battery materials, they do face three major problems. First of all, the pre-selected charge (discharge) states may not be representative for the full picture of the structural changes during charge (discharge). In other words, the important information might be missed for those charge (discharge) states which were not selected for ex situ XRD studies. Secondly, the structure of the sample may have changed after removed from the cell. Finally, it is impossible to use the ex situ XRD to study the dynamic effects during high rate charge-discharge, which is crucial for the application of lithium-ion batteries for electric vehicle. A few in situ studies have been done using conventional x-ray tube sources. All of the in situ XRD studies using conventional x-ray tube sources have been done in the reflection mode in cells with beryllium windows. Because of the weak signals, data collection takes a long time, often several hundred hours for a single charge-discharge cycle. This long time data collection is not suitable for dynamic studies at all. Furthermore, in the reflection mode, the x-ray beam probes mainly the surface layer of the cathode materials. Iri collaboration with LG Chemical Ltd., BNL group designed and constructed the cells for in situ studies. LG Chemical provided several blended samples and pouch cells to BNL for preliminary in situ study. The LG Chemical provided help on integrate the blended cathode into these cells. The BNL team carried out in situ XAS and XRD studies on the samples and pouch cells provided by LG Chemical under normal charge-discharge conditions at elevated temperature.« less
  • Abstract
  • High performance materials that can withstand radiation, heat, multiaxial stresses, and corrosive environment are necessary for the deployment of advanced nuclear energy systems. Nondestructive in situ experimental techniques utilizing high energy x-rays from synchrotron sources can be an attractive set of tools for engineers and scientists to investigate the structure–processing–property relationship systematically at smaller length scales and help build better material models. In this paper, two unique and interconnected experimental techniques, namely, simultaneous small-angle/wide-angle x-ray scattering (SAXS/WAXS) and far-field high-energy diffraction microscopy (FF-HEDM) are presented. Finally, the changes in material state as Fe-based alloys are heated to high temperatures ormore » subject to irradiation are examined using these techniques.« less