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Title: A lithium–oxygen battery based on lithium superoxide

Abstract

Batteries based on sodium superoxide and on potassium superoxide have recently been reported(1-3). But, there have been no reports of a battery based on lithium superoxide (LiO2), despite much research(4-8) into the lithium-oxygen (Li-O2) battery because of its potential high energy density. Several studies(9-16) of Li-O2 batteries have found evidence of LiO2 being formed as one component of the discharge product along with lithium peroxide (Li2O2). In addition, theoretical calculations have indicated that some forms of LiO2 may have a long lifetime(17). Our studies also suggest that it might be possible to form LiO2 alone for use in a battery. However, solid LiO2 has been difficult to synthesize in pure form(18) because it is thermodynamically unstable with respect to disproportionation, giving Li2O2 (refs 19, 20). We show that crystalline LiO2 can be stabilized in a Li-O2 battery by using a suitable graphene-based cathode. Various characterization techniques reveal no evidence for the presence of Li2O2. A novel templating growth mechanism involving the use of iridium nanoparticles on the cathode surface may be responsible for the growth of crystalline LiO2. Our results demonstrate that the LiO2 formed in the Li-O2 battery is stable enough for the battery to be repeatedly charged andmore » discharged with a very low charge potential (about 3.2 volts). We also anticipate that this discovery will lead to methods of synthesizing and stabilizing LiO2, which could open the way to high-energy-density batteries based on LiO2 as well as to other possible uses of this compound, such as oxygen storage.« less

Authors:
 [1];  [2];  [3];  [4];  [5];  [4];  [4];  [6];  [1];  [1];  [6];  [2];  [2];  [7];  [8];  [5];  [2];  [4];  [1]
+ Show Author Affiliations
  1. Argonne National Lab. (ANL), Argonne, IL (United States). Chemical Sciences and Engineering Division
  2. Hanyang Univ., Seoul (Korea, Republic of). Dept. of Energy Engineering
  3. Argonne National Lab. (ANL), Argonne, IL (United States). Materials Science Division; Univ. of Utah, Salt Lake City, UT (United States). Dept. of Metallurgical Engineering
  4. Argonne National Lab. (ANL), Argonne, IL (United States). Materials Science Division
  5. Univ. of Illinois, Chicago, IL (United States). Dept. of Mechanical and Industrial Engineering
  6. Argonne National Lab. (ANL), Argonne, IL (United States). Center for Nanoscale Materials
  7. Univ. of Utah, Salt Lake City, UT (United States). Dept. of Metallurgical Engineering
  8. Univ. of Louisville, KY (United States). Conn Center for Renewable Energy Research
Publication Date:
Research Org.:
Argonne National Laboratory (ANL), Argonne, IL (United States); Energy Frontier Research Centers (EFRC) (United States). Center for Electrical Energy Storage (CEES)
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)
OSTI Identifier:
1352638
Grant/Contract Number:  
AC02-06CH11357
Resource Type:
Accepted Manuscript
Journal Name:
Nature (London)
Additional Journal Information:
Journal Name: Nature (London); Journal Volume: 529; Journal Issue: 7586; Journal ID: ISSN 0028-0836
Publisher:
Nature Publishing Group
Country of Publication:
United States
Language:
English
Subject:
25 ENERGY STORAGE

Citation Formats

Lu, Jun, Jung Lee, Yun, Luo, Xiangyi, Chun Lau, Kah, Asadi, Mohammad, Wang, Hsien-Hau, Brombosz, Scott, Wen, Jianguo, Zhai, Dengyun, Chen, Zonghai, Miller, Dean J., Sub Jeong, Yo, Park, Jin-Bum, Zak Fang, Zhigang, Kumar, Bijandra, Salehi-Khojin, Amin, Sun, Yang-Kook, Curtiss, Larry A., and Amine, Khalil. A lithium–oxygen battery based on lithium superoxide. United States: N. p., 2016. Web. doi:10.1038/nature16484.
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Lu, Jun, Jung Lee, Yun, Luo, Xiangyi, Chun Lau, Kah, Asadi, Mohammad, Wang, Hsien-Hau, Brombosz, Scott, Wen, Jianguo, Zhai, Dengyun, Chen, Zonghai, Miller, Dean J., Sub Jeong, Yo, Park, Jin-Bum, Zak Fang, Zhigang, Kumar, Bijandra, Salehi-Khojin, Amin, Sun, Yang-Kook, Curtiss, Larry A., & Amine, Khalil. A lithium–oxygen battery based on lithium superoxide. United States. https://doi.org/10.1038/nature16484
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Lu, Jun, Jung Lee, Yun, Luo, Xiangyi, Chun Lau, Kah, Asadi, Mohammad, Wang, Hsien-Hau, Brombosz, Scott, Wen, Jianguo, Zhai, Dengyun, Chen, Zonghai, Miller, Dean J., Sub Jeong, Yo, Park, Jin-Bum, Zak Fang, Zhigang, Kumar, Bijandra, Salehi-Khojin, Amin, Sun, Yang-Kook, Curtiss, Larry A., and Amine, Khalil. Mon . "A lithium–oxygen battery based on lithium superoxide". United States. https://doi.org/10.1038/nature16484. https://www.osti.gov/servlets/purl/1352638.
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@article{osti_1352638,
title = {A lithium–oxygen battery based on lithium superoxide},
author = {Lu, Jun and Jung Lee, Yun and Luo, Xiangyi and Chun Lau, Kah and Asadi, Mohammad and Wang, Hsien-Hau and Brombosz, Scott and Wen, Jianguo and Zhai, Dengyun and Chen, Zonghai and Miller, Dean J. and Sub Jeong, Yo and Park, Jin-Bum and Zak Fang, Zhigang and Kumar, Bijandra and Salehi-Khojin, Amin and Sun, Yang-Kook and Curtiss, Larry A. and Amine, Khalil},
abstractNote = {Batteries based on sodium superoxide and on potassium superoxide have recently been reported(1-3). But, there have been no reports of a battery based on lithium superoxide (LiO2), despite much research(4-8) into the lithium-oxygen (Li-O2) battery because of its potential high energy density. Several studies(9-16) of Li-O2 batteries have found evidence of LiO2 being formed as one component of the discharge product along with lithium peroxide (Li2O2). In addition, theoretical calculations have indicated that some forms of LiO2 may have a long lifetime(17). Our studies also suggest that it might be possible to form LiO2 alone for use in a battery. However, solid LiO2 has been difficult to synthesize in pure form(18) because it is thermodynamically unstable with respect to disproportionation, giving Li2O2 (refs 19, 20). We show that crystalline LiO2 can be stabilized in a Li-O2 battery by using a suitable graphene-based cathode. Various characterization techniques reveal no evidence for the presence of Li2O2. A novel templating growth mechanism involving the use of iridium nanoparticles on the cathode surface may be responsible for the growth of crystalline LiO2. Our results demonstrate that the LiO2 formed in the Li-O2 battery is stable enough for the battery to be repeatedly charged and discharged with a very low charge potential (about 3.2 volts). We also anticipate that this discovery will lead to methods of synthesizing and stabilizing LiO2, which could open the way to high-energy-density batteries based on LiO2 as well as to other possible uses of this compound, such as oxygen storage.},
doi = {10.1038/nature16484},
journal = {Nature (London)},
number = 7586,
volume = 529,
place = {United States},
year = {Mon Jan 11 00:00:00 EST 2016},
month = {Mon Jan 11 00:00:00 EST 2016}
}
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    A rechargeable lithium–oxygen battery with dual mediators stabilizing the carbon cathode
    journal, July 2017

    The role of nanotechnology in the development of battery materials for electric vehicles
    journal, December 2016

    Highly reversible zinc metal anode for aqueous batteries
    journal, April 2018

    A high-energy-density and long-life lithium-ion battery via reversible oxide–peroxide conversion
    journal, October 2019

    Theoretical prediction of LiScO 2 nanosheets as a cathode material for Li–O 2 batteries
    journal, January 2018

    • Liu, Zhixiao; Deng, Huiqiu; Zhang, Shiguo
    • Physical Chemistry Chemical Physics, Vol. 20, Issue 34
    • DOI: 10.1039/c8cp01756e

    C x N y particles@N-doped porous graphene: a novel cathode catalyst with a remarkable cyclability for Li–O 2 batteries
    journal, January 2018

    • Wu, Aiming; Shen, Shuiyun; Yan, Xiaohui
    • Nanoscale, Vol. 10, Issue 26
    • DOI: 10.1039/c8nr01049h

    Nature inspired cathodes using high-density carbon papers with an eddy current effect for high-rate performance lithium–air batteries
    journal, January 2018

    • Kim, Min-Cheol; So, Jin-Young; Moon, Sang-Hyun
    • Journal of Materials Chemistry A, Vol. 6, Issue 20
    • DOI: 10.1039/c8ta00281a

    Enhanced cycling stability of Li–O 2 batteries by using a polyurethane/SiO 2 /glass fiber nanocomposite separator
    journal, January 2018

    • Luo, Kun; Zhu, Guangbin; Zhao, Yuzhen
    • Journal of Materials Chemistry A, Vol. 6, Issue 17
    • DOI: 10.1039/c8ta00879e

    Promoting defective-Li 2 O 2 formation via Na doping for Li–O 2 batteries with low charge overpotentials
    journal, January 2019

    • Lyu, Zhiyang; Wang, Tao; Guo, Rui
    • Journal of Materials Chemistry A, Vol. 7, Issue 17
    • DOI: 10.1039/c9ta01606f

    Exploring the charge reactions in a Li–O 2 system with lithium oxide cathodes and nonaqueous electrolytes
    journal, January 2019

    • Zhang, Tao; Amine, Rachid; Bi, Xuanxuan
    • Journal of Materials Chemistry A, Vol. 7, Issue 26
    • DOI: 10.1039/c9ta03763b

    Lithium-air batteries: Challenges coexist with opportunities
    journal, April 2019

    • Wang, Chengyi; Xie, Zhaojun; Zhou, Zhen
    • APL Materials, Vol. 7, Issue 4
    • DOI: 10.1063/1.5091444

    High-capacity rechargeable batteries based on deeply cyclable lithium metal anodes
    journal, May 2018

    • Shi, Qiuwei; Zhong, Yiren; Wu, Min
    • Proceedings of the National Academy of Sciences, Vol. 115, Issue 22
    • DOI: 10.1073/pnas.1803634115

    Tuning anion solvation energetics enhances potassium–oxygen battery performance
    journal, July 2019

    • Sankarasubramanian, Shrihari; Kahky, Joshua; Ramani, Vijay
    • Proceedings of the National Academy of Sciences, Vol. 116, Issue 30
    • DOI: 10.1073/pnas.1901329116

    Nanostructured transition metal dichalcogenide electrocatalysts for CO 2 reduction in ionic liquid
    journal, July 2016

    A high-energy-density lithium-oxygen battery based on a reversible four-electron conversion to lithium oxide
    journal, August 2018

    Building Better Batteries in the Solid State: A Review
    journal, November 2019

    • Mauger, Alain; Julien, Christian M.; Paolella, Andrea
    • Materials, Vol. 12, Issue 23, p. 3892
    • DOI: 10.3390/ma12233892

    A Hybrid Na//K + -Containing Electrolyte//O 2 Battery with High Rechargeability and Cycle Stability
    journal, January 2019

    High-Energy-Density Metal-Oxygen Batteries: Lithium-Oxygen Batteries vs Sodium-Oxygen Batteries
    journal, September 2017

    • Song, Kyeongse; Agyeman, Daniel Adjei; Park, Mihui
    • Advanced Materials, Vol. 29, Issue 48
    • DOI: 10.1002/adma.201606572

    Developing a “Water-Defendable” and “Dendrite-Free” Lithium-Metal Anode Using a Simple and Promising GeCl 4 Pretreatment Method
    journal, July 2018

    Review of Electrolytes in Nonaqueous Lithium-Oxygen Batteries
    journal, March 2018

    • Guo, Haipeng; Luo, Wenbin; Chen, Jun
    • Advanced Sustainable Systems, Vol. 2, Issue 8-9
    • DOI: 10.1002/adsu.201700183

    Recent Advances in Perovskite Oxides as Electrode Materials for Nonaqueous Lithium-Oxygen Batteries
    journal, February 2017

    • Tan, Peng; Liu, Meilin; Shao, Zongping
    • Advanced Energy Materials, Vol. 7, Issue 13
    • DOI: 10.1002/aenm.201602674

    Porous Carbon Composites for Next Generation Rechargeable Lithium Batteries
    journal, May 2017

    Hierarchically Porous, Ultrathick, “Breathable” Wood-Derived Cathode for Lithium-Oxygen Batteries
    journal, September 2017

    Effect of Componential Proportion in Bimetallic Electrocatalysts on the Aprotic Lithium-Oxygen Battery Performance
    journal, April 2018

    Insights into Structural Evolution of Lithium Peroxides with Reduced Charge Overpotential in Li−O 2 System
    journal, June 2019

    • Tan, Guoqiang; Chong, Lina; Zhan, Chun
    • Advanced Energy Materials, Vol. 9, Issue 27
    • DOI: 10.1002/aenm.201900662

    Hydronium-Ion Batteries with Perylenetetracarboxylic Dianhydride Crystals as an Electrode
    journal, February 2017

    • Wang, Xingfeng; Bommier, Clement; Jian, Zelang
    • Angewandte Chemie, Vol. 129, Issue 11
    • DOI: 10.1002/ange.201700148

    Why Do Lithium-Oxygen Batteries Fail: Parasitic Chemical Reactions and Their Synergistic Effect
    journal, July 2016

    • Yao, Xiahui; Dong, Qi; Cheng, Qingmei
    • Angewandte Chemie International Edition, Vol. 55, Issue 38
    • DOI: 10.1002/anie.201601783

    Understanding LiOH Chemistry in a Ruthenium-Catalyzed Li-O 2 Battery
    journal, November 2017

    • Liu, Tao; Liu, Zigeng; Kim, Gunwoo
    • Angewandte Chemie International Edition, Vol. 56, Issue 50
    • DOI: 10.1002/anie.201709886

    Alkali-Oxygen Batteries Based on Reversible Superoxide Chemistry
    journal, October 2018

    • McCulloch, William David; Xiao, Neng; Gourdin, Gerald
    • Chemistry - A European Journal, Vol. 24, Issue 67
    • DOI: 10.1002/chem.201802101

    Applications of Conventional Vibrational Spectroscopic Methods for Batteries Beyond Li-Ion
    journal, March 2018

    Atomic‐Layer‐Deposited Amorphous MoS 2 for Durable and Flexible Li–O 2 Batteries
    journal, May 2019

    CeO2@NiCo2O4 nanowire arrays on carbon textiles as high performance cathode for Li-O2 batteries
    journal, November 2017

    A lithium–oxygen battery with a long cycle life in an air-like atmosphere
    journal, March 2018

    • Asadi, Mohammad; Sayahpour, Baharak; Abbasi, Pedram
    • Nature, Vol. 555, Issue 7697
    • DOI: 10.1038/nature25984

    Anion-redox nanolithia cathodes for Li-ion batteries
    journal, July 2016

    Revealing the reaction mechanisms of Li–O2 batteries using environmental transmission electron microscopy
    journal, March 2017

    • Luo, Langli; Liu, Bin; Song, Shidong
    • Nature Nanotechnology, Vol. 12, Issue 6
    • DOI: 10.1038/nnano.2017.27

    Bridging the academic and industrial metrics for next-generation practical batteries
    journal, February 2019

    A flexible polymer-based Li–air battery using a reduced graphene oxide/Li composite anode
    journal, January 2018

    • Guo, Ziyang; Li, Jinli; Xia, Yuan
    • Journal of Materials Chemistry A, Vol. 6, Issue 14
    • DOI: 10.1039/c8ta01117f

    Lithium–oxygen batteries with triplex Li + -selective solid membranes
    journal, January 2019

    • Choi, Youngbin; Jung, Keeyoung; Kim, Hyeong-Jun
    • Chemical Communications, Vol. 55, Issue 53
    • DOI: 10.1039/c9cc03652k

    Polysulfide-driven low charge overpotential for aprotic lithium–oxygen batteries
    journal, January 2019

    • Zhou, Yin; Lyu, Zhiyang; Liu, Zhenjie
    • Journal of Materials Chemistry A, Vol. 7, Issue 15
    • DOI: 10.1039/c9ta00267g

    Design strategies toward catalytic materials and cathode structures for emerging Li–CO 2 batteries
    journal, January 2019

    • Hu, Anjun; Shu, Chaozhu; Xu, Chenxi
    • Journal of Materials Chemistry A, Vol. 7, Issue 38
    • DOI: 10.1039/c9ta06506g

    Spinel NiCo 2 S 4 as Excellent Bi-Functional Cathode Catalysts for Rechargeable Li-O 2 Batteries
    journal, January 2019

    • Xu, Mengting; Hou, Xiaoyan; Yu, Xuebin
    • Journal of The Electrochemical Society, Vol. 166, Issue 6
    • DOI: 10.1149/2.1151906jes

    Catalysts in metal–air batteries
    journal, April 2018

    Recent Progress on Catalysts for the Positive Electrode of Aprotic Lithium-Oxygen Batteries †
    journal, May 2019

    Advances in Manganese-Based Oxides Cathodic Electrocatalysts for Li-Air Batteries
    journal, February 2018

    • Liu, Bao; Sun, Yinglun; Liu, Li
    • Advanced Functional Materials, Vol. 28, Issue 15
    • DOI: 10.1002/adfm.201704973

    Drawing a Pencil-Trace Cathode for a High-Performance Polymer-Based Li-CO 2 Battery with Redox Mediator
    journal, January 2019

    • Li, Jinli; Zhao, Huimin; Qi, Haocheng
    • Advanced Functional Materials, Vol. 29, Issue 11
    • DOI: 10.1002/adfm.201806863

    Research Progress towards Understanding the Unique Interfaces between Concentrated Electrolytes and Electrodes for Energy Storage Applications
    journal, March 2017

    • Zheng, Jianming; Lochala, Joshua A.; Kwok, Alexander
    • Advanced Science, Vol. 4, Issue 8
    • DOI: 10.1002/advs.201700032

    Structure Design and Composition Engineering of Carbon‐Based Nanomaterials for Lithium Energy Storage
    journal, March 2020

    • Geng, Hongya; Peng, Yan; Qu, Liangti
    • Advanced Energy Materials, Vol. 10, Issue 10
    • DOI: 10.1002/aenm.201903030

    A Long-Life Lithium-Air Battery in Ambient Air with a Polymer Electrolyte Containing a Redox Mediator
    journal, May 2017

    Simultaneous Stabilization of Potassium Metal and Superoxide in K-O 2 Batteries on the Basis of Electrolyte Reactivity
    journal, June 2018

    Energy and fuels from electrochemical interfaces
    journal, December 2016

    • Stamenkovic, Vojislav R.; Strmcnik, Dusan; Lopes, Pietro P.
    • Nature Materials, Vol. 16, Issue 1
    • DOI: 10.1038/nmat4738

    Sustainability and in situ monitoring in battery development
    journal, December 2016

    • Grey, C. P.; Tarascon, J. M.
    • Nature Materials, Vol. 16, Issue 1
    • DOI: 10.1038/nmat4777

    A high-rate and long-life organic–oxygen battery
    journal, February 2019

    Stable, yet “naked”, azo radical anion ArNNAr − and dianion ArNNAr 2− (Ar = 4-CN-2,6- i Pr 2 -C 6 H 2 ) with selective CO 2 activation
    journal, January 2020

    • Wang, Wenqing; Tan, Gengwen; Feng, Rui
    • Chemical Communications, Vol. 56, Issue 22
    • DOI: 10.1039/c9cc07382e

    A Hybrid Na//K + -Containing Electrolyte//O 2 Battery with High Rechargeability and Cycle Stability
    journal, January 2019

    A Review of Model-Based Design Tools for Metal-Air Batteries
    journal, January 2018

    Understanding the Reaction Chemistry during Charging in Aprotic Lithium–Oxygen Batteries: Existing Problems and Solutions
    journal, February 2019

    • Shu, Chaozhu; Wang, Jiazhao; Long, Jianping
    • Advanced Materials, Vol. 31, Issue 15
    • DOI: 10.1002/adma.201804587

    Recent Advances in Non-Aqueous Electrolyte for Rechargeable Li-O 2 Batteries
    journal, June 2016

    • Li, Yang; Wang, Xiaogang; Dong, Shanmu
    • Advanced Energy Materials, Vol. 6, Issue 18
    • DOI: 10.1002/aenm.201600751

    Phenol-Catalyzed Discharge in the Aprotic Lithium-Oxygen Battery
    journal, May 2017

    • Gao, Xiangwen; Jovanov, Zarko P.; Chen, Yuhui
    • Angewandte Chemie, Vol. 129, Issue 23
    • DOI: 10.1002/ange.201702432

    High‐Performance K–CO 2 Batteries Based on Metal‐Free Carbon Electrocatalysts
    journal, January 2020

    • Zhang, Wenchao; Hu, Chuangang; Guo, Zaiping
    • Angewandte Chemie, Vol. 132, Issue 9
    • DOI: 10.1002/ange.201913687

    Hydronium-Ion Batteries with Perylenetetracarboxylic Dianhydride Crystals as an Electrode
    journal, February 2017

    • Wang, Xingfeng; Bommier, Clement; Jian, Zelang
    • Angewandte Chemie International Edition, Vol. 56, Issue 11
    • DOI: 10.1002/anie.201700148

    How to Control the Discharge Product in Sodium-Oxygen Batteries: Proposing New Pathways for Sodium Peroxide Formation
    journal, February 2017

    • Schröder, Daniel; Bender, Conrad L.; Pinedo, Ricardo
    • Energy Technology, Vol. 5, Issue 8
    • DOI: 10.1002/ente.201600539

    Key Aspects of Lithium Metal Anodes for Lithium Metal Batteries
    journal, March 2019

    High-Performance Anode Materials for Rechargeable Lithium-Ion Batteries
    journal, March 2018

    Highly dispersed metal and oxide nanoparticles on ultra-polar carbon as efficient cathode materials for Li–O 2 batteries
    journal, January 2017

    • Lu, Xueyi; Hao, Guang-Ping; Sun, Xiaolei
    • Journal of Materials Chemistry A, Vol. 5, Issue 13
    • DOI: 10.1039/c7ta00777a

    Multistaged discharge constructing heterostructure with enhanced solid-solution behavior for long-life lithium-oxygen batteries
    journal, December 2019

    Understanding LiOH Chemistry in a Ruthenium-Catalyzed Li-O2 Battery.
    text, January 2017

    • Liu, Tao; Liu, Zigeng; Kim, Gunwoo
    • Apollo - University of Cambridge Repository
    • DOI: 10.17863/cam.18109

    Why Do Lithium-Oxygen Batteries Fail: Parasitic Chemical Reactions and Their Synergistic Effect
    journal, July 2016

    • Yao, Xiahui; Dong, Qi; Cheng, Qingmei
    • Angewandte Chemie International Edition, Vol. 55, Issue 38
    • DOI: 10.1002/anie.201601783

    Understanding LiOH Chemistry in a Ruthenium-Catalyzed Li-O 2 Battery
    journal, November 2017

    • Liu, Tao; Liu, Zigeng; Kim, Gunwoo
    • Angewandte Chemie International Edition, Vol. 56, Issue 50
    • DOI: 10.1002/anie.201709886

    High-Purity Lithium Metal Films from Aqueous Mineral Solutions
    journal, January 2018

    Heme biomolecule as redox mediator and oxygen shuttle for efficient charging of lithium-oxygen batteries
    journal, October 2016

    • Ryu, Won-Hee; Gittleson, Forrest S.; Thomsen, Julianne M.
    • Nature Communications, Vol. 7, Issue 1
    • DOI: 10.1038/ncomms12925

    Organic hydrogen peroxide-driven low charge potentials for high-performance lithium-oxygen batteries with carbon cathodes
    journal, June 2017

    • Wu, Shichao; Qiao, Yu; Yang, Sixie
    • Nature Communications, Vol. 8, Issue 1
    • DOI: 10.1038/ncomms15607

    Multistaged discharge constructing heterostructure with enhanced solid-solution behavior for long-life lithium-oxygen batteries
    journal, December 2019

    Quasi–solid state rechargeable Na-CO 2 batteries with reduced graphene oxide Na anodes
    journal, February 2017

    A Hybrid Na//K + -Containing Electrolyte//O 2 Battery with High Rechargeability and Cycle Stability
    journal, January 2019

    Building Better Batteries in the Solid State: A Review
    journal, November 2019

    • Mauger, Alain; Julien, Christian M.; Paolella, Andrea
    • Materials, Vol. 12, Issue 23, p. 3892
    • DOI: 10.3390/ma12233892
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