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A multifunctional additive improves the electrolyte properties of magnesium borohydride towards magnesium-sulfur batteries Huimin Xu, Zhonghua Zhang, Jiajia Li, Lixin Qiao, Chenglong Lu, Kun Tang, Shanmu Dong, Jun Ma, Yongjun Liu, Xinhong Zhou, and Guanglei Cui ACS Appl. Mater. Interfaces, Just Accepted Manuscript • Publication Date (Web): 27 Jun 2018 Downloaded from http://pubs.acs.org on June 27, 2018

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ACS Applied Materials & Interfaces

A multifunctional additive improves the electrolyte properties of magnesium borohydride towards magnesium-sulfur batteries

Huimin Xu,a,b,† Zhonghua Zhang,d,† Jiajia Li,c Lixin Qiao,a Chenglong Lu,a Kun Tang,a Shanmu Dong,b Jun Ma,b Yongjun Liu,a,* Xinhong Zhou,a,* and Guanglei Cuib,*

a

College of Chemistry and Molecular Engineering, Qingdao University of Science and Technology,

Qingdao, 266042, P. R. China. b

Qingdao Industrial Energy Storage Research Institute, Qingdao Institute of Bioenergy and

Bioprocess Technology, Chinese Academy of Sciences, Qingdao, 266101, P. R. China. c

Institute of Materials Science and Engineering, Ocean University of China, Songling Road 238,

Qingdao 266100, Shandong Province, PR. China. d

College of Materials Science and Engineering, Qingdao University of Science and Technology,

Qingdao 266042, China. †

H. Xu and Z. Zhang contributed equally to this work.

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ABSTRACT: Highly reductive magnesium borohydride (Mg(BH4)2) is compatible with metallic Mg, making it a promising Mg-ion electrolyte for rechargeable Mg batteries. However, pure Mg(BH4)2 in ether-based solutions displays very limited solubility (0.01 M), low oxidative stability ( 99%). Owing to the newly-generated active cation and anion species revealed by Raman, NMR and MS spectra, the electrochemical potential window is increased from 1.8 V to 2.8 V vs. Mg on stainless steel electrode, rendering electrolytes the ability to examine high voltage cathodes. More importantly, on account of the non-nucleophilicity of active electrolyte species, we present the first example of magnesium-sulfur (Mg-S) batteries using Mg(BH4)2-based electrolytes, which exhibit a high discharge capacity of 955.9 mAh g−1 and 526.5 mAh g−1 at the initial and 30th charge/discharge cycles, respectively. These achievements not only provide an efficient and specific strategy to eliminate the major roadblocks facing Mg(BH4)2-based electrolytes, but also highlight the profound effect of functional additives on the electrochemical performances of unsatisfied Mg-ion electrolytes. KEYWORDS: Energy storage, Magnesium-sulfur battery, Electrolyte, Magnesium borohydride,


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Functional additive 1. INTRODUCTION Rechargeable magnesium (Mg) batteries have been regarded as one of the promising candidates to power the future electric vehicles and support the large-scale energy storage systems owing to the high theoretical volumetric capacity (3832 mAh cm−3 for Mg metal anode vs. 2062 mAh cm−3 for Li metal anode), low cost and large natural abundance of Mg.1-4 Mg batteries might also raise less safety concerns because the electrochemical deposition of Mg does not involve the formation of either thick solid electrolyte interface (SEI) layers or metallic dendrites.5-8 However, the commercialization of such promising batteries has not yet been realized due to the unsatisfied properties of Mg-ion electrolytes, including the poor compatibility with cathode materials, insufficient electrochemical window and undesired Mg plating/stripping properties.9-15 Extensive investigations demonstrate that the chemical reaction between Mg metal and simple anions (e.g. ClO4−, BF4−) forms insoluble Mg salts which can completely passivate the metallic Mg anode.16 The highly reductive environments exploited by Mg metal narrow down the choices of Mg salts in Mg-ion electrolytes. Magnesium organohaloaluminate electrolytes derived from the high reductive Grignard solutions, demonstrated by Prof. Gregory and Prof. Aurbach and their co-workers, may represent the most promising Mg-ion electrolytes in terms of the high Coulombic efficiencies and low over-potential during Mg plating/stripping processes.1, 17 However, most of magnesium organohaloaluminate electrolytes severely corrode non-inert current collectors and are not compatible with high capacity electrophilic cathode materials.18-20 Exploring efficient Mg-ion electrolytes with excellent overall performances in terms of widened electrochemical window, fair ionic conductivity, high Mg plating/stripping Coulombic efficiency, excellent compatibility with



the electrode materials, and non-corrosivity towards non-inert current collectors is still a big challenge at this early stage. Another strong reducing agent, magnesium borohydride (Mg(BH4)2), has also been proved to be compatible with Mg anode by Mohtadi et al., who open the door for designing Mg(BH4)2-based electrolytes for Mg batteries.21 It should be pointed out that the development of high performance Mg(BH4)2-based electrolytes faces formidable challenges: 1) The saturated concentration of Mg(BH4)2 in most ether-based solvents is very low (about 0.01 M), resulting in limited ionic conductivity of Mg(BH4)2-based electrolytes (commonly less than 0.1 mS cm−1); 2) Mg(BH4)2 electrolytes exhibit very low anodic stability (less than 1.8 V vs. Mg on stainless steel), which precludes the examination of high voltage cathode materials; 3) The pure Mg(BH4)2 electrolyte shows very limited Mg plating/stripping Coulombic efficiency (15%~40%) mainly due to the insufficient dissociation of Mg2+ and BH4− in ether-based solvents.22-25 In consideration of these drawbacks, it is unlikely to utilize pure Mg(BH4)2 salts in designing a high-performance Mg-ion electrolyte. Manipulating the solvation structure of electrolytes (including the degree of salt dissociation, the type of solvents, and so on) by introducing functional additives or another active Mg salts may represent an effective strategy to improve the electrochemical properties of Mg(BH4)2-based electrolytes. Mohtadi et al. have reported that the choice of solvents and the addition of LiBH4 have a profound effect on the electrochemical performances of Mg(BH4)2-based electrolytes, such as the Mg plating/stripping Coulombic efficiency, response current density, and overpotentials.21 These facts have also been demonstrated by Shao et al..24 The drastic performance improvement has been ascribed to much greater dissociation degree of Mg2+ and BH4− caused by the stronger chelating


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properties of dimethoxyethane (DME). One of the most frequently-used Mg(BH4)2-based electrolyte has been constructed, which consists of 0.1 M Mg(BH4)2 and 1.5 M LiBH4 in DGM (designated as Mg(BH4)2/LiBH4 electrolyte). The Mg(BH4)2/LiBH4 electrolyte displays a high Coulombic efficiency (~100%), fair electrochemical voltage window (~ 1.8 V vs. Mg), reasonable ionic conductivity of 3.27 mS cm−1, and a relatively high response Mg stripping peak current density of ~12.0 mA cm−2. In order to achieve better Mg plating/stripping properties, NuLi et al. have prepared the Mg(BH4)2/LiBH4 in tetraglyme (TG) solvent via 90 °C heating treatment, which displayed a higher Mg(BH4)2 solubility up to 0.5 M and widened electrochemical potential window (2.4 V vs. Mg on stainless steel).26 NuLi et al. also introduced PP14TFSI ionic liquid into Mg(BH4)2/LiBH4 in TG/DME solvents, which displayed a wide electrochemical window up to 3.0 V vs. Mg.27 Despite these achievements, the Mg(BH4)2/LiBH4 electrolyte still suffers from limited anodic stability and low Mg(BH4)2 solubility in conventional ether solvent. In addition, the Mg(BH4)2/LiBH4 electrolyte makes the cathode reaction more complex, which might involve Li-ion intercalation to a great extent.28-30 The energy density of the so called “dual ion battery” or “hybrid Mg2+/Li+ battery” largely depends on the cell voltage and concentration of Li-ions in electrolytes. These aspects make Mg(BH4)2/LiBH4 electrolyte unsuitable for any practical application towards high energy density Mg batteries. To achieve high Mg(BH4)2 dissociation in DME, the strong ionic bonding between Mg2+ and BH4− should be broken. Recently, Watkins et al. have demonstrated that high degree of BH4− dissociation from Mg(BH4)2 can be accomplished by designing chelating ionic liquids.31 Persson et al. have also tuned the solvation structure by simply mixing two competing Mg salts, namely, the Mg(BH4)2 and Mg(TFSI)2.32 However, these electrolytes involve TFSI− anions which may be



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decomposed and passivate Mg anodes due to the vulnerability of [MgTFSI]+ ion pairs in highly reductive conditions.33

In addition, these Mg(BH4)2-based electrolytes display very limited

solubility of Mg(BH4)2 (0.01 M), leading to insufficient Coulombic efficiency ( 99%). Owing to the newly-generated active species, the 0.5 M Mg(BH4)2/THFPB-DGM electrolyte exhibits a wide electrochemical potential window up to 2.8 V vs. Mg on SS electrode. More importantly, the non-nucleophilicity of the 0.5 M Mg(BH4)2/THFPB-DGM electrolyte makes it possible to construct Mg-S batteries using Mg(BH4)2-based electrolytes. The as-fabricated Mg-S cells display discharge voltage plateau of 1.4 V vs. Mg, high specific capacity of 955.9 mAh g−1, as well as reasonable capacity retention of ≈55.1% after 30 cycles. Our work not only offers a specific and highly efficient avenue to achieve high performance Mg(BH4)2-based electrolytes, but also highlights the fact that functional additives could make a big difference for any unsatisfactory Mg salts electrolyte solutions. These achievements could provide useful knowledge on the future exploration of high performance battery electrolytes and high energy density Mg-S battery materials. ASSOCIATION CONTENT Supporting Information


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CV curves of different electrolytes, galvanostatic cycling of symmetrical cell Mg||0.5 M Mg(BH4)2/1.0 M THFPB-DGM||Mg, Nyquist plots, LSV, 1H NMR spectra and MS spectra of fresh and cycled electrolytes, SEM image and EDS spectrum of Mg anode after 20 cycles. AUTHOR INFORMATION Corresponding Author *E-mail: [email protected]. *E-mail: [email protected]. *E-mail: [email protected]. ORCID Guanglei Cui: 0000-0002-8008-7673 Author Contributions All authors have given approval to the final version of the manuscript. Notes The authors declare no competing financial interest.

ACKNOWLEDGEMENTS This work was supported by the National Natural Science Foundation for Distinguished Young Scholars of China (Grant No. 51625204), the funding from the Youth Innovation Promotion Association of CAS (Grant No. 2016193) and the National Natural Science Foundation of China (Grant No. 51502319). The authors thank the Qingdao Key Lab of Solar Energy Utilization and Energy Storage Technology. REFERENCES (1) Aurbach, D.; Lu, Z.; Schechter, A.; Gofer, Y.; Gizbar, H.; Turgeman, R.; Cohen, Y.; Moshkovich, M.; Levi, E. Prototype Systems for Rechargeable Magnesium Batteries. Nature 2000,



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Multifunctional Additives Improve the Electrolyte Properties of

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