Supplemental Information. Crumpled Graphene Balls Stabilized. Dendrite-free Lithium Metal Anodes

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1 JOUL, Volume 2 Supplemental Information Crumpled Graphene Balls Stabilized Dendrite-free Lithium Metal Anodes Shan Liu, Aoxuan Wang, Qianqian Li, Jinsong Wu, Kevin Chiou, Jiaxing Huang, and Jiayan Luo

2 Supplemental Information Materials Synthesis. GO was prepared by a modified Hummer s method as reported elsewhere 1. 2 mg ml -1 GO dispersion in water with were nebulized by an ultrasonic atomizer to form aerosol droplets, which were carried by N 2 gas at 1L/min to fly through a horizontal tube furnace (tube diameter = 1 in.) preheated at 400 o C. A Teflon filter was placed at the exhaust to collect the crumpled graphene particles. Then the sample was placed in a tube furnace and heated under Ar at 800 o C for 1 hr (ramping rate of 5 o C/min). Characterization. SEM (Hitachi S4800, Japan) operated at 5.0 kv and TEM (JEOL, Japan) operated at 200 kv were employed to characterize the morphology of Li deposition on crumpled graphene balls anode and Cu foil anode. To transfer the used Li for characterization, after Li was electrodeposited onto CGB/Cu, the cells were opened in the Ar filled glove box and the electrodes were rinsed with DOL and dried. Electrodes were mounted onto SEM stages and sealed in Ar-filled transfer vessels for immediate SEM observation. Unavoidable contact with air was brief, and may contribute to some slight surface features on the Li metal seen in SEM images. Nitrogen adsorption/desorption isotherms were obtained using a Belsorp-Mini instrument (BEL, Japan). The pore size distributions were calculated using the density functional theory method from the adsorption branches of the isotherms. In-situ TEM observation. A Cu rod is used as the sample holder with a small amount of crumpled graphene balls dispersed on its tip and the other is a W probe scratched by Li metal strip driven by Piezo-motor capable of 3-D positioning. A layer of Li x O was grown on the surface of Li metal when exposed to air for a few second during the holder transferring and acted as a solid electrolyte for the nano-cell Li batteries. Electrochemistry. The as-obtained crumpled graphene balls and polyvinylidene fluoride binder (PVDF) (mass ratio of crumpled graphene balls:pvdf = 9:1) were mixed into a slurry by magnetic stirring in N-methylpyrrolidone for 24 hr. Then the slurry was coated onto Cu foil and dried in a vacuum drying oven at 60 o C for 6 hr. The foil was punched into disks with a diameter of 12 mm as the working electrode. The loading mass of crumpled graphene balls approximately 0.56 mg cm -2, corresponding to the average electrode thickness of 8 μm. The mass loading for 40 and 120 μm is approximately 2.3 and 7.0 mg cm -2, respectively. The crumpled graphene balls electrodes were assembled in 2032-type coin cells with Li metal as the reference and counter electrode. The electrolyte was 1 M lithium bis(trifluoromethane)sulfonamide (LiTFSI) in 1,3-dioxolane /1,2-dimethoxyethane (DOL/DME, 1:1 by volume, 30 μl, Sigma Aldrich) with 1 wt% LiNO 3 additives. Pretreatment of the working electrode was achieved by cycling the battery between 0 and 2 V for 10 cycles. The electrode was then tested by depositing and dissolving a controlled amount of Li at different current densities. To calculated the specific Li storage capacity, the electrode with crumbled graphene balls loading mass of approximately 0.56 mg cm -2, corresponding to the average electrode thickness of 8 μm. In this case, the maximum amount of Li deposition is 0.75 ma hr cm -2, So the specific Li storage capacity of crumpled balls is 0.75 ma hr cm -2 /0.56 mg cm -2 *103 = 1344 ma hr g -1. To test Coulombic efficiency, a fixed amount of Li was deposited on crumpled graphene balls/cu electrode and then stripped

3 away up to 1.2 V at various current densities for each cycle. EIS measurements were obtained over the frequency range of 0.1 Hz to 100 KHz with amplitude of 5 mv using a CHI 660 electrochemical workstation. To test the CGB@Li anode in a full cell, LiFePO 4 (MTI, Corp) with an areal capacity of ~ 1 ma hr cm -2 was used as cathode material. The LiFePO 4 electrode was prepared by mixing LiFePO 4, Super P, polyvinylidene difluoride (PVDF) in the ratio of 8:1:1 with N-methyl-2-pyrrolidone as the solvent. The loading mass of the active material was ~8 mg. The CGB@Li anode was CGB deposited with ~ 1 ma hr cm -2 of Li. The cathode/anode capacity ratio = 1:1.

4 Table S1. Comparison of crumpled graphene balls with various porous Cu host materials. The date is from the literature and corresponding calculation. Host materials Density (g cm -3 ) Pore size Free volume Reference 3D Cu μm 22.0% Nat. Commun., 2015, 6, 8058 Cu Nanowire membrane μm 83.9% Nano Lett. 2016,16, 4431 De-alloyed Cu μm 36.0% Adv. Mater., 2016, 28, 6932 Crumpled graphene balls μm 75.3% This work Calculation: The density and the porosity factor of Cu Nanowire membrane is 8.9 g cm -3 and 83.9 %, respectively. So the density of Cu Nanowire membrane is 8.9 g cm -3 x 16.1% = 1.43 g cm -3 ; the free volume of De-alloyed Cu is 36%, so the density of De-alloyed Cu is 8.9 g cm -3 x 64% = 5.7 g cm -3 ; the free volume of 3D Cu is 22%, so the density of 3D Cu is 8.9 g cm -3 x 78% = 6.94 g cm -3. These data are from the cited references.

5 Table 2. Scaffolds for Li metal anodes. Scaffold Thickness (μm) Thickness increase Current (ma cm -2 ) Capacity (ma hr cm -2 ) Coulombic efficiency (%) Electrolyte 3D Cu M LiTFSI DME/DOL De-alloyed Cu ~97 1 M LiTFSI DME/DOL, 1% LiNO 3 3D glass fiber Indidudual M LiTFSI cloth fiber: 10 μm DME/DOL, 2% LiNO 3 Hollow carbon M LiPF 6 with Au NPs EC/DEC Graphene M LiFSI in CNT DME Unstacked M LiTFSI graphene DME/DOL N-doped graphene Carbon coated Ni foam Cu nanowire network Graphitized carbon fibers Crumpled graphene balls M LiTFSI DME/DOL, 5% LiNO 3 Ni pore size: 150 μm, Carbon: 3-4 mg cm ~98 1 M LiTFSI DME/DOL, 1% LiNO M LiTFSI DME/DOL, 1% LiNO 3, 5uM Li 2 S M LiTFSI DME/DOL, 1% LiNO M LiTFSI ~ DME/DOL, 1% LiNO 3 Reference Nat. Commun., 2015, 6, 8058 Adv. Mater., 2016, 28, 6932 Adv. Mater., 2016, 28, 2888 Nat. Energy, 2016, 1, ACS Nano, 2017, 11, 6362 Adv.Mater. 2016, 28, 2155 Angew. Chem., 2017, 56, 7764 J. Am. Chem. Soc., 2017, 139, 5916 Nano Lett., 2016, 16, 4431 Adv. Mater., 2017, This work

6 Figure S1. FTIR spectra of GO and CGB.

7 Figure S2. Deconvoluted XPS spectra of crumple graphene balls, (A) C 1s and (B) O 1s of CGB.

8 Figure. S3. Top view (A) and cross section (B) SEM images of the crumpled graphene balls electrode.

9 Figure S4. TEM snapshot images taken during the lithiation process in a crumple graphene balls. (A) Pristine of crumple graphene balls and (B-F) Li deposition process onto crumple graphene balls taken at different time. Inset of (F) show the electron energy loss spectroscopy of Li@CGB. Scale bars of A-F: 50 nm.

10 Figure. S5. SEM of crumpled graphene balls from 8 μm thick crumpled graphene balls electrode after depositing 0.75 ma hr cm -2 (A) and 1 ma hr cm -2 (B) of Li.

11 Figure. S6. Representative top-view SEM images 8 μm thick CGB electrode coated Cu after depositing (A) 0.1 ma hr cm -2, (B) 0.5 ma hr cm -2, (C) 0.75 ma hr cm -2, (D) 1 ma hr cm -2 and then dissolving (E) 0.5 ma cm -2 of Li and (F) after 30 cycles. The Li deposition/dissolution states in (A-F) are indicated in (G) galvanostatic discharge/charge voltage profiles at a current density of 1 ma cm -2.

12 Figure. S7. Typical voltage profile during initialization process. The batteries were first cycled at 0-2 V (vs. Li + /Li) at 0.5 ma cm -2 for ten cycles for initialization prior to further electrochemical procedure. The Li storage capacity of crumpled graphene balls electrode between 0-2 V is ~120 ma hr g -1 (without first cycle).

13 Figure S8. Voltage hysteresis of the Li plating/stripping on planar Cu and CGB for 0.5 ma hr cm -2. The current density is 0.5 ma cm -2.

14 Figure. S9. Columbic efficiency of crumpled graphene balls electrodes and the controlled Cu electrodes with different Li deposited amount at different current density: (A) plating 2 ma hr cm -2 with a current density 1.0 ma cm -2, (B) planting 3.0 ma hr cm -2 with a current density 1.0 ma cm -2, (C) planting 12.0 ma hr cm -2 with a current density 1.0 ma cm -2, (D) planting 8.0 ma hr cm -2 with a current density 2.0 ma cm -2, (E) planting 1.0 ma hr cm -2 with a current density 3.0 ma cm -2, (F) planting 6.0 ma hr cm -2 with a current density 3.0 ma cm -2.

15 Figure S10. Coulombic efficiency of planar Cu and CGB with (A) plating 0.5 ma hr cm -2 with current density 0.5 ma cm -2 and (B) plating 1.0 ma hr cm -2 with current density 1.0 ma hr cm -2. The stripping upper voltage is 1.2 V. The electrolyte is 1 M LiPF 6 in EC/DEC.

16 Figure. S11. Columbic efficiency of different electrodes with Li deposited amount of 1 ma hr cm -2 at a current rate of 1 ma cm -2.

17 Figure. S12. N 2 adsorption-desorption isotherm of graphene aerogel and pore size distribution (inset).

18 Figure. S13. SEM of graphene aerogel (A,C) and super P (B,D) before and after Li deposition.

19 Figure. S14. EIS spectra of Li plated on crumpled graphene ball electrodes and the controlled planar Cu electrodes after 1st and 10th galvanostatic cycles.

20 Figure S15. Full cell Performance. (A) Typical galvanostatic profiles of and Li foil/lfp full cells at 0.2 C (according cathode capacity). Inset: enlarged profiles exhibiting the polarization. (B) The charge/discharge profiles of the full cells of CGB@Li/LFP at difference cycle at 0.5 C. (C) Cycling performance of the full cells with three different anodes at 0.5 C. (D) The rate performance of the full cells with three different anodes.

21 References 1. William, S., Hummers, J., Offeman. R. E. (1958). Preparation of graphitic oxide J. Am. Chem. Soc. 80, 1339.

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