Internationale Ausgabe: DOI: 10.1002/anie.201905251Lithium BatteriesDeutsche Ausgabe: DOI: 10.1002/ange.201905251

Temperature-dependent Nucleation and Growth of Dendrite-FreeLithium Metal AnodesKang Yan, Jiangyan Wang, Shuoqing Zhao, Dong Zhou, Bing Sun,* Yi Cui,* and Guoxiu Wang*

Abstract: It is essential to develop a facile and effective methodto enhance the electrochemical performance of lithium metalanodes for building high-energy-density Li-metal based bat-teries. Herein, we explored the temperature-dependent Linucleation and growth behavior and constructed a dendrite-free Li metal anode by elevating temperature from roomtemperature (20 8C) to 60 8C. A series of ex situ and in situmicroscopy investigations demonstrate that increasing Lideposition temperature results in large nuclei size, lownucleation density, and compact growth of Li metal. Wereveal that the enhanced lithiophilicity and the increased Li-iondiffusion coefficient in aprotic electrolytes at high temperatureare essential factors contributing to the dendrite-free Li growthbehavior. As anodes in both half cells and full cells, thecompact deposited Li with minimized specific surface areadelivered high Coulombic efficiencies and long cycling stabil-ity at 60 8C.

It is widely recognized that lithium-based batteries includingLi metal-ion, Li–sulfur and Li–air batteries are promisingnext generation batteries, owing to their ultra-high capacitiesand energy densities.[1] Significant progress has been achievedon sulfur cathodes since the Li–sulfur batteries with superhigh capacities were reported in 2009.[2] New materials arealso explored for high-performance oxygen cathode of Li–airbatteries.[3] The performances of both Li–sulfur and Li–airbatteries significantly depend on Li metal anodes. However,the research on Li metal anode only started to flourish overthe past five years.[4] Dendrite-free Li metal anodes with highCoulombic efficiencies are the ultimate goal to achieve high-energy-density Li metal batteries. It was widely recognized

that partial strong electric field leads to non-uniform Li iondistribution thus resulting in dendrite generation. Therefore,reducing local current density by increasing the surface areaof current collector is a popular strategy to suppress Lidendrite.[5] Moreover, considerable approaches have beendeveloped to suppress Li dendrite formation during repeatedplating/striping process. These include surface protectivelayer,[6] large area conductive/non-conductive hosts[7] andnovel ion refluxing structures.[8] However, the formation andgrowth mechanisms of Li dendrite are still intricate andobscure due to many factors in the complex battery system.Although previous investigations probed Li dendrite growthregarding various factors,[9] the common factor of temper-ature is seldom studied in the spectrum of dendrite formation.Apart from consumer electronics that work at room temper-ature, emerging applications expect batteries to operateunder thermal extremes. As the choice of anodes in nextgeneration high-energy-density batteries, Li metal anoderequires the critical examination on its thermal character-istics.

Herein, we revealed the dramatic changes of Li nucleationand growth behavior under the influence of operationtemperatures. Enhanced lithiophilicity and rapid Li ionmigration induced by the increase of temperature contributedto large nuclei size and small nucleation density, whichresulted in uniform and compact Li deposition. We furtherdemonstrated that the differences of Li nucleation behaviorsoriginate from the onsets of Li nuclei formation via in situoptical microscope observation. At 60 8C, the formation of Lidendrite was effectively suppressed and the solid electrolyteinterface (SEI) was stabilized, the corresponding Li j jCu halfcells and Li j jLi4Ti5O12 (LTO) full cells achieved extendedlife-spans and increased Coulombic efficiencies.

We first elucidated the differences of Li nuclei layers atvarious temperatures and current densities using Li j jCu halfcells in ether-based electrolyte (1m lithium bis (trifluorome-thanesulfonyl)imide (LiTFSI) in 1,3-dioxolane/1,2-dime-thoxymethane (DOL/DME, 1:1 v/v) with 1 wt % LiNO3). Toinvestigate the morphologies of Li nuclei layers, a fixed arealcapacity of 0.1 mAh cm�2 was used, which exactly fulfilled theinitial Li nucleation processes. As shown in scanning electronmicroscope (SEM) images (Figure 1) and statistic histograms(Figure S1 in the Supporting Information), Li nuclei sizedecreases significantly and Li nucleation density increasesremarkably with the increase of current density at the fixedtemperature, which is well consistent with previousresearch.[9a] Notably, we discovered a thermal-phenomenapertaining to Li nucleation behavior. By elevating temper-ature from �20 8C to 60 8C, the Li nuclei show enlarged sizeand decreased density at the same current density. For

[*] K. Yan, S. Zhao, Dr. D. Zhou, Dr. B. Sun, Prof. G. WangCentre for Clean Energy TechnologySchool of Mathematical and Physical Sciences, Faculty of ScienceUniversity of Technology SydneySydney, NSW 2007 (Australia)E-mail: bing.sun@uts.edu.au

guoxiu.wang@uts.edu.au

Dr. J. Wang, Prof. Y. CuiDepartment of Materials Science and EngineeringStanford UniversityStanford, CA 94305 (USA)

Prof. Y. CuiSLAC National Accelerator LaboratoryStanford Institute for Materials and Energy Sciences2575 Sand Hill Road, Menlo Park, CA 94025 (USA)E-mail: yicui@stanford.edu

Supporting information and the ORCID identification number(s) forthe author(s) of this article can be found under:https://doi.org/10.1002/anie.201905251.

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instance, at the current density of 0.05 mAcm�2, Li nuclei arediscrete and compact at 60 8C (Figure 1). While at 20 8C, Linuclei become smaller and denser. As the temperaturefurther decreases to �20 8C, the Li nuclei become evensmaller and more crowded. The statistic histograms moreclearly elucidate the dramatic changes of Li nuclei size andnucleation density (Figure 2a). At 0.05 mAcm�2 and �20 8C,the Li nuclei size and nuclei density are 1.4 mm and 4.0 �106 nuclei cm�2, respectively. In contrast, the nuclei sizeincreases twenty times and the nucleation density drops toone percent as temperature increases from �20 8C to 60 8C.The same tendencies were also observed when we varied thecurrent density (Figure S2). Upon the systematical ex situSEM observations, we identified that high temperaturefavored large and sparse Li nuclei formation. In carbonateelectrolyte (1m LiPF6 in ethylene carbonate/dimethyl carbon-ate (EC/DMC, 1:1 v/v)), we also observed Li deposition layer

became more compact at higher temperature (Figure S3),indicating the universal influence of temperature on Linucleation behavior.

As a conventional method for quantifying electrochemicalnucleation, chronoamperometry has been used to modelheterogeneous nucleation behavior.[10] Therefore, we furtherinvestigated Li nucleation density under the influence oftemperature by chronoamperometry measurements. TypicalLi nucleation curves were obtained by employing threedifferent onset potentials that correspond to three depositioncurrent densities (0.05, 0.5 and 5 mA cm�2; Figure S4). Thewell-defined proportional trend between the current (I) andthe root of time (t1/2) illustrated that Li nucleation behaviorfollowed three-dimensional instantaneous model (Fig-ure S5).[11] In order to eliminating systemic deviation thatcaused by diffusion gradient, we did simulation by introducingdiffusion coefficient and slope value of I–t1/2 curve intonucleation model at a low current density (0.05 mAcm�2).The detailed modeling and simulation are described in thesupporting information. As shown in Figure 2 b, nucleationdensities obtained from both experimental statistic and modelsimulation decrease dramatically with increasing temper-ature, clearly proving the degressive Li nucleation density atascending temperature.

Chronopotentiometry measurements were also conductedto evaluate Li nucleation property. All the voltage–capacityprofiles exhibit voltage dips at the beginning of Li nucleationwhich followed by voltage plateaus (Figure 2c). The valuebetween the bottom of voltage dip and the flat part of voltageplateau represents the Li nucleation overpotential, whichidentifies the degree of lithiophilicity on the current collectorsurface.[12] Li nucleation overpotential significantly decreasedas the temperatures increased from �20 8C to 60 8C, illustrat-ing the lowest nucleation energy barrier and the best

lithiophilicity at 60 8C. Furthermore, the plateausdepict the mass-transfer overpotential, which aremainly determined by the current density and themigration properties of Li ions in electrolyte. Thelowest mass-transfer overpotential was found at 60 8Cat the same current density, indicating the facile Linucleation growth process at high temperature. Theenhanced lithiophilicity facilitated the formation of Liembryos on current collector, and the depressed mass-transfer overpotential further strengthened the nucleigrowth, thus contributing to large Li nuclei size atelevated temperature. In addition, the decreasingtendencies of nucleation overpotential and mass-transfer overpotential with increasing temperaturewere well demonstrated by simulations (Figure 2d,Figure S6,S7), illustrating large Li nuclei induced bythermal elevation.

To better understand the mechanism of Li nucleilayer changes, we conducted in situ optical observa-tion to visualize the critical Li crystallization andnucleation processes. Figure 3a and Supporting Vid-eos S1, S2 show the in vivo Li nucleation growthprocesses at 60 8C and 20 8C at the same currentdensity (0.5 mAcm�2). The videos display that numer-ous Li embryos emerged within transient time (ca.

Figure 1. SEM images of Li nuclei layers at varied current densitiesand temperature conditions with the capacity limitation of0.1 mAhcm�2.

Figure 2. a) Statistic histograms of Li nuclei size and nucleation density for Liplating at 0.05 mAcm�2. b) Change in Li nucleation densities with temperature.c) Chronoamperometric comparison of Li nucleation at varied temperature at0.05 mAcm�2. d) Change in nucleation overpotentials and experimental andsimulated mass-transfer overpotentials with temperature.

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10 s) at both 60 8C and 20 8C, clearly certifying the instanta-neous nucleation procedure as predicted by previous inves-tigations.[13] In the video S1 and S2, Li nuclei generatedconcurrently as the plating profile passed the voltage dip,indicating the necessary overpotential of metallic Li hetero-geneous deposition. The following voltage plateau signified Linuclei growth, which was clearly revealed by the gradualaccretion on Li nuclei size. Larger and sparser Li nuclei wereobserved at 60 8C compared with that at 20 8C from the snapimage at 60 s (Figure 3a). At 60 8C, large Li nuclei graduallygrew up and expanded, and large amounts of interspaces werestill visible at 720 s. Although the growth of Li nuclei wasdistinct at 20 8C, the nuclei overlaps were clearly observedafter 480 s. In situ optical observations successfully correlateSEM observation and simulation analysis, demonstrating thatthe discriminations of Li nucleation were influenced bytemperature from the very beginning.

Accordingly, we proposed the temperature-dependent Linucleation and growth mechanism. As shown in the sche-matics (Figure 3 b), excellent lithiophilicity promotes inter-actions between Li ions in electrolyte and current collector atelevated temperature (e.g. 60 8C). This effect leads to thegathering of large amount of Li ions on the surface of currentcollector, thus resulting in large Li nuclei formation in the

initial stage. Meanwhile, the high mobility of Li ions ensuresswift migration to the separated Li nuclei points. As platingcontinues, large and sparse Li nuclei grow gradually until theyfuse with their neighbors. Ultimately, a compact Li depositionlayer forms after further plating. In contrast, at room temper-ature (e.g. 20 8C), the contact between Li ions and currentcollector is weakened by poor lithiophilicity. Therefore, smallLi nuclei are generated because limited Li ions gathersimultaneously. Meanwhile, sluggish mobility of Li ionscontributes to dense Li nuclei because Li ions are easilycaptured by nearby nuclei points. Inevitability, further Lideposition easily results in the overlap of Li nuclei and thegeneration of Li dendrites. Notably, the Li ions diffusioncoefficients are greatly increased at elevated temperature(Figure S8). The Li ions diffusion coefficient at 60 8C (1.05 �10�5 cm�2 s�1) shows 3 times higher than that at 20 8C (3.4 �10�6 cm�2 s�1), and 17 times higher than that at �20 8C (6.1 �10�7 cm�2 s�1). The migration of Li ions through SEI is alsopromoted according to the significant decrease of chargetransfer resistance (Rct) with the increase of temperature(Figure S9, Table S3). Furthermore, the strengthened Li ionde-solvation ability at high temperature has been demon-strated.[14] As a result, fast Li ions diffusion and migrationabilities and enhanced Li ion de-solvation performancesynergically contribute to large and sparse Li nuclei gener-ation and compact Li deposition layer formation. Thisstrongly supports the temperature-dependent Li nucleationand growth mechanism.

For further investigation, the Li deposition layers withhigh areal capacities at different temperatures were system-atically observed (Figure S10–S13). At 60 8C, the compact andsmooth lithium layer was found at 0.5 mAcm�2 with the arealcapacity of 1 mAh cm�2. Large area of blank Cu foil surfacewas still visible among Li agglomerates (Figure S10). Thisconfirmed that compact and packed Li occupied minimalspace and possessed very low surface area which minimizedSEI formation. After increasing the areal capacities, similarlithium layers were also observed except the hiding of blankCu foil (Figure S11). By contrast, the Li deposition layerformed at 20 8C consisted of large amount of twisted dendriticLi as well as massive interspaces. When the temperature downto �20 8C, thick Li dendrites and more vacancies wereobserved on Li deposition layer. The porous and dendriticLi deposition layers induce increased consumption of electro-lyte and Li due to the SEI formation at 20 8C and �20 8C.Note, the obvious changes of component and nanostructure ofSEI layers at varied temperatures were clearly demonstratedusing Cryo-EM characterization (Figure 3c, d). The SEIformed at 20 8C was an amorphous polymeric interphase,while the SEI formed at 60 8C consisted of an amorphouspolymeric interphase and an inorganic Li2O outer layer. Inaddition, the thickness of SEI layer increases from 17 nm at20 8C to 23 nm at 60 8C.

To evaluate the electrochemical performances of Lianodes at varied temperatures, we tested the Li j jCu halfcells at 0.5 mAcm�2 with the areal capacity of 1 mAhcm�2

(Figure 4a). A quadruple enhancement of cyclability wasobtained by increasing the temperature from 20 8C to 60 8C,and the average Coulombic efficiency at 60 8C was amelio-

Figure 3. a) In situ optical snap images of Li nuclei growth at 60 8Cand 20 8C. b) Schematic illustration of proposed Li nuclei generationand growth mechanism. Cryo-EM images of SEI formed at c) 60 8C andd) 20 8C.

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rated to 98.9% from that of 97.7 % at 20 8C. Furthermore, theelectrochemical performance improvements of half cells ledby temperature elevation showed similar trends at largercurrent densities and higher areal capacities (Figure S14 andS15). Apart from the compact and uniform texture of Lideposition layer, the high Coulombic efficiency and longcycling life at high temperature were further warranted by thethicker multilayered SEI formed at 60 8C, since the stableLi2O layer more effectively passivated the anode. Thecorresponding voltage profiles showed reduced overpoten-tials during Li plating/striping at elevated temperature (Fig-ure 4b and Figure S16), which was attributed to the enhancedLi ion migration ability and reduced electrolyte resistance athigh temperature.

The influence of temperature on the electrochemicalbehaviors of Li anodes were further evaluated using Li j jLisymmetric cells. In Figure 4c, the symmetric cells operated at60 8C exhibits long life span, which is more than double of thatat 20 8C. The lowest overpotential and the best cyclabilitywere also achieved at different current densities at 60 8C(Figure S17). The significantly improved electrochemicalperformances of symmetric cells at elevated temperatureare consistent with the results of Li j jCu half cells. In general,low Coulombic efficiency and poor cyclability of Li anodesare caused by the formation of SEI and the accumulation of“dead” Li upon cycling. Based on the above testing results, weconfirm that high temperature benefits reversible Li plating/stripping, retards the side reaction of SEI formation andeffectively suppresses the accumulation of “dead” Li.

As a proof of concept, we assembled Li j jLi4Ti5O12 (LTO)full cells to examine their thermal characteristics. The anodeswere employed by pre-depositing Li on Cu foil with a fixedcapacity of 5 mA hcm�2. The full cells were tested at0.5 mAcm�2 at 60 8C and 20 8C, respectively. In Figure 4d,the initial discharge energy densities of full cells wereimproved from 233 Whkg�1 to 255 Whkg�1 as the operation

temperature increased from 20 8C to 60 8C. Further-more, the cycle life of full cell was significantlyprolonged, and the energy efficiency was distinctlyenhanced at 60 8C. The improved energy density athigh temperature was contributed by the reduceddischarge overpotentials and increased dischargespecific capacity (Figure S18 and S19). Consideringthat a novel effective device has been reported toimprove the performances of batteries at low temper-ature,[15] we demonstrate the practicability of promot-ing the performances of Li metal-based full cellsefficiently at high temperature.

In conclusion, we discovered the crucial impact oftemperature on the nucleation behavior and electro-chemical performance of Li metal anodes. Ex situ andin situ microscope observations clearly demonstratedthat larger Li nuclei with smaller nucleation densityformed on Cu foil at higher temperature. Theenhanced lithiophilicity and Li-ion migration abilityat elevated temperature were shown to facilitate theformation of large nuclei size with small nucleationdensity. Moreover, we obtained dendrite-free Lideposition layers with an areal capacity as high as

5 mAh cm�2 at 60 8C. The Li j jCu half cells and Li j jLisymmetric cells exhibited long cyclability, high Coulombicefficiency, and low overpotential at high temperature. Inaddition, Li j jLTO full cells delivered outstanding perform-ances at 60 8C, which greatly surpassed that of the full cells at20 8C. Therefore, elevating temperature has been proved to bean efficient and facile method for developing high-perfor-mance Li metal-based batteries. This strategy may also beextended for preventing dendrite growth in other recharge-able metal-based batteries.

Acknowledgements

We gratefully acknowledge the financial support by Austral-ian Research Council (ARC) through ARC DiscoveryProject (DP160104340 and DP170100436) and ARC Discov-ery Early Career Researcher Award (DE180100036). Wethank Linda Xiao for her kind help on microscope operation.K.Y. thanks the financial support from the China ScholarshipCouncil (No. 201606030088).

Conflict of interest

The authors declare no conflict of interest.

Keywords: dendrite-free · ion migration · Li metal anodes ·nucleation and growth · temperature-dependent behavior

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Manuscript received: April 27, 2019Accepted manuscript online: May 30, 2019Version of record online: && &&, &&&&

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Zuschriften

Lithiumbatterien

K. Yan, J. Wang, S. Zhao, D. Zhou,B. Sun,* Y. Cui,*G. Wang* &&&&—&&&&

Temperature-dependent Nucleation andGrowth of Dendrite-Free Lithium MetalAnodes

Elektrodenplattierung : Starke Lithiophilieund schnelle Li+-Wanderung bei erhçhterTemperatur ermçglichen die Bildunggroßer, verstreuter Li-Keime und lieferndamit einen Beitrag zu einer kompaktenund glatten Li-Abscheidungsschicht aufAnoden. So konnten dendritfreie Li-Metallanoden mit exzellenter elek-trochemischer Leistung f�r metall-basierte Batterien erzielt werden.

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