Bismuth ion battery – A new member in trivalent battery technology

Journal Pre-proof Bismuth Ion Battery – A New Member in Trivalent Battery Technology Ting Xiong, Wee Siang Vincent Lee, Yonghua Du, Juezhi Yu, Shibo Xi, Haijun Wu, Stephen John Pennycook, Ping Yang, Junmin Xue PII:

S2405-8297(19)31022-0

DOI:

https://doi.org/10.1016/j.ensm.2019.10.026

Reference:

ENSM 969

To appear in:

Energy Storage Materials

Received Date: 31 July 2019 Revised Date:

23 October 2019

Accepted Date: 23 October 2019

Please cite this article as: T. Xiong, W.S. Vincent Lee, Y. Du, J. Yu, S. Xi, H. Wu, S.J. Pennycook, P. Yang, J. Xue, Bismuth Ion Battery – A New Member in Trivalent Battery Technology, Energy Storage Materials, https://doi.org/10.1016/j.ensm.2019.10.026. This is a PDF file of an article that has undergone enhancements after acceptance, such as the addition of a cover page and metadata, and formatting for readability, but it is not yet the definitive version of record. This version will undergo additional copyediting, typesetting and review before it is published in its final form, but we are providing this version to give early visibility of the article. Please note that, during the production process, errors may be discovered which could affect the content, and all legal disclaimers that apply to the journal pertain. © 2019 Elsevier B.V. All rights reserved.

Bismuth Ion Battery – A New Member in Trivalent Battery Technology Ting Xionga,b, Wee Siang Vincent Lee*a, Yonghua Duc, Juezhi Yua, Shibo Xic, Haijun Wua, Stephen John Pennycooka, Ping Yangc, Junmin Xue*a a

National University of Singapore, Department of Materials Science and Engineering,

Singapore 117573. b

Centre for Advanced 2D Materials and Graphene Research Centre, National University of

Singapore, Singapore 117546. c

Institute of Chemical and Engineering Sciences, Agency for Science, Technology and

Research, Singapore, 627833.

Abstract: To provide alternative battery technologies to lithium ion battery, multivalent metal ion batteries with their high theoretical capacities and ease of preparation have gradually gained attention from both academia and industries. In this work, we report bismuth ion battery (BIB) as a promising trivalent metal ion battery, next to the only known aluminum ion battery. Our BIB successfully demonstrates battery behavior with discharge plateaus at 0.5 and 0.2 V. Gravimetric capacity of 300 mAh g-1 at current density of 0.2 A g-1 was obtained with ca. 98 % coulombic efficiency. In addition, stable cyclic life was achieved after 100 cycles at 0.3 A g-1 which further suggests its suitability as potential trivalent metal ion battery.

1 2

Bismuth Ion Battery – A New Member in Trivalent Battery Technology

3 4

Abstract: To provide alternative battery technologies to lithium ion battery,

5

multivalent metal ion batteries with their high theoretical capacities and ease of

6

preparation have gradually gained attention from both academia and industries. In this

7

work, we report bismuth ion battery (BIB) as a promising trivalent metal ion battery,

8

next to the only known aluminum ion battery. Our BIB successfully demonstrates

9

battery behavior with discharge plateaus at 0.5 and 0.2 V. Gravimetric capacity of 300

10

mAh g-1 at current density of 0.2 A g-1 was obtained with ca. 98 % coulombic

11

efficiency. In addition, stable cyclic life was achieved after 100 cycles at 0.3 A g-1

12

which further suggests its suitability as potential trivalent metal ion battery.

13

14

1. Introduction

15

With the ever-increasing dependency on portable energy storage devices, battery

16

technologies are under significant scrutiny by both academia and industries. Notably,

17

as the forerunner in battery technologies, lithium ion battery (LIB) has shown

18

significant improvements over the past decades [1-5]. However, due to the eventual

19

bottleneck in LIB research, interest in multivalent metal ion battery has gradually

20

increased to diversify the battery technology research. Such interest is further

21

propelled by their higher theoretical capacities (more electrons per metal ion) and ease

22

of fabrication [6-10]. Although substantial effort has been devoted into researching

23

the only known trivalent ion battery, aluminum ion battery (AIB) still faces numerous

24

challenges such as severe electrode corrosion, limited suitable cathode selection,

25

electrolyte selection, low capacity, and poor cyclic life which impede its future

26

development [11,12]. Despite these limitations, demands for high capacity and

27

compact battery technologies remain insatiable, and trivalent metal ion battery is still

28

an exciting explorative strategy towards developing high performing battery

29

technology. However, selection of trivalent metal as next promising trivalent battery

30

technology is highly limited as most of the known trivalent metals either possesses

31

unfavorable physical state that can make processing highly challenging, or highly

32

toxicity which requires high barrier packaging. This inevitably translates to an uphill

33

struggle in developing the next member of the trivalent metal ion battery technology.

34

Herein, we report a benchtop assembled stable trivalent metal ion battery based on

35

bismuth metal to leverage on its predominant Bi3+ state and its benign environment

36

profile [13-15]. Our device, bismuth ion battery (BIB) comprised of bismuth pellet as

37

anode, V2O5 as cathode, and 1 M Bi(NO3)3•5H2O in Dimethyl sulfoxide (DMSO) as

38

electrolyte. The electrochemical mechanism of BIB consists of 3 steps process; (1)

39

intercalation of Bi3+ into V2O5, (2) eventual reduction of V5+ to V4+ to maintain charge

40

neutrality, and (3) phase change whereby BixV2O5 phase is formed. The as-assembled

41

BIB was able to deliver a capacity of 300 mAh g-1 at current density of 0.2 A g-1.

42

Stable cyclic life was also demonstrated as the BIB was able to retain ca. 90 % of its

43

initial capacity after cycling at 0.3 A g-1 for 100 cycles. Based on this successful

44

preliminary work, we believe that BIB shows potential as viable trivalent metal ion

45

battery due to its ease of preparation, stable Bi, and high electrochemical performance.

46

We expect the performance of our proposed BIB can be further optimized with in-

47

depth studies in cathode and electrolyte selection.

48

2. Materials and methods

49

Materials. DL-Tartaric acid, NaOH pellet, NaH2PO2, Bi(NO3)3·5H2O, Dimethyl

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sulfoxide (DMSO) and V2O5 were purchased from Sigma-Aldrich. Carbon paper

51

(without Micro Porous Layer and PTFE, 0.18 mm, 77% porosity) was purchased from

52

Ce-Tech Co. Ltd.

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2.1 Preparation of Bi particles

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In a typical synthesis, Bi particles were synthesized under an aqueous condition

55

according to a reported method [16]. In a typical synthesis, 0.1 g of DL-Tartaric acid,

56

0.5 g of NaOH and 40 mL of NaH2PO2 (5M) were added to 60 ml of distilled water

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firstly at room temperature and stirred for 30 min. Then, 1 M Bi(NO3)3·5H2O

58

dissolved in 5 mL of HNO3 (4M) was added to the above solution and stirred for 10

59

min. Next, the resulted suspension was transferred to water bath of 60 oC and stirred

60

for 6 h. The resulting black precipitate was filtered and washed with distilled water

61

and absolute ethanol to remove impurities, and then dried at 60 oC to get the final

62

product.

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2.2 Characterization

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The powder X-ray diffraction (XRD) pattern was measured by a powder

65

diffractometer (Bruker D8 Advanced Diffractometer System) with a Cu Kα (1.5418 Å)

66

source. Scanning electron microscopy (SEM) images were recorded on a ZEISS SEM

67

Supra 40 (5 kV). SEM samples were prepared by dripping the sample solutions onto a

68

silicon substrate. Transmission electron microscopy (TEM) was performed on a

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JEOL-3010 (300 kV acceleration voltage). TEM samples were prepared by dripping

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the sample solutions onto a copper grid. Scanning transmission electron microscopy

71

(STEM) studies were conducted using a JEOL ARM200F atomic resolution analytical

72

electron microscope equipped with a cold field-emission gun, a new ASCOR fifth

73

order aberration corrector, and Gatan Quantum ER spectrometer. STEM was operated

74

at 200 kV. Raman spectrometry was conducted on a Horiba MicroRaman HR

75

Evolution System using an argon laser beam with an excitation wavelength of 514.5

76

nm. Surface composition was analyzed by X-ray photoelectron spectroscopy (XPS)

77

using

78

monochromatized Al Ka X-ray source (1486.6 eV) scanning a spot size of 700 µm by

79

300 µm. X-ray absorption spectroscopy (XAS) experiment were performed using

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XAFCA beamline of Singapore Synchrotron Light Source (SSLS).

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2.3 Electrochemical measurements

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All electrochemical tests were performed at room temperature. Cyclic voltammetry

83

(CV), galvanostatic charge/discharge and electrochemical impedance spectroscopy

84

(EIS) measurement were conducted using an electrochemical system (Bio-logic VMP

85

3). The V2O5 particles were mixed with carbon black and polyvinyl difluoride in a

86

ratio of 7:2:1 with N-methyl-2-pyrrolidone. The mixture was hand-grinded for at least

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20 min to obtain a slurry. The slurry was later coated onto carbon paper which served

88

as a current collector, and then heated at 80 ℃ overnight for further use as cathode.

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Bismuth pellet was obtained by pressing the Bi powder at 10 atmospheric pressure. Bi

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pellet and filter paper were used as the anode and separator, respectively, and 1M

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Bi(NO3)3·5H2O dissolved in Dimethyl sulfoxide was employed as the electrolyte. For

92

the three electrode test, the Bi pellet or V2O5 was used as the work electrode using 1

93

M Bi(NO3)3 binary mixture electrolyte at 0.5 mV s−1. Bi pellet was used as both the

94

reference electrode and counter electrode in the three-electrode cell. A CR2025-type

95

coin cell was assembled in room condition to evaluate the electrochemical

96

performance. For both CV and Charge/Discharge of full cell test, the measurement

97

voltage was controlled in the range of 0 – 1.2 V for test. The current densities of 0.2,

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0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1, 2, 3 and 4 A g−1 were used for Charge/Discharge

99

measurement. EIS test was measured in the frequency range from 0.01 to 105 Hz.

100

Capacity, energy density and power density were calculated based on the mass of the

101

active materials from the cathode. The mass of the active material is about 1 mg,

102

pasted onto a 1.2 cm in diameter carbon paper. Based on this information, the mass

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loading is ca. 0.88 mg cm-2. The thickness of our active material is ca. 3 µm and as

104

such our electrode density is ca. 2.95 g cm-3.

105

a

Kratos

Analytical

Axis

UltraDLD

UHV

spectrometer

with

a

3. Results and discussion

106

Bi metal particles were prepared via a facile liquid–solid stirring method. The X-ray

107

diffraction (XRD) peaks presented in Fig. S1a could be indexed to hexagonal bismuth

108

(JCPDS card No. 05–0519), and the as-prepared Bi possessed particle-like

109

morphology (Fig. S1b). Characterization of commercial V2O5 powder was also

110

conducted (Fig. S1d, S1e and S1f) and the XRD peaks can be indexed to

111

orthorhombic V2O5 (JCPDS card No. 65-0131).

112 113

Fig. 1. Electrochemical performance of Bi ion battery. a) Cyclic voltammetry (CV)

114

curves of Bi anode and V2O5 cathode in a three-electrode cell using 1 M Bi(NO3)3

115

binary mixture electrolyte at 0.5 mV s−1. A small piece of Bi pellet was used as the

116

reference electrode and counter electrode in the three-electrode cell, respectively, b)

117

Charge/discharge profiles of the cell tested with the charge/discharge current densities

118

varying from 0.2 to 4 A g−1, c) Rate performance and d) Cycling performance in

119

terms of specific capacity and the corresponding coulombic efficiency at a current

120

density of 0.3 A g−1.

121

The electrochemical stability window for the electrolyte (1 M Bi(NO3)3ꞏ 5H2O in

122

DMSO) was evaluated with cyclic voltammetry (CV) on carbon paper electrodes

123

using Saturated calomel electrode (SCE) as the reference electrode as shown in Fig.

124

S2. The overall stability window could reach ~1.6 V. The behaviors of Bi

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plating/striping and ion insertion/extraction V2O5 electrode were firstly evaluated

126

using cyclic voltammetry (CV) in a three-electrode cell, consisting of two Bi pellets

127

as both counter and reference electrode in 1 M Bi(NO3)3•5H2O in DMSO solvent

128

electrolyte due to the electrolyte salt solubility in DMSO. Obvious Bi

129

plating/stripping process can be observed in Fig. 1a which suggests the feasibility of a

130

reversible reaction, i.e. Bi ↔ Bi3+ + 3e-. Furthermore, the tight overlapping of initial

131

cycle and fifth cycle of the Bi plating/stripping process shown in Fig. S3a indicates

132

that this process is highly reversible. On the other hand, two distinct redox peaks can

133

be observed for V2O5 which could be ascribed to the Bi ion insertion/extraction

134

process. Our proposed Bi ion battery (BIB) was assembled with the as-prepared Bi

135

pellet as anode and V2O5 as cathode. First, we test the BIB in pure DMSO solvent,

136

and the result shows that no solvent insertion process is observed, excluding the

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solvent insertion mechanism (Fig. S3b). When using 1 M Bi(NO3)3ꞏ 5H2O in DMSO

138

as the electrolyte, as shown in Fig. 1b, BIB exhibited battery behavior with sloping

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plateau at ca. 0.5 V followed with the flat plateau at ca. 0.2 V. By considering the

140

cathode mass, the BIB delivered a reversible discharge capacity of ca. 300 mAh g−1 at

141

0.2 A g-1 and ca. 61 mAh g-1 at high current density of 4 A g-1, as shown in Fig. 1c.

142

Also, our Bi ion battery could deliver high energy density of 94.1Wh kg-1, superior to

143

most aluminum ion batteries (Table S1). Fast electrode kinetics and low contact

144

resistances of the BIB was also confirmed with electrochemical impedance

145

spectroscopy (EIS) in Fig. S4. The slope in the low frequency region is attributed to

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Bi3+ diffusion in the bulk material, while the semicircles in the middle- and high-

147

frequency regions correspond to Bi3+ diffusion through the surface layer and charge

148

transfer reaction, respectively [17]. The cycle life performance of BIB was

149

investigated by a continuous cycling test at 0.3 A g-1 for 100 cycles. From Fig. 1d,

150

BIB retained 90 % of its initial capacity after the cycling test, and coulombic

151

efficiencies ca. 98 % were recorded for each of the cycle. At a rate of 1 A g−1 (Fig.

152

S5), BIB was able to achieve ca. 80 % capacity retention after 1000 cycles, indicating

153

its good stability. It should be noted that dendrites were observed on the Bi pellet after

154

cycling (Fig. S6), which could decrease the theoretical capacity and the stability.

155 156

Fig. 2. Characterization of V2O5 cathode at 3 states (equilibrium, discharged 0 V,

157

and charged 1.2 V). a) Normalized V K-edge XANES, b) Bi 4f XPS spectra, c) V 2p

158

XPS spectra, d) Raman spectra of V2O5 at the initial state, fully discharged state and

159

the fully charged state.

160

In order to have a clearer understanding of the mechanism and its reversibility, X-ray

161

absorption near-edge structure (XANES), X-ray photoelectron spectroscopy (XPS),

162

and Raman spectroscopy were employed. For each of the experiments, we prepared

163

our BIB in 3 different states of charge, i.e. (1) equilibrium/initial state, (2) fully

164

discharged, and (3) fully charged. As shown in the XANES result (Fig. 2a), four

165

features associated with electronic transition and vanadyl bond were observed for the

166

3 different states of charge. The V k-edge shifted to lower energy when the BIB was

167

fully discharged from its equilibrium voltage, i.e. open circuit voltage. This indicates

168

a decrease in V valence which may be caused by the Bi3+ intercalation into V2O5. As

169

the voltage of BIB increased to 1.2 V, the V k-edge shifted back to that of the BIB in

170

equilibrium. This promising XANES result suggests that Bi3+ insertion/extraction

171

in/out of V2O5 is reversible [18,19]. To further confirm the Bi3+ insertion/extraction,

172

Bi 4f XPS was recorded for V2O5 cathode as shown in Fig. 2b. In the equilibrium

173

state (initial state), no Bi-associated peak was observed. Interestingly, when the BIB

174

was discharged to 0 V, obvious Bi3+ doublet peaks, corresponding to Bi 4f5/2 and Bi

175

4f7/2, was observed which indicates the presence of Bi species in our V2O5 in the

176

discharged state. When charged to 1.2 V, Bi3+ doublet peaks could still be observed

177

but the peak intensities are less intensive as compared to that at 0 V. This result hints

178

that some of the Bi3+ is unable to fully remove from V2O5, which is consistent with

179

small irreversible loss for the first cycle as shown in Fig. S7. However, with further

180

cycles, there is no capacity loss as the capacity remain stable across the same current

181

density after 5 cycles, indicating the irreversible insertion of Bi3+ just occur during the

182

first cycle. Concurrently, V 2p XPS spectrum was also recorded at V2O5 at these 3

183

different states of charge (Fig. 2c). When discharged to 0 V, V4+ peak appeared.

184

When charging state was at 1.2 V, V4+ peak with low intensity could be observed,

185

consistent with the observed Bi3+ peak with low intensity. Similarly, in the O 1s XPS

186

spectra of the discharged V2O5, the peak at 532.1 eV associated with Bi–O bond

187

could be observed, and the intensity weaken when it is charged to 1.2 V (Fig. S8) [20].

188

Notably, no signal of sulphur is detected for V2O5 at the initial state, fully discharged

189

state and the fully charged state, further confirming the storage mechanism is not

190

solvent insertion (Fig. S9). Raman spectra (Fig. 2d) was conducted on V2O5 at 3

191

different charging states. Weaker intensity was observed for discharged state, i.e. 0 V,

192

as compared to equilibrium state and charged state. This is due to the cathode material

193

becoming more metallic which substantially reduces the penetration depth of the

194

Raman excitation light thus reducing intensity [21]. When charged to 1.2V, the

195

charged V2O5 is roughly the same with the initial stage, indicating negligible structure

196

transformation of V2O5 induced by the insertion and extraction of bismuth ions during

197

cycles. From the combined results of XANES, XPS, and Raman, some deduction can

198

be made: When BIB is fully discharged from its equilibrium state, Bi3+ may

199

intercalate into V2O5 (hence the presence of Bi3+ doublet in Fig. 2b, discharged state,

200

and weaken Raman intensities). This subsequently led to the reduction of V5+ in V2O5

201

to V4+ to ensure charge neutrality due to the intercalation of Bi3+ (hence, the shift in

202

XANES and presence of V4+ in Fig. 2c, discharged state). As BIB becomes fully

203

charged, Bi3+ extract from the V2O5 framework while leading to the oxidization of

204

V4+ back to V5+, and meantime a small amount of V4+ exists due to the trap of some

205

Bi3+ ions for the first cycle.

206

Scanning electron microscopy (SEM), transmission electron microscopy (TEM)

207

and scanning transmission electron microscopy (STEM) mapping were further

208

employed to provide greater insights of the electrochemical mechanism. V2O5

209

retained particle-like structure during/after the electrochemical process as confirmed

210

by SEM images in Fig. S10a, S10b and S10c. Both the fully discharged and fully

211

charged V2O5 showed similar morphology to the initial sample. The color of the V2O5

212

changed from brown for initial V2O5 to dark for fully discharged V2O5, and it

213

recovered to brown for the fully charged V2O5, indicating the reversibility of the

214

phase transformation. For the fresh V2O5, the lattice spacing of 0.576 nm

215

corresponding to (200) plane could be observed (Fig. S10d). While for the fully

216

discharged V2O5, the spacing was found to be 0.668 nm. The enlarged lattice spacing

217

could be due to the insertion of Bi3+ (Fig. S10e). Notably, some amorphous domains,

218

which may be caused by the compressive stress in the V2O5 upon Bi3+ insertion, could

219

be observed. When charged to 1.2 V, the lattice spacing decreased to 0.586 nm (Fig.

220

S10f). The slighter larger lattice spacing may be due to incomplete removal of Bi3+

221

from the interlayer, which is supported by the Bi 4f XPS result, and the irreversible

222

capacity loss. According to the TEM and STEM mapping (Fig. S11), uniform

223

distributions of V, O and Bi were observed throughout the entire selected area of the

224

cathode material which suggests possible Bi3+ insertion.

225 226

Fig. 3. a) Corresponding galvanostatic charge and discharge curves at 0.2 A g-1, b)

227

enlarged XRD patterns, c) XRD patterns, d) enlarged XRD patterns of the three new

228

peaks, and e) Schematic of the energy storage over Bi/V2O5 cell in 1 M Bi(NO3)3

229

binary mixture electrolyte.

230

To study the mechanism in detail, ex-situ x-ray diffraction (XRD) was conducted at

231

each

232

charge/discharge curves at 0.2 A g−1 and the corresponding XRD patterns of V2O5

233

electrode at different states shown in Fig. 3b, 3c and 3d. Interestingly, two

234

observations can be made: (1) continuous shifting of V2O5 (001) characteristic XRD

235

diffraction peak at 20.3o to lower angles during discharging and eventually shifting to

236

higher angle back to initial angle during charging (Fig. 3b). This shift towards lower

237

angle during discharging suggests the widening of interlayer spacing which is in good

238

agreement with our TEM result (Fig. S10e). The subsequent shift towards higher

239

angle back to 20.3o hints the recovering of the interlayer spacing when the Bi3+ is

240

extracted. (2) The emergence and disappearance of three new diffraction peaks during

241

discharging/charging can be observed (Fig. 3c and 3d). This phenomenon may be

242

attributed to the reversible formation/disappearing of a BixV2O5 phase during

243

discharge/charge processes. Based on the XRD result, some conclusions can be made.

244

For discharging process, Bi3+ intercalation into V2O5 occurs between potential of 1.2

245

to 0.35 V. This is supported by the shift to lower angle due to expansion of V2O5

246

interlayer spacing to accommodate Bi3+. Next, phase change of V2O5 occurs at

247

potential of ca. 0.35 V whereby new diffraction peaks were first observed. During

248

charging, Bi3+ extraction occurs ca. 0 V and the process continues till 0.6 V. On the

249

other hand, phase change of BixV2O5 occurs between 0.4 to 0.8 V.

charging and

discharging stages. Fig. 3a shows

the galvanostatic

250

Hence, based on the collective results, the electrochemical mechanism of BIB is

251

proposed in Fig. 3e. During discharging, Bi3+ intercalates into the V2O5 framework,

252

causing the expansion of interlayer spacing as shown in TEM, and XRD results. As

253

Bi3+ intercalates into the V2O5 framework, to maintain charge neutrality, V5+ reduces

254

to V4+ (according to XPS) and subsequently form a new BixV2O5 phase (based on

255

XRD). During the charging process, Bi3+ is firstly removed from V2O5 framework and

256

this leads to the oxidation of V4+ to V5+ (according to XANES, XPS, and XRD) to

257

form V2O5. As such, we propose the following equations for the discharging process

258

of our BIB;

259

anode: xBi → xBi3+ + 3xe−

260

cathode: xBi3+ + 3xe− + V2O5 → BixV2O5

261

overall: xBi + V2O5 → BixV2O5

262

4. Conclusion

263

In this work, bismuth ion battery is proposed as the next step towards trivalent metal

264

ion battery technology. Our BIB was able to demonstrate battery behavior and

265

electrochemical mechanism was discussed. The electrochemical mechanism involves

266

3 stages; (1) intercalation of Bi3+ into V2O5 framework leading to expansion of

267

interlayer spacing, (2) reduction of V5+ to V4+ in order to maintain charge neutrality,

268

(3) phase change to form a new BixV2O5 phase. Our experimental results show clear

269

indications of these stages and good reversibility was also determined. We expect our

270

BIB to be a viable trivalent metal ion battery whereby more optimizations such as

271

cathode/electrolyte selection can be conducted to further enhance its performance.

272 273

Supporting Information

274

Supporting Information is available.

275

Author information

276

Corresponding Author

277

*E-mail: [email protected] (Wee Siang Vincent Lee); [email protected]

278

(Junmin Xue). Tel./fax +65 65164655.

279

Notes

280

The authors declare no competing financial interest.

281

Acknowledgements

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This work was supported by Singapore MOE Tier 1 funding R-284-000-162-114 and

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Singapore MOE Tier 2 MOE 2018-T2-1-149.

284

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Declaration of interests The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.