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Achieving High‐Capacity Cathode Presodiation Agent Via Triggering Anionic Oxidation Activity in Sodium Oxide

July 2024
36(36)

DOI:10.1002/adma.202407720

Authors:

Compensating for the irreversible loss of limited active sodium (Na) is crucial for enhancing the energy density of practical sodium‐ion batteries (SIBs) full‐cell, especially when employing hard carbon anode with initially lower coulombic efficiency. Introducing sacrificial cathode presodiation agents, particularly those that own potential anionic oxidation activity with a high theoretical capacity, can provide additional sodium sources for compensating Na loss. Herein, Ni atoms are precisely implanted at the Na sites within Na2O framework, obtaining a (Na0.89Ni0.05□0.06)2O (Ni–Na2O) presodiation agent. The synergistic interaction between Na vacancies and Ni catalyst effectively tunes the band structure, forming moderate Ni–O covalent bonds, activating the oxidation activity of oxygen anion, reducing the decomposition overpotential to 2.8 V (vs Na/Na⁺), and achieving a high presodiation capacity of 710 mAh/g≈Na2O (Na2O decomposition rate >80%). Incorporating currently‐modified presodiation agent with Na3V2(PO4)3 and Na2/3Ni2/3Mn1/3O2 cathodes, the energy density of corresponding Na‐ion full‐cells presents an essential improvement of 23.9% and 19.3%, respectively. Further, not limited to Ni–Na2O, the structure–function relationship between the anionic oxidation mechanism and electrode–electrolyte interface fabrication is revealed as a paradigm for the development of sacrificial cathode presodiation agent.

Characterization of Na2O‐based high capacity presodiation agent. a) Voltage profile for (Na2O + NiO) composite cathode at 10 mA g⁻¹ with a 4.5 V upper cutoff potential; the inset shows the pure Na2O cathode capacity (<15 mAh g⁻¹) at cutoff 4.5 V. b) Schematic illustration of the preparation procedure of NNO composite presodiation agent by high‐energy ball milling. c) sXRD pattern and d) NPD pattern of NNO presodiation agent and the results of fitting via Rietveld refinement. e) The density of states (DOS) of Na2O (top) and Ni–Na2O (bottom). f) Gibbs free energy diagrams during the pure Na2O and Ni–Na2O decomposition process.

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The structural and local covalent environment evolution during NNO decomposition. a) Ex situ sXRD patterns and the results of fitting via Rietveld refinement of NNO presodiation agent in different voltages. The sXRD peak intensities of Ni–Na2O presodiation agent at 2θ = 14.0°, 19.8°, 23.3°, 24.3°, and 28.3° (Ni–Na2O), 2θ = 16.4°, 18.9°, and 26.9° (NiO), respectively. b–d) TEM images of charged NNO presodiation agent cathode at pristine, charge 4.3 V, and discharge 1.5 V. Insets present the corresponding SEAD patterns. The red and yellow marker lines represent the NiO and Ni–Na2O phases, respectively, and the white ones represent the amorphous phase. e) Ni K‐edge X‐ray absorption near‐edge structure (XANES) spectra at different voltage states. Upper left inset: enlarged pre‐edge of Ni K‐edge XANES spectra and a schematic illustration of Ni–O tetrahedral (tetra.) configuration (Ni in Na2O) and octahedral (octa.) configuration (Ni in NiO). Inset below right: edge positions of Ni K‐edge at different voltage states. f) Ni K‐edge EXAFS spectra (weighted by k³) of pristine and charged 4.5 V NNO presodiation agent. The Ni molar percentage pie chart of Ni–Na2O (green region) and NiO (purple region) in NNO presodiation agent. The fitted Ni–O coordination numbers (C.N.) are shown in the inset.

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Analysis of oxygen behavior upon Na2O oxidation in NNO. a) The top panel shows the galvanostatic charge curve for the initial charging process of the NNO presodiation agent cathode at a current density of 50 mA g⁻¹. Five points are labeled in the charge curve: OCV, 3.25 V,3.45 V, 3.65 V, and 4.5 V, respectively. b) The middle panel shows OEMS results of corresponding time‐resolved evolution rates for O2 and CO2 during initial charging. c) TMS result: amounts of O2 and CO2 collected from the NNO presodiation agent plates with different specific voltages. d) O K‐edge XANES spectra of the NNO presodiation agent cathode and standard samples at TEY modes. The peak at 533 eV represents oxygen in the antifluorite structure of Na2O; the peak at 531.4 eV represents σ* (O─O) peroxide species; and the peak at 531.2 eV represents the hybridized state of O 2p and Ni 3d orbitals in NiO. e) The schematic diagram illustrating the dynamics of electrochemical transfer oxidation process during the charging of Ni–Na2O. The electronic structure of Na2O exhibits a charge transfer electronic ground state in the reduced phase (left). The O (2p) lone pairs denote |O2p. The splitting of the O 2p narrow band into distinct σ, π, π*, and σ* states is illustrated by the red (ΔσO─O) and green (ΔπO─O) arrows, with respect to the conversion of O─O dimer species (bottom horizontal axis).

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Electrochemical performance after presodiation. a) Initial charge profiles of Na3V2(PO4)3 (NVP) and Na2/3Ni2/3Mn1/3O2 (NNMO) with n wt % (n = 0%, 5%, and 10%) NNO presodiation agent cathodes at 10 mA g⁻¹ in the range from 2.5 to 4.3 V and from 2.0 to 4.15 V, respectively. b) Cycling performance of NVP without or with NNO presodiation agent cathodes at 50 mA g⁻¹ in the range from 2.5 to 4.3 V. Inset: the bar chart corresponds to the charge and discharge capacity of the initial cycle at 10 mA g⁻¹. c) Galvanostatic charge/discharge curves of HC||NVP without or with 10 wt% NNO presodiation agent coin‐type full‐cell at 10 mA g⁻¹ (1 st) and 50 mA g⁻¹ (5–50 th) in the range from 1.0 to 4.2 V. d) Cycling performance of HC||NVP without or with 10 wt% NNO presodiation agent coin‐type full‐cell in the range from 1.0 to 4.2 V. e) Galvanostatic charge/discharge curves of HC||NNMO without or with 10 wt% NNO presodiation agent coin‐type full‐cell at 10 mA g⁻¹ (1st) and 50 mA g⁻¹ (5–50 th) in the range from 0.5 to 4.0 V. f) Cycling performance of HC||NNMO without or with 10 wt% NNO presodiation agent coin‐type full‐cell in the range from 0.5 to 4.0 V.

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The impact of NNO on the electrode–electrolyte interface and associated perspective on presodiation agent. a) TOF‐SIMS characterization of pure NVP and NVP‐NNO cycled cathode electrodes after 150 cycles. The normalized depth profiles of the interface and bulk fragments illustrate the structure of CEI. b) 3D renderings of selected secondary ion fragments of different CEI. The sputtered volume is 100 µm (length) × 100 µm (width) × 150 nm (height). c) TEM images of NVP‐NNP after 200 cycles. The IFFT results for the surface and bulk regions are also listed in the figure. The light green‐dashed ground state region is identified as NVP structure, white is defined as carbon layer region, and yellow is assessed as a CEI architecture. d) Scheme of CEI formation and changes on NVP and NVP‐NNO cathodes summarized from characterization data in FEC‐containing electrolytes. e) Perspectives for cathode presodiation agent.

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RESEARCH ARTICLE

www.advmat.de

Achieving High-Capacity Cathode Presodiation Agent Via

Triggering Anionic Oxidation Activity in Sodium Oxide

Yilong Chen, Yuanlong Zhu, Zhefei Sun, Xiaoxiao Kuai,* Jianken Chen, Baodan Zhang,

Jianhua Yin, Haiyan Luo, Yonglin Tang, Guifan Zeng, Kang Zhang, Li Li, Juping Xu,

Wen Yin, Yongfu Qiu, Yeguo Zou, Ziyang Ning,* Chuying Ouyang, Qiaobao Zhang,*

Yu Qiao,* and Shi-Gang Sun

Compensating for the irreversible loss of limited active sodium (Na) is crucial

for enhancing the energy density of practical sodium-ion batteries (SIBs)

full-cell, especially when employing hard carbon anode with initially lower

coulombic eﬃciency. Introducing sacriﬁcial cathode presodiation agents,

particularly those that own potential anionic oxidation activity with a high

theoretical capacity, can provide additional sodium sources for compensating

Na loss. Herein, Ni atoms are precisely implanted at the Na sites within

Na2O framework, obtaining a (Na0.89Ni0.05 □0.06)2O(Ni–Na

2O) presodiation

agent. The synergistic interaction between Na vacancies and Ni catalyst

eﬀectively tunes the band structure, forming moderate Ni–O covalent bonds,

activating the oxidation activity of oxygen anion, reducing the decomposition

overpotential to 2.8 V (vs Na/Na+), and achieving a high presodiation

capacity of 710 mAh/g≈Na2O (Na2O decomposition rate >80%). Incorporating

currently-modiﬁed presodiation agent with Na3V2(PO4)3and

Na2/3Ni2/3 Mn1/3O2cathodes, the energy density of corresponding Na-ion

full-cells presents an essential improvement of 23.9% and 19.3%, respectively.

Further, not limited to Ni–Na2O, the structure–function relationship between

the anionic oxidation mechanism and electrode–electrolyte interface

fabrication is revealed as a paradigm for the development of sacriﬁcial

cathode presodiation agent.

Y.Chen,Y.Zhu,X.Kuai,J.Chen,B.Zhang,J.Yin,H.Luo,Y.Tang,

G. Zeng, K. Zhang, L. Li, Y. Zou, Y. Qiao, S.-G. Sun

State Key Laboratory of Physical Chemistry of Solid Surfaces

Department of Chemistry

College of Chemistry and Chemical Engineering

Xiamen University

Xiamen 361005, China

E-mail: kuaixiaoxiao@yeah.net;yuqiao@xmu.edu.cn

Y. C h e n , X . K u a i , Y. Z o u , Y. Q i a o

Fujian Science & Technology Innovation Laboratory for Energy

Materials of China (Tan Kah Kee Innovation Laboratory)

Xiamen 361005, China

The ORCID identiﬁcation number(s) for the author(s) of this article

can be found under https://doi.org/10.1002/adma.202407720

DOI: 10.1002/adma.202407720

1. Introduction

At present, lithium-ion batteries (LIBs)

reign as the preeminent technology for

energy storage in portable devices and

automotive applications.[1]However, the

scarcity of lithium resources and geo-

graphical limitations makes it impossible

to sustain and meet the exploding mar-

ket demand.[2]Considering the widespread

availability and cost-eﬀectiveness of sodium

resources, sodium-ion batteries (SIBs) tech-

nology emerges as a compelling alternative

to LIBs.[3]In the initial cycle of SIBs, the

anode side irreversibly consumes the ﬁnite

sodium ions released from the cathode, re-

sulting in a decrease in initial coulombic

eﬃciency (ICE), and consequently, lower-

ing energy density.[4]Releasing the inherent

entire capacity of cathode materials across

the full battery system is a complex and

challenging endeavor. Especially when cou-

pled with mainstream hard carbon (HC) an-

odes, their relatively lower ICE (70–90%) in-

evitably triggers irreversible consumption

Z. Sun, Q. Zhang

State Key Laboratory of Physical Chemistry of Solid Surfaces

College of Materials

Xiamen University

Xiamen 361005, China

E-mail: zhangqiaobao@xmu.edu.cn

J. Xu, W. Yin

Institute of High Energy Physics

Chinese Academy of Sciences

Beijing 100049, China

J. Xu, W. Yin

Spallation Neutron Source Science Center

Dongguan 523803, China

Y. Q i u

School of Materials Science and Engineering

Dongguan University of Technology

Guangdong 523808, China

2407720 (1 of 11)

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Depth‐of‐Discharge Dependent Capacity Decay Induced by the Accumulation of Oxidized Lattice Oxygen in Li‐Rich Layered Oxide Cathode

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More and more basic practical application scenarios have been gradually ignored/disregarded, in fundamental research on rechargeable batteries, e.g. assessing cycle life under various depths‐of‐discharge (DODs). Herein, although benefit from the additional energy density introduced by anionic redox, we critically revealed that lithium‐rich layered oxide (LRLO) cathodes present anomalously poor capacity retention at low‐DOD cycling, which is essentially different from typical layered cathodes (e.g. NCM), and pose a formidable impediment to the practical application of LRLO. We systemically demonstrated that DOD‐dependent capacity decay is induced by the anionic redox and accumulation of oxidized lattice oxygen (Oⁿ⁻). Upon low‐DOD cycling, the accumulation of Oⁿ⁻ and the persistent presence of vacancies in the transition metal (TM) layer intensified the in‐plane migration of TM, exacerbating the expansion of vacancy clusters, which further facilitated detrimental out‐of‐plane TM migration. As a result, the aggravated structural degradation of LRLO at low‐DOD impeded reversible Li⁺ intercalation, resulting in rapid capacity decay. Furthermore, prolonged accumulation of Oⁿ⁻ persistently corroded the electrode‐electrolyte interface, especially negative for pouch‐type full‐cells with the shuttle effect. Once the “double‐edged sword” effect of anionic redox being elucidated under practical condition, corresponding modification strategies/routes would become distinct for accelerating the practical application of LRLO.

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Hard carbon (HC) is subjected to low initial Coulombic efficiency (ICE) and unsteady solid electrolyte interphase (SEI), which limits the energy density and cycling performance. Meanwhile, studies related to emerging chemical presodiation have specifically focused on proper redox potential and overlooked its safety hazard. To address these drawbacks of HC and chemical presodiation, a series of high‐safety chemical presodiation solutions based on tetraethylene glycol dimethyl ether (TEGDME) are proposed for uniform and fast presodiation of HC and Bi anodes. Among them, Na‐4‐methylbiphenyl in TEGDME solution exhibits the lowest redox potential (0.146 V vs Na⁺/Na), which achieves the inhibition of initial irreversible sodium uptake. Meantime, the potential‐driven decomposition of fluoroethylene carbonate endows presodiated HC (pNa‐HC) a fast‐ion conducting and robust F‐rich SEI. Accordingly, pNa‐HC delivers an ideal ICE of 99.1% compared to HC (65.28%). Meanwhile, pNa‐HC exhibits significantly enhanced rate performance and cycling life (193.39 mAh g⁻¹ after 2300 cycles at 1000 mA g⁻¹) benefiting from reduced kinetic energy barriers. When pNa‐HC pairs with Na3V2(PO4)3 cathode, the full cell demonstrates a desirable ICE of 91.25%. This work provides a novel and universal solvent design strategy to realize high‐safety chemical pre‐metallation.

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Achieving High‐Capacity Cathode Presodiation Agent Via Triggering Anionic Oxidation Activity in Sodium Oxide

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