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Uniform Lithium Deposition Induced by Polyacrylonitrile Submicron Fiber Array for Stable Lithium Metal Anode Jialiang Lang, Jianan Song, Longhao Qi, Yuzi Luo, Xinyi Luo, and Hui Wu ACS Appl. Mater. Interfaces, Just Accepted Manuscript • DOI: 10.1021/acsami.7b00181 • Publication Date (Web): 14 Mar 2017 Downloaded from http://pubs.acs.org on March 14, 2017

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ACS Applied Materials & Interfaces

Uniform Lithium Deposition Induced by Polyacrylonitrile Submicron Fiber Array for Stable Lithium Metal Anode Jialiang Lang1,‡, Jianan Song1,‡, Longhao Qi1, Yuzi Luo2, Xinyi Luo1, and Hui Wu 1,* 1

The State Key Lab of New Ceramic and Fine Processing, School of Materials Science and

Engineering, Tsinghua University, Beijing 100084, China. 2

School of Materials Science and Engineering, University of Science and Technology Beijing,

Beijing 100084, China. KEYWORDS: lithium metal battery, polyacrylonitrile, fiber array, draw-spinning, stable cycling performance

ABSTRACT: The lithium dendrite growth and low coulombic efficiency (CE) during lithium plating/striping cycles are the main obstacles for practical applications of lithium metal anode. Herein, we demonstrate that polyacrylonitrile (PAN) submicron fiber array could guide the lithium ions to uniformly disperse and deposit onto current collector. The PAN submicron fiber array nearly does not increase the volume of electrode with ultralow mass. By this simple design,

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we achieved stable cycling of lithium metal anode with an average CE of ~ 97.4% for 250 cycles at a current density of 1 mA cm-2 with total Li capacity of 1 mAh cm-2.

Rechargeable batteries have been widely used in energy storage systems for decades.1 Particularly, lithium ion batteries (LIBs) have attracted intense attention due to their high energy/power density and cycle stability.1-3 However, with the dramatic development in consumer electronic devices, electric vehicles and large-scale energy storages, traditional LIBs with graphite anode are not able to keep up with the booming demand according to their limited energy density.4,5 Lithium metal delivers an ultrahigh theoretical specific capacity (3860 mAh g1

) and possesses the lowest electrochemical potential (-3.04 V vs. the standard hydrogen

electrode), therefore Li metal is expected to be a promising candidate as anode material for next generation rechargeable batteries.6 Moreover, Li metal electrodes are imperative for lithiumsulfur (Li-S) batteries and lithium-air batteries, which could potentially deliver high theoretical energy density with realizable low cost.7-10 However, the growth of Li dendrites during cycling causes serious safety problems, such as internal short circuits, which severely limits the widespread applications of Li metal anode.11 Besides, due to the high reactivity to Li metal, it reacts with most liquid electrolytes and forms a solid electrolyte interfacial (SEI) film on the surface to prevent further reactions between Li and electrolytes.12 Unfortunately, the huge volume change during Li plating/striping cycles could lead to a broken SEI film, which makes ‘fresh Li’ exposed to electrolyte again and facilitates dendrite growth in the defects caused by the Li ion concentrating.13 Such sustaining progress not


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only consumes the electrolyte and Li metal leading to a low CE, but also produces large amount of ‘dead Li’ and ‘dead SEI, which increases the internal resistance of the cell.14 Suppressing Li dendrite growth and stabilizing SEI film are the keys to improve the performance of Li metal anode. Using electrolyte additives, including lithium nitrate, polysulfide,15 trace-amount of water16 and halogenated salt,17 is an effective method to reinforce SEI layer. Besides, Zhang’s group demonstrated that the highly concentrated electrolyte could deliver a high CE of ~98.4% at a high current density of 4 mA cm-2 for more than 1000 cycles.18 These electrolytes exhibit low reactivity than the dilute electrolytes, therefore reduce side reactions between Li metal and the electrolytes. The formation of a stable and compact SEI film also prevents further reactions of Li metal. Hu’s group designed a composite solid electrolyte composed of a 3D lithium-ion-conducting ceramic network and polyethylene oxide with Li salt, which could effectively suppress Li dendrites owing to its high mechanical properties.19 Li metal with surface modification also exhibits stable cyclic performance with high CE. Guo’s group reported an artificial Li3PO4 SEI layer by in situ reaction of Li metal with polyphosphoric acid.20 The stable and uniform SEI film not only enhances Li ion conductivity, but also restrains Li dendrite growth. Ultrathin two-dimensional atomic crystal and hollow carbon nanospheres can also function as protective layer for Li metal anode.21,22 Previous studies show that three dimensional glass-fiber with polar functional groups exhibits enhanced affinity with electrolyte and could be employed to uniformly distribute Li ions.23 However, this glass-fiber structure not only increases the mass of the cell, but also occupies some extra space. Herein, we demonstrated that PAN fiber array with large quantities of polar functional groups could guide Li metal to uniformly deposit on both Cu foil and Li metal. PAN fibers exhibit high electrochemical stability with Li metal and electrolyte and the fiber array can be fabricated by a


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draw-spinning method which is industrially acceptable with a low cost. Moreover, there is very slight increase in both space and mass for the full cell. Using the modified current collector, an average CE of 97.4% is achieved for 250 cycles at the current density of 1 mA cm-2 with a total of 1 mAh cm-2 of lithium in ether-based electrolyte. As aforementioned, SEI film is unstable during Li plating/striping cycles due to its brittleness.24 So there are some defects forming in the SEI film, which makes ‘fresh Li’ exposed to the electrolyte again. Li ions concentrate in the vicinity of the defects, causing the rapid growth of Li dendrites at these places (Figure 1a).25 To address this issue, we design a novel electrode by modifying the current collector with PAN fiber array. Previous studies show that additional coatings with polar functional groups can enhance the affinity of electrodes with electrolytes and the polar functional groups can bind with Li ions.13,23 There are a large amount of polar functional groups, such as C=N and C≡N (Figure S1, Supporting Information), on the surface of the PAN fibers, which can function as absorbers of Li ions. When defects are formed in the SEI film, Li ions are absorbed at the defects due to the locally higher electric field. The polar functional groups on the PAN fiber array can effectively bind with Li ions and restrain the concentrating of Li ions at the defects, thereby facilitating the uniform Li ionic flux (Figure 1b). The PAN fiber array can also ensure a large holdup of the electrolyte. Therefore, a homogeneous Li deposition is achieved on the modified current collector. Cu foils are widely used current collectors for LIBs and Li metal batteries. Via drawspinning, the PAN fiber array was coated on the Cu foil (Figure 1c, Figure S2, Supporting Information). The PAN fiber array shows a uniform morphology with an average diameter of 1.1 µm (Figures S3, S4, Supporting Information). The cyclic voltammetry (CV) curve of the PANCu current collector shows no obvious cathodic peak and anodic peak (Figure S5, Supporting


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Information), which indicates that the PAN fibers exhibit an electrochemical stability against Li metal and the electrolyte. The bare Cu foils are selected as control samples in this work. Scanning electron microscope (SEM) characterization was performed to compare the morphology of Li deposition on bare Cu and the modified PAN-Cu current collector. Figures 2a-c show the SEM images of deposited Li on bare Cu with different areal capacities at the current density of 1 mA cm-2. The deposited Li on bare Cu shows an inhomogeneous and threadlike structure with a high surface area, which may lead to more side reactions between Li anode and the electrolyte. In contrast, the morphology of Li deposited on the modified PAN-Cu electrode is more uniform with a pancakelike structure (Figures 2d-i). And the PAN fiber array is on the surface of Li metal even at a high areal capacity of 3 mAh cm-2. The SEM images of the control electrodes with a low magnification are shown in Figure S6. The cross-sectional images clearly show that Li was plated under the PAN fiber array due to the weak contact between the PAN fibers and the Cu foil (Figures 2j-l). The PAN fiber array hinders the concentration of Li ions in the vicinity of the defects, thereby facilitating a uniform deposition of Li. The more compact structure of the deposited Li on the modified PAN-Cu electrode with a lower surface area enables a high CE of Li plating/striping cycles. The PAN fiber array also maintained a stable structure and morphology after Li deposition and dissolution, which also indicates that the PAN fibers are stable with Li metal (Figure S7, Supporting Information). To further investigate the overall electrochemical performances of the modified PAN-Cu electrode, the galvanostatic cycling test was conducted with Li foil as the counter electrode, the modified PAN-Cu and bare Cu as working electrode. The ether-based electrolyte with lithium nitrate (2 wt%) as additive was used and the LiNO3 additive was used for stabilizing the SEI


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film.26 CE is an important index which reflects the cyclic performance of Li anode. We calculated the CE from the ratio of the amount of Li striping versus the amount of Li depositing onto the working electrode for each cycle. All the batteries were first cycled between 0 V and 1 V at the current density of 0.05 mA cm-2 to form a stable SEI on the surface of the electrodes (Figure S8, Supporting Information). As shown in Figures 3a, b, the modified PAN-Cu electrode delivers an average CE of 98.1% and 97.4% at the current density of 0.5 mA cm-2 and 1 mA cm-2 with a total of 1 mAh cm-2 of Li deposition, respectively. Moreover, a stable cycling was achieved for 250 cycles. In contrast, the CE of the control electrode dropped to below 90% after 60 cycles at 1mA cm-2 and 70 cycles at 0.5 mA cm-2. The lower CE of the control electrode indicates that more consumption of Li metal and the electrolyte occurred due to the side reactions between Li anode and the electrolyte.22 The modified electrodes benefit from the compact structure and low surface area of deposited Li, thereby reducing the side reactions and delivering an enhanced CE.27 The voltage profiles of Li plating/striping cycles are shown in Figures 3c, d. The Li plating voltage of the modified electrode is ~ -34 mV for the 10th cycle and ~ -29mV for the 50th and 100th cycles. The Li striping voltage of the modified electrode is ~ 35 mV for the 10th cycle and ~ 30 mV for the 50th and 100th cycles. In comparison, the Li plating voltage of the control electrode is ~ -53 mV for the 10th cycle, ~ -48 mV for the 50th cycle and ~ -70mV for the 100th cycles. The Li striping voltage of the control electrode is ~ 51 mV for the 10th cycle, ~ 45 mV for the 50th cycle and ~ 78mV for the 100th cycles. The overpotential of the modified electrode is lower and more stable than that of the control electrode due to the more uniform and compact structure of the deposited Li.28 Whereas the overpotential of the control electrode increased remarkably from the 50th cycle to 100th cycle due to the large amount of dead SEI and dead Li,


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which increased the internal resistance of the cell.29 To further explain the high performance of the modified electrode, we disassembled the batteries after the 100th plating of Li (1 mAh cm-2). SEM images show that the modified electrode exhibits a dense morphology while the control electrode exhibits a loose and porous structure (Figure S9, Supporting Information). Electrochemical impedance spectroscopy (EIS) of the modified electrode also reveals the stable structure of the deposited Li (Figure S10, Supporting Information). The charge transfer impedance stayed at around 11 ohms between the 50th deposition and the 100th deposition, indicating a stable and thin SEI film on the modified electrode.30 Even for a high capacity of 3 mAh cm-2 of Li deposition, a stable cycling was achieved with an average CE of ~ 96.5% for 100 cycles at a current density of 1 mA cm-2 (Figure S11, Supporting Information). A symmetric test was conducted with two Li foil as the electrodes. The PAN fiber array was transferred onto the Li foil and the PAN-Li electrode was regarded as the modified electrode. The bare Li foil was regarded as the control electrode. 3 mAh cm-2 of Li deposition/dissolution was conducted for 150 cycles at a high current density of 3 mA cm-2. As shown in Figure 4a, the modified electrode delivers a low overpotential in the initial stage and the overpotential only increased slightly from the 1st cycle to the 150th cycle. In comparison, the overpotential of the control electrode increased over 200% from ~ 80 mV to ~ 250 mV. Owing to the better affinity with the electrolyte, the modified electrode delivers a lower overpotential. During cycling, the modified electrode benefited from the uniform deposition of Li and the stable and thin SEI film, therefore exhibited a stable voltage profile. Caused by the constant side reactions between the control electrode and the electrolyte, severe electrolyte consumption and an accumulated SEI film led to the rising overpotential of the control electrode. After 20 cycles, the batteries were disassembled to investigate the morphology of the electrodes. SEM images show that the


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modified electrode possesses a compact structure with a low surface area, while the control electrode exhibits a porous and loose structure (Figures 4b, c). The digital photos also reveal the obvious differences between them. The modified electrode is silver white, which is similar with the nature color of Li metal, indicating a thin SEI film and a dense Li structure. In contrast, the control electrode is dark black, which is caused by the porous structure and the large amount of SEI film. We also assembled full batteries with LiFePO4 as cathode. The cycling performance of the modified electrode is greatly improved compared with the control electrode (Figure S12, Supporting Information). After 100 cycles, the reversible capacity of the PAN-Cu electrode is 127 mAh g-1 with an average CE of 99.8%, corresponding to a capacity retention of 86.4%. In contrast, the reversible capacity of the bare Cu electrode is 64.1 mAh g-1 after 100 cycles. The PAN-Cu electrode also delivers a higher and more stable CE in the carbonate-based electrolyte than the bare Cu electrode (Figure S13, Supporting Information). In summary, we designed a novel Li metal electrode with PAN fiber array as a functional coating which achieves a stable cycling performance. The PAN fiber array with polar groups enables a homogeneous deposition of Li metal and effectively suppresses the dendrite growth. Moreover, the PAN fiber array occupies very small space with an ultralight mass, therefore nearly has no influence on the energy density of the full cell. An average CE of 97.4% for 250 cycles was achieved at the current density of 1 mA cm-2 with a capacity of 1 mAh cm-2. For a symmetric cell, a stable cycling with a low and stable overpotential was obtained even at a high current density of 3 mA cm-2 for 300 hours. The modified electrode can be easily fabricated with a low cost via an industrially acceptable method. Furthermore, such method is potentially applied to other metal electrodes which suffer from the similar problems with Li metal electrode.


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Figure 1. Schematic diagrams of Li deposition and process of fabricating PAN-Cu electrode. (a) Schematic diagram of Li deposition on bare Cu electrode. (b) Schematic diagram of Li deposition on PAN-Cu electrode. (c) Schematic diagram showing the process of fabricating PAN-Cu electrode.

Figure 2. Morphology of Li deposition on bare Cu electrode and PAN-Cu electrode with different areal capacities of Li at the current density of 1 mA cm-2. (a-c) Top-view SEM images of Li deposition on bare Cu for a total of 1 mAh cm-2, 2 mAh cm-2 and 3 mAh cm-2. (d-f) Topview SEM images of Li deposition on PAN-Cu for a total of 1 mAh cm-2, 2 mAh cm-2 and 3


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mAh cm-2 with a low magnification. (g-i) Top-view SEM images of Li deposition on PAN-Cu for a total of 1 mAh cm-2, 2 mAh cm-2 and 3 mAh cm-2 with a high magnification. (j-l) Crosssectional SEM images of Li deposition on PAN-Cu for a total of 1 mAh cm-2, 2 mAh cm-2 and 3 mAh cm-2. Scale bars in (a-c, g-i) are 2 µm. Scale bars in (d-f, j-l) are 10 µm.


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Figure 3. Cycling performances of the Cu electrode and the PAN-Cu electrode at various current rates. (a) Comparison of the CE of Li deposition on bare Cu and PAN-Cu electrode at current density of 0.5 mA cm-2 with 1 mAh cm-2 of Li plated in each cycle. (b) Comparison of the CE of Li deposition on bare Cu and PAN-Cu electrode at current density of 1 mA cm-2 with 1 mAh cm2

of Li plated in each cycle. (c) Voltage profiles of the Li plating/stripping process for PAN-Cu

electrode at 1 mA cm-2. (d) Voltage profiles of the Li plating/stripping process for the bare Cu electrode at 1 mA cm-2.

Figure 4. Symmetrical cell testing of bare Li electrode and PAN-Li electrode. (a) Comparison of voltage profiles of the Li plating/stripping process at the current density of 3 mA cm-2 for a total of 3 mAh cm-2 of Li. (b) SEM image and digital photo of PAN-Li electrode after 20 cycles. (c) SEM image and digital photo of Li electrode after 20 cycles. Scale bars in (b,c) are 2 µm.


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ASSOCIATED CONTENT Supporting Information. Fourier transform infrared spectroscopy of PAN submicron fibers. Digital photo of PAN-Cu current collector. SEM images of PAN-Cu current collector. Statistics of the PAN submicron fiber diameter distribution. Cyclic voltammogram of the PAN-Cu electrode. SEM images of Li deposition on bare Cu electrode with different areal capacity of Li. SEM images of PAN-Cu current collector after the 1st cycle of Li plating and stripping. Voltage profiles of the electrode for the SEI formation process during the first ten cycles of charge/discharge. Morphology of Li deposition on bare Cu electrode and PAN-Cu electrode after 100 cycles. EIS for the modified electrode with the Li foil as the counter electrode. Comparison of the CE of Li deposition on bare Cu and PAN-Cu electrode with high areal capacity. Cycling performance of the Li|LiFePO4 battery system using Li metal electrode and PAN-Li electrode. The material is available free of charge via the Internet at http://pubs.acs.org. AUTHOR INFORMATION Corresponding Author Hui Wu* E-mails: [email protected] Author Contributions The manuscript was written through contributions of all authors. All authors have given approval to the final version of the manuscript. ‡These authors contributed equally. Notes The authors declare no competing financial interest. ACKNOWLEDGMENT


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Hui Wu acknowledges the support from the National Basic Research of China (Grants 2015CB932500), and National Natural Science Foundations of China (Grant 51661135025 and 51522207). REFERENCES (1) Goodenough, J. B. Energy Storage Materials: A Perspective. Energy Stor. Mater. 2015, 1, 158-161. (2) Armand, M.; Tarascon, J. M. Building Better Batteries. Nature 2008, 451, 652–657. (3) Goodenough, J. B.; Park, K. S. The Li-Ion Rechargeable Battery: A Perspective. J. Am. Chem. Soc. 2013, 135, 1167-1176. (4) Tarascon, J. M.; Armand, M. Issues and Challenges Facing Rechargeable Lithium Batteries. Nature 2001, 414, 359–367. (5) Evarts, E. C. Lithium Batteries: To the Limits of Lithium. Nature 2015, 526, S93-S95. (6) Xu, W.; Wang, J.L.; Ding, F.; Chen, X.L.; Nasybulin, E.; Zhang, Y.H.; Zhang, J.G. Lithium Metal Anodes for Rechargeable Batteries. Energy Environ. Sci. 2014, 7, 513–537. (7) Grande, L.; Paillard, E.; Hassoun J.; Lee, Y. J.; Sun, Y. K.; Passerini, S.; Scrosati, B. The Lithium/Air Battery: Still an Emerging System or a Practical Reality? Adv. Mater. 2015, 46, 784800. (8) Bruce, P. G.; Freunberger, S. A.; Hardwick, L. J.; Tarascon, J. M. Li-O-2 and Li-S Batteries with High Energy Storage. Nat. Mater. 2012, 11(1), 19-29.


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(30) Yun, Q. B.; He, Y. B.; Lv, W.; Zhao, Y.; Li, B. H.; Kang, F. Y.; Yang, Q. H. Chemical Dealloying Derived 3D Porous Current Collector for Li Metal Anodes. Adv. Mater. 2016, 28, 6932-6939.


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Uniform Lithium Deposition Induced by ... - ACS Publications

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