Conductive Polymer Binder-Enabled SiOâSnxCoyCz Anode for High

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A conductive polymer binder–enabled SiOSnxCoyCz anode for high-energy lithium-ion batteries Hui Zhao, Yanbao Fu, Min Ling, Zhe Jia, Xiangyun Song, Zonghai Chen, Jun Lu, Khalil Amine, and Gao Liu ACS Appl. Mater. Interfaces, Just Accepted Manuscript • DOI: 10.1021/acsami.6b00312 • Publication Date (Web): 10 May 2016 Downloaded from http://pubs.acs.org on May 13, 2016

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ACS Applied Materials & Interfaces

A conductive polymer binder–enabled SiO-SnxCoyCz anode for high-energy lithium-ion batteries Hui Zhao,a Yanbao Fu,a Min Ling,a Zhe Jia,a Xiangyun Song,a Zonghai Chen,b Jun Lu,b Khalil Amine,b and Gao Liua* a

Applied Energy Materials Group, Energy Storage and Distributed Resources Division, Lawrence

Berkeley National Laboratory, Berkeley, California, 94720, United States b *

Argonne National Laboratory, Chicago, Illinois, 60439, United States Tel.: +1-510-486-7207; Email: [email protected] (G. Liu)

Abstract: A SiOSnCoC composite anode is assembled using conductive polymer binder for the application in next generation high energy density lithium ion batteries. A specific capacity of 700 mAh/g is achieved at a 1C (900 mA/g) rate. High active material loading anode with an areal capacity of 3.5 mAh/cm2 is demonstrated by mixing SiOSnCoC with graphite. To compensate for the lithium loss in the 1st cycle, stabilized lithium metal powder (SLMP) is used for prelithiation, when paired with a commercial cathode, a stable full cell cycling performance with a 86% 1st cycle efficiency is realized. By achieving these important metrics toward a practical application, this conductive polymer binder/SiOSnCoC anode system presents great promise to enable the next generation high-energy lithium ion battery. Keywords: lithium-ion battery, high capacity anode, conductive polymer binder, prelithiation, practical application

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Introduction The development of high capacity alloy anode such as tin and silicon for lithium-ion battery application has received significant attention, due to their well-improved capacities compared to the state-of-the-art graphite anode.1,2,3 However, a tremendous volume expansion of over 300% occurs in the full lithiation of Si,4 the active material particles tend crack during the lithiation process, and excessive solid electrolyte interphase (SEI) formation is triggered, both contribute to a fast capacity decay.5 To achieve a successful commercial application of these new high capacity anode, material loading on the lithium ion electrode is also an important metric.6 Typically, the areal capacity of Si-based electrode is only less than 1 mAh/cm2, the area capacity of Si anode is not obviously improved unless a sophisticated electrode architecture design is involved in the electrode fabrication process.7,8 There is an urgent need to further increase the Si anode material loading while maintaining a stable electrochemical performance.9 An areal capacity of ~3 mAh/cm2 at a C/20 rate was recently achieve by a nano-architectural design.8 Silicon oxide10, silicon/carbon composite and silicon-containing alloy represent the new trend in the advancement of high-capacity anode materials, which have intermediate capacities (800~1500 mAh/g) and reduced volume changes (100~150%). Because of the smaller volume changes, it is easier to achieve a high-loading electrode while achieving a satisfactory electrochemical performance.11 A new anode material was developed based on 50 wt% SiO and 50 wt% Sn30Co30C40 composite (molecular composition: SiSn0.23Co0.23C0.3O).12 This composite combines the advantageous properties of both SiO (high capacity) and SnCoC (stable cycling performance). In this work, we developed an improved electrode based on this new SiO-SnCoC composite toward practical application in lithium-ion batteries. 2


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Experimental Materials. We purchased the agents and chemicals from Sigma-Aldrich, these agents were used without further purification. SiOSnCoC anode material is fabricated using a procedure in a previous report.9 Celgard 2400 separator is obtained from Celgard. Lithium-ion electrolyte were purchased from BASF, including 1 M LiPF6 in ethylene carbonate, diethyl carbonate (EC/DEC=3/7 w/w) containing 30 wt% fluoroethylene carbonate (FEC). Electrode lamination and cell testing. The slurry preparation, electrode coating and cell fabrication can be found in the literature.5,13All the electrode laminate in this study is composed of 5% binder, 15% Super P carbon black and 80% active anode materials. The performance of the assembled 2325 coin cells was evaluated with Maccor Series 4000 Battery Test system in a thermal chamber at 30 oC.14 The cut-off voltage of cell testing is between 1.0 V and 0.01V, assuming a theoretical value of 900 mAh/g for SiO. SLMP was loaded on top of the SiO electrode evenly by spreading out method. The electrode with SLMP was then calendared with rolling press (EQ-MR 100A from MTI Corportion) to activate SLMP. The cell with SLMP was rested for 24 hours to allow full prelithiation before cycling. Characterization. A JSM-7500F scanning electron microscopy (SEM) was used to characterize the morphology of the electrode surface.15,16,17 Electrodes after cycling were rinsed with dimethyl carbonate (DMC) solvent to remove residual electrolyte inside the argon filled glove box. A homemade transfer system equipped with a gate valve and a magnetic manipulator are used for the transfer of the highly sensitive samples from the pure argon atmosphere of the glove box to the SEM system. Transmission Electron Microscopy (TEM) images was produced by a 200 kilovolt FEI monochromated F20 UT Tecnai.18,19,20 3



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Results and Discussion

Figure 1. (a) The chemical structure of PFM conductive polymer binder. (b) SEM morphology of the SiOSnCoC pristine particles. (c) TEM image of the SiOSnCoC particle. (d) High-resolution TEM image of the SiOSnCoC, indicating the existence of the crystalline Si phases in nanodomain.

Poly (9,9-dioctylfluorene-co-fluorenone-co-methyl benzoic ester) (PFM) was specially designed and synthesized, which combins adhesion and electrical conduction to provide molecular-level electronic connections between the active material and the conductive polymer matrix,21,22 as shown in Figure 1a. The SEM image of the pristine SiOSnCoC particles is shown in Figure 1b, indicating a bimodal distribution of the particle size, a typical morphology of particle material synthesized by high-energy ball-milling method. The smaller particles have a diameter of typically several hundred nanometers, and bigger particles have diameter of several micrometers. The TEM images in Figure 1c and 1d further discloses some details on the anode structure. Crystalline Si phases exist as nanodomains, which contribute to most of the specific capacities 4


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when used in lithium ion batteries.

Figure 2. (a) Cycling performance of SiOSnCoC half cells using either PFM (at 1C, 900 mA/g) and PVDF binder (at C/10, 90 mA/g). (b) The 1st cycle and 40th cycle voltage curves of the SiOSnCoC/PFM half cell. (c) Areal capacity and specific capacity vs. cycle no. for the SiOSnCoC/graphite/PFM high loading electrode at C/10. (d) The 1st cycle and 25th cycle voltage curves of the SiOSnCoC/graphite/PFM high loading half cell.

When cycling the half cell at a 1C rate, the PFM-based half cell exhibits a stable cycling with a specific capacity of above 700 mAh/g for over 50 cycles (Figure 2a). PVDF binder, on the other hand, shows a drastic capacity decay even at a slow rate of C/10. The 1st cycle and 40th cycle voltage curves of the PFM/SiOSnCoC cell are shown in Figure 2b. Different from a lot of other Si-based anode with crystalline Si phases,23 the good conductivity of this SiOSnCoC realizes 1st cycle lithiation without much overpotential. Also comparing the delithiation voltage curves at 1st and 40th cycles, the minimum capacity decay is further confirmed. To increase the Si material loading to a benchmark areal capacity of above 3 mAh/cm2, a graphite/SiOSnCoC composite electrode is assembled and tested. This composite electrode 5



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employs 5% PFM binder, 15% carbon black, 20% graphite and 60% SiOSnCoC. As shown in Figure 2c, a high capacity value of 3.5 mAh/cm2 is successfully reached using the composite electrode at a C/10 rate. The 1st cycle and 25th cycle voltage curves shown in Figure 1d indicates minimum capacity loss during cycling of this high loading cell. Addition of Si-based material into the commercial cell anodes with a small portion represents a most promising route toward the commercial application of high capacity Si anode, the currents conductive polymer binder-based laminates exhibits a great potential toward the practical application. PVDF/SiOSnCoC

PFM/SiOSnCoC

PFM/SiOSnCoC/graphite

Qca(mAh/g)

836.4

806.6

511.13

ηb (%)

59.77%

54.45%

50.77%

Qca (mAh/g)

335.7

695.3

463.8

ηb (%)

99.35

99.49

99.27

st

1 cycle

th

40 cycle a

charge (delithiation) capacity

b

Coulombic efficiency

Table 1. Electrochemical data of the half cells using SiOSnCoC anode.

The electrochemical data of PVDF and PFM-based lithium ion cell, and the PFM/SiOCoC/graphite composite are shown in Table 1. The overall cell efficiency based on PFM binder is higher than 99.5% after 40 cycles (Figure S1 in supporting information). With 20% graphite and 60% SiOSnCoC in the composite electrode, the specific capacity reaches 500 mAh/g, which is a much higher value compared to the state-of-the-art graphite anode (372 mAh/g). While the areal capacity of this high-loading cell reaches 3.5 mAh/cm2, this system proves to be a competitive alternative high energy anode.

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Figure 3. (a) (b) SEM images of the pristine SiOSnCoC/PFM electrode. (c) (d) SEM images of the SiOSnCoC/PFM electrode cycled at C/10 for 10 cycles.

The morphology of the pristine (Figure 3a and 3b) and cycled (Figure 3c and 3d) SiOSnCoC/PFM are shown in Figure 3. A very nice porosity is exhibited in the pristine electrode, which is critical for accommodating the volume expansion on the particle level, as well as to soak electrolyte for a good lithium ion transport.24,25 FEC-containing electrolyte is used for the cell testing, the cycled electrode shows a typical solid electrolyte interphase (SEI) formation in the FEC-containing electrolyte. No excessive SEI is visualized in the SEM images, this contributes to a good coulombic efficiency shown in Table 1. To prove the application of this conductive polymer binder-based SiSnCoC high capacity anode in a full cell configuration, a commercial N1/3M1/3C1/3 is used to assemble the full cell. However, the efficiencies at 1st cycles shown in Table 1 is only around 50%, which irreversibly consumes the lithium in the cathode in the first cycle, this could be a detrimental problem for 7



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practical application. A prelithiation method is needed for the full cell application.

Figure 4. (a) Full cell cycling performance of SiOSnCoC/PFM anode with NMC cathode with or without SLMP prelithiation. (b) The 1st cycle and (c) 30th cycle voltage curves of the SiOSnCoC/PFM full cell with or without SLMP prelithiation. (d) The open circuit voltage curves of the two full cells with and without SLMP. (e) SEM image of the SiOSnCoC/PFM anode in the full cell without SLMP after 24 hour equilibration, exhibiting similar morphology as the pristine electrode. (f) SEM image of the SiOSnCoC/PFM anode in the full cell with SLMP after 24 hour equilibration, indicating a complete SEI formation.

To compensate for the irreversible capacity loss in the first cycle, stabilized lithium metal powder (SLMP®) is used to prelithiate the SiOSnCoC anode in the full cell. SLMP is a micro-size lithium metal powder with ~2 wt% lithium carbonate surface coating.26,27 SLMP was directly loaded on the anode surface, which proved to be a simple and effective way of applying SLMP.28 8


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The amount of loaded SLMP was calculated to theoretically eliminate all the irreversible capacity in the first cycle. A calendar machine was used to pressure-activate the SLMP particles. This operation breaks the lithium carbonate (Li2CO3) shell and allows lithium to be in direct electrical contact with the SiOSnCoC materials in the anode.29 A 24-hour rest period was used to allow the crushed SLMP to fully prelithiate the anode before current-driven charging of the cells. As a good control, the full cell without SLMP was also rested for 24 hours before cycling. A formation process using two cycles at C/10 prior to C/3 cycling was applied to both full cells. Apparent improvement was shown for the SLMP-loaded full cells (Figure 4a). The first cycle CE increased from 48% to ~86% with the SLMP. SLMP enabled the NMC/SiOSnCoC full cell to maintain a reversible capacity of ~150 mAh/g after more than 35 cycles at C/3. The full cell without SLMP prelithiation started only with a capacity of ~90 mAh/g and dropped to ~65 mAh/g after 35 cycles. The first cycle voltage curves of the full cells are shown in Figure 4b. Compared to the regular cell without SLMP, the voltage profile at both ends (start of charge and end of discharge) are distinctly different, indicating different lithiation and delithiation of SiOSnCoC during these two stages. In the first cycle charge process, SLMP eliminated the needs for SEI formation, so the curve goes directly to the anode lithiation voltage region. When SLMP is not used, this charging curve shows a long multi-plateau curvature accounting for a capacity of ~40 mAh/g, which is typical for SEI formation. The SEM image of the SiOSnCoC electrode rested for 24 hours in a full cell without SLMP is shown in Figure 4e and 4f. Compared to the pristine electrode (Figure 3a,b), no apparent morphology change occurred during this equilibration period. When the full cell is loaded with SLMP on the SiOSnCoC electrode, the SEM image in Figure 4f shows a clear SEI formation due to the electrolyte decomposition after 24-hour rest period. 9



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Full cell without SLMP

Full cell with SLMP

Qda(mAh/g)

90.6

181.5

ηb (%)

47.52%

86.05%

Qda (mAh/g)

70.5

144.0

ηb (%)

99.57

1st cycle

th

35 cycle a

discharge (delithiation) capacity

99.49 b

Coulombic efficiency

Table 2. Electrochemical data of the full cells with or without SLMP prelithiation.

The electrochemical data of the full cells are shown in Table 2. The SLMP prelithiation successfully increases the 1st cycle efficiency from 47.52% to 86.05%, which is a comparable value to the state-of-the-art NMC/graphite full cells. Both cells show an efficiency a around 99.5% at the 35th cycle (efficiency plot of the full cell with SLMP is shown in Figure S2 in supporting information), this indicates that SLMP prelithiation only affect the cell behavior at the 1st cycle, without much effect in the following cycles.

Conclusions By the combination of a new composite anode material SiOSnCoC with a special-design conductive polymeric binder, several key parameters for a commercial Si-based lithium ion battery are achieved, including high specific capacity (700 mAh/g at a 1C rate), high material loading (areal capacity of 3.5 mAh/cm2), fast charge/discharge without significant cell decay, stable cycling when paired with a commercial cathode, and a high 1st cycle coulombic efficiency (86%) in the full cell. This conductive polymer binder/SiOSnCoC anode system presents great promise to enable the next generation high-energy lithium ion battery.

ASSOCIATED CONTENT Supplementary Information Details about coulombic efficiency of the cell based on this conductive polymer-based high

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capacity anode. This material is available free of charge via the Internet at http://pubs.acs.org

AUTHOR INFORMATION Corresponding Author *E-mail: [email protected]

Notes The authors declare no competing financial interests.

ACKNOWLEDGEMENTS This work was funded by the Assistant Secretary for Energy Efficiency, Vehicle Technologies Office of the U.S. Department of Energy (U.S. DOE) under the Advanced Battery Materials Research (BMR) and Applied Battery Research (ABR) Programs. TEM is performed at the National Center for Electron Microscopy. All these projects and facilities are supported by the Director Office of Science, Office of Basic Energy Sciences, of the U.S. Department of Energy, under Contract # DE-AC02-05 CH11231.

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Conductive Polymer Binder-Enabled SiOâSnxCoyCz Anode for High

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