A passivation-free solid electrolyte interface

regulated by magnesium bromide additive for

highly reversible magnesium batteries

Deviprasath Chinnadurai, a Wei Ying Lieu, a,b Sonal Kumar, a Gaoliang Yang, a Yuanjian Li a,

Zhi Wei Seh* a

a
Institute of Materials Research and Engineering, Agency for Science, Technology and

Research (A*STAR), 2 Fusionopolis Way, Innovis, Singapore 138634, Singapore.

b
Pillar of Engineering Product Development, Singapore University of Technology and

Design, 8 Somapah Road, Singapore 487372, Singapore.

*Email: sehzw@imre.a-star.edu.sg

KEYWORDS: Magnesium batteries, Magnesium halides, High reversibility, Solid electrolyte

interface, Magnesium bromide

Experimental Methods
Electrolyte fabrication

Magnesium bis(hexamethyldisilazide) (Mg(HMDS)2, 97%), tetrabutylammonium

borohydride (TBABH4, 97%), and 1,2-dimethoxyethane (DME, 99% and anhydrous) were

acquired from Sigma Aldrich. Magnesium bis(trifluoromethanesulfonimide) (Mg(TFSI)2,

99.5%) and magnesium triflate (Mg(OTf)2, 99.5%) were purchased from Solvionic. Prior to

electrolyte fabrication, the solvents were dehydrated with molecular sieves (pore size 0.3 nm,

size 4-8 mesh) for at least 12 hours. Each electrolyte was made by mixing the predetermined

amount of Mg(HMDS)2 and TBABH4 and MgX2 (X=Cl, I, F, Br) in a glass vial, followed by

addition of the solvent, and the solution was stirred at an elevated temperature of 50°C for at

least 12 hours at a stirring speed of 400 rpm before being used.

Material characterization

The morphology of Mg deposits was characterized by JEOL 6700F scanning electron

microscopy (SEM). The elemental analysis and chemical composition of samples were

characterized by X-ray diffraction (Bruker, with Cu-Kα radiation of 1.5418 Å), X-ray

photoelectron spectroscopy (Thermo Fisher Scientific, with Al Kα radiation of 1486.6 eV),

and time-of-flight secondary ion mass spectrometry (IONTOF GmbH, Germany

measurements).

Electrochemical characterization

Coin cells used in this work were fabricated in an Ar-filled glovebox with an O2 content of

≤1.7 ppm and H2O content of ≤0.1 ppm. Glass fibre separators (by WhatmanTM, GF/D) were

used in all the coin cell-based characterization. Before being used, the glass fiber separator

was dried in a 150 °C oven for 4 hours. Coulombic efficiency of the magnesium plating and

stripping process were estimated by conducting galvanostatic cycling in a two-electrode

asymmetric half-cell (coin cell 2032). A polished magnesium metal anode (⌀12.7 mm, by

Hefei Kejing Materials Technology Co. LTD) was used as the counter electrode while a

vacuum-dried carbon-coated aluminium foil was used as the working electrode (⌀11.28 mm,

by MTI), with glass fiber separator soaked with 80 μL of electrolyte. The Coulombic

efficiency (CE) of the cell was calculated by dividing the magnesium dissolution capacity by

the magnesium deposition capacity. To accurately establish the magnesium anode plating and

stripping overpotential and cycling properties of each electrolyte, galvanostatic cycling was

conducted using a 2-electrode symmetrical Mg||Mg cell in a coin cell configuration.

Cyclic voltammetry (CV), linear sweep voltammetry (LSV), multistep chronoamperometry

(CA), electrochemical impedance spectroscopy (EIS) were performed on a Gamry Reference

600+ Potentiostat. CV, LSV and CA measurements were conducted in a three-electrode cell

with Mg as reference and counter electrode and different metals as the working electrode.

EIS measurements were carried out in a coin cell, the Nyquist plots were measured between

frequency of 100 kHz and 0.1 Hz with a sinusoidal voltage of 5 mV amplitude. For the full

cell, the Mo6S8 materials were prepared as previously,1 mixed with Super P carbon and

polyvinylidene difluoride (PVDF) binder in a mass ratio of 8: 1: 1 in N-methyl-2-pyrrolidone

(NMP) solvent. The homogenous slurry was then coated on Ni foil and dried in the vacuum

oven at 60 ℃ for 12 h. The electrodes were punched into 12-mm-diameter disks before use,

and the areal mass loading of Mo6S8 is around 1.32 mg/cm2. The C rate was calculated based

on the theoretical capacity of Mo6S8 at 129 mAh/g (1 C = 129 mA/g). The CE of

Mg//MgMo6S8 cell for each cycle was calculated based on the ratio of discharge capacity to

charge capacity.
Figure S1. The initial plating curves of Mg//Al cell in each halide electrolyte system with
calculated nucleation and plating overpotential.
Figure S2. Nyquist plots measured at different temperature in 0.1 M Mg(HMDS)2 + 30 mM
TBABH4 (a) + 20 mM MgCl2 (b) + 20 mM MgI2 (c) + 20 mM MgF2 (d) +20 mM MgBr2 (e-f)
Arrhenius plots of Rint and Rct with measured activation energy at interface.

Figure S3. Galvanostatic cycling performance of Mg//Al symmetric cells at 0.5 mA/cm2 and
0.5 mAh/cm2 in a 0.1 M Mg(HMDS)2 + 30 mM TBABH4 in DME + 20 mM of MgBr2.
Figure S4. (a-b) Voltage profile of Mg//Al cells cycled at different current rates at a fixed
areal capacity of 0.5 mAh/cm2 in 0.1 M Mg(HMDS)2 + 30 mM TBABH4 + 20 mM MgBr2 (c)
columbic efficiency vs cycle number.
Figure S5. (a-b) Voltage profile of Mg//Al cells cycled at different areal capacities at a fixed
current of 0.5 mA/cm2 in 0.1 M Mg(HMDS)2 + 30 mM TBABH4 + 20 mM MgBr2; (c)
columbic efficiency vs cycle number.

Figure S6. (a-b) Voltage profile of Mg//Mg cells cycled at different current density at 0.5
mAh/cm2 in 0.1 M Mg(HMDS)2 + 30 mM TBABH4 + 20 mM MgBr2; (c-d) voltage profile of
Mg//Al cells cycled at different areal capacities at a fixed current of 0.5 mA/cm2.

Figure S7. (a) LSV curves at 5 mV/s in 0.1 Mg(HMDS)2 + 30 mM TBABH4 + 20 mM

MgBr2/20 mM MgCl2 with SS and Pt as working electrode; (b) chronoamperometry at
different potentials with Pt as working electrode.
Figure S8. The deconvoluted surface XPS spectra of (a) O 1s, (b) Si 2p (c) B 1s and, (d) N

1s, in 0.1 M Mg(HMDS)2 + 30 mM TBABH4 + 20 mM MgX2 (X-Cl, I, F, Br)

Figure S9. (a) SEM images of Mg deposits at a current density of 0.5 mA/cm2 and areal
capacity of 0.5 mAh/cm2 on Al and Mg anode. (b) low, and high magnification with cross
section image of Mg deposits on Al cathode after 3 cycles. (c) XRD pattern of Mg deposits
on a Al/C cathode at 3 mAh/cm2 and 0.5 mAh/cm2.
Figure S10. SEM images of Mg coated on an Al-C cathode at different currents at 1
mAh/cm2 in 0.1 M Mg(HMDS)2 + 30 mM TBABH4 + 20 mM MgBr2.

Figure S11. SEM images of Mg coated on an Mg anode at different currents at 1 mAh/cm2 in

0.1 M Mg(HMDS)2 + 30 mM TBABH4 + 20 mM MgBr2
 • Al

(101)
(002)
(100)
MgBr2

# # # # Mg

MgF2
Intensity (a.u)

MgI2

• MgCI2
•

30 33 36 39 42 45
2 Theta (deg)

Figure S12. XRD pattern of Mg deposits at 0.5 mA cm2, 0.5 mAh/cm2, in 0.1 M
Mg(HMDS)2 + 30 mM TBABH4 + 20 mM MgX2 (X-Cl, I, F, Br).

Figure S13. XPS depth profiling analysis of Mg anode from a Mg//Mg cell in plated state in
0.1 M Mg(HMDS)2 + 30 mM TBABH4 + 20 mM MgBr2 after 20 cycles: (a) O 1s; (b) Si 2p;
(c) N 1s.
Figure S14. (a) First cycle voltage profile of Mg//Al cells at varied Mg(HMDS)2 in 30 mM
TBABH4 and 20 mM MgBr2; (b) columbic efficiency vs cycle number curves.

Figure S15. Voltage profiles of Mg//Al cells in 0.1 M Mg(HMDS)2 + 30 mM TBABH4 +100
mM MgBr2.
Figure S16. (a) voltage profiles measured at different current density at 1 mAh/cm2; (b)
coulombic efficiency vs cycle number curves at different currents; (c) cycling data and
voltage profile measured at different areal capacity at 0.5 mA/cm2; (d) coulombic efficiency
curves at different areal capacities at 0.5 mA/cm2 of Mg//Al cells in 0.1 M Mg(HMDS)2 + 30
mM TBABH4 + 50 mM MgBr2.
Figure S17. (a) Voltage profiles of Mg//Al cells in 0.1 M Mg(HMDS)2 + 30 mM TBABH4 +
50 mM MgBr2 measured at an applied current of 1 mA/cm2 at 0.1 mAh/cm2; (b) at 1
mAh/cm2; (c) at 3 mAh/cm2; (d) at 12 mAh/cm2; (e) Coulombic efficiency vs cycle number
Figure S18. Voltage profiles of Mg//Mg cells in 0.1 M Mg(HMDS)2 + 30 mM TBABH4 + 50
mM MgBr2 measured at 1 mA/cm2 for: (a) 0.1 mAh/cm2; (b) 1 mAh/cm2

Figure S19. (a-b) cycling data and voltage profiles measured of Mg//Mg cells at different
current density at 1 mAh/cm2; (c) cycling voltage measured at different areal capacity at 0.5
mA/cm2 of Mg//Mg cells in 0.1 M Mg(HMDS)2 + 30 mM TBABH4 + 50 mM MgBr2
Figure S20. (a-c) Cyclic voltammetry in a three-electrode cell at 5 mV/s with Pt, SS, and Mo
metals as working electrode; (d-f) chronoamperometry measured at different potential with
Pt, SS and Mo strips as working electrodes in 0.1 M Mg(HMDS)2 + 30 mM TBABH4 + 50
mM MgBr2.

Figure S21. (a) Cyclic voltammetry in a three-electrode cell at 5 mV/s with Al metal as
working electrode; (b) LSV; (c) chronoamperometry measured at different potential in 0.1 M
Mg(HMDS)2 + 30 mM TBABH4 + 50 mM MgBr2.
Figure S22. (a) First cycle voltage profile of Mg//Al in 30 mM TBABH4 and 20 mM MgBr2
+30 mM TBABH4 with presence of different Mg salts; b) coulombic efficiency vs cycle
number curves.

Table S1. Calculated parameters from EIS fitting curves measured at different temperatures.

Electrolyte
0.1 M Temperature °C Rb (Ω) RSEI (Ω) Rct (Ω) Rint (Ω)
Mg(HMDS)2 +
30 mM TBABH4
+MgCl2 25.8 44.89 219129 1.747E6 1.96613E6
30 41.8 152346 1.386E6 1.53835E6
40 37.68 21566 826353 847919
50 36.28 12791 494435 507226
60 33.16 2995 325364 328359
70 32.65 1315 170617 171932

+Mgl2 25.8 187.2 16915 972673 989588

30 179.5 486.6 1.139E6 1.13949E6
40 169.3 124.3 828181 828305.3
50 153.5 206.7 443245 443451.7
60 155.8 861.8 342850 343711.8
70 156.5 228.5 207382 207610.5

+MgF2 25.8 37.15 88780 1.517E6 1.60578E6

30 35.49 76468 1.48E6 1.55647E6
40 33.35 49765 1.093E6 1.14277E6
50 32.78 61132 878882 940014
60 32.73 62605 674274 736879
70 44.72 74793 467748 542541

+MgBr2 25.8 28.47 110881 782250 893131

30 27.81 108548 727319 835867
40 26.27 80819 528421 609240
50 25.51 69864 391103 460967
60 24.87 59446 290939 350385
70 24.08 65510 139294 204804
Table S2. Summary of ionic conductivity and electrochemical performance of 0.1 M
Mg(HMDS)2 + 30 mM TBABH4 + 20 mM MgX2 (X- Cl, I, F, Br).

Electrolyte Ionic Initial plating Average CE Cycle life Nucleation

conductivity overpotential overpotential
(mS/cm)
Mg//Al (V) Mg//Al (%) Mg//Al Mg//Mg (V)

MgCl2 0.28 0.22 98.9 226 415 0.71

Mgl2 0.05 0.60 97.12 59 20 0.70

MgF2 0.29 0.68 82.88 5 310 0.54

MgBr2 0.46 0.43 99.0 274 460 0.39

Table S3. Electrochemical performance of Mg//Al cells in 0.1 M Mg(HMDS)2 + 30 mM

TBABH4 in DME at different molarity of MgBr2 measured at 0.5 mA/cm2 and 0.5 mAh/cm2.

MgBr2 concentration Initial plating/stripping Initial CE (%) Average CE (%) Cycle

overpotential (V)
10 mM 0.89 84.96 98.90 175
20 mM 0.81 89.43 99.00 274
50 mM 0.54 95.52 99.10 575
100 mM 0.64 95.56 99.26 1028

Table S4. Comparative table of Mg//Mg half-cell performance from previous studies with
our work.

Electrolyte Current Areal capacity Time Cycle Maximum Reference

density (mAh/cm2) (h) current
(mA/cm2) density
(mA/cm2)
2
OMBB/DME 0.1 0.05 700 700 1
3
MgTFSI2+MgCl2 1.0 1.0 300 150 5
+rPDI/DME
4
MgCl2+AlCl3 /THF-IL 0.05 0.0125 50 100 0.5
5
Mg(HMDS)2 0.5 0.125 130 260 5
+AlCl3/DG

6
MgBhfip /DME 0.1 0.05 1200 1200 1
7
Mg-FPB/DG 0.1 - 500 1
8
MgCl2+YCl3 /DG-IL 0.5 1 500 125 -
9
MgCl2+AlCl3+ LiCl/THF- 0.5 0.5 500 250 0.5
IL
10
MgTFSI2 +GeCl4/DME 0.02 0.005 1000 2000 10
11
MgCl2+AlCl3+ MgTFSI2 0.2 0.05 90 180 2
/THF
12
MgTFSI2 /DME-IL 0.1 0.025 90 180 3
13
Mg(CF3SO3)2 0.05 0.05 200 100 2
+MgCl2+AlCl3 /DME
14
Mg(HMDS)Br /THF 0.6 0.3 1000 1000 3
15
MgFPA/THF 1 0.5 1200 1200 -
1
Mg(OTf)2+MgCl2/DME 0.5 0.5 500 250 3
16
MAT/TG 0.1 0.05 1000 1000 0.5
17
MACT/DME 0.025 0.0125 2000 2000 2.5
18
MgBhfip+Bi (OTf)3/DME 1.0 0.5 500 500 -
19
Mg(OTf)2+ TBAC/DME 0.5 0.5 600 300 3.0
0.1 M Mg(HMDS)2 + 30 0.5 0.5 2000 1000 4 This
mM TBABH4+50 mM 1.0 1.0 1076 583 work
MgBr2

Table S5. Comparative table of Mg-asymmetric half-cell performance in previous studies

with our work.

Electrolyte Current Areal Time Cycle Coulombic Maximum Reference

density capacity (h) number efficiency current
(mA/cm2) (mAh/cm2) (%) density
(mA/cm2)
20
MBA-B(Otfe)3 0.5 0.5 200 100 98 1.0
in THF
21
Li[B(hfip)4] 0.5 0.25 500 500 99 -
in DME
22
MBA-2MgCl2 0.088 0.044 100 100 98 -
in THF
3
0.25 M 1 1 200 100 94
Mg(TFSI)2 + 2
M MgCl2+rPDI
in DME
23
APC 0.5 0.5 100 50 88 -

24
[Mg(THF)6] 0.5 0.25 120 120 99 -
[AlCl4]2-THF-
PYR14TFSI+MgF2
25
Mg(HMDS)2 + 0.5 0.5 300 150 98.3 1.5
TBABH4
26
Mg(HMDS)2 + 0.5 0.5 552 226 98.9 -
TBABH4 + MgCl2
19
0.5 0.5 400 200 97.7 4
Mg(OTf)2+ TBAC
1
Mg(OTf)2 + 0.5 0.5 200 100 99.1 3
MgCl2
0.1 M 0.5 0.5 1146 575 99.10 4 This
Mg(HMDS)2 + 30 1.0 0.1 399 2000 99.38 work
mM TBABH4+50 1.0 1 324 162 99.21
mM MgBr2 1.0 3 268 44 98.93
1.0 12 72 3 98.32
0.1 M 0.5 0.5 2046 1028 99.26 This
Mg(HMDS)2 + 30 work
mM TBABH4+100
mM MgBr2
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