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1 In the format provided by the authors and unedited. DOI: /NNANO Revealing the reaction mechanisms of Li-O 2 batteries using environmental transmission electron microscopy Langli Luo, Bin Liu, Shidong Song, Wu Xu, Ji-Guang Zhang, and Chongmin Wang * *Correspondence to: Chongmin.Wang@pnnl.gov 1. Description of the Supplementary Videos Supplementary Video S1. In situ HAADF STEM observation of the morphological evolution of the reaction product upon discharging/charging of the Li-O 2 battery, featuring the formation of hollow spherical particle during discharging (oxygen reduction reaction (ORR)) and shrinkage of the hollow sphere upon charging (oxygen evolution reaction). The frame speed is 16 times fast of the real time. Supplementary Video S2. In situ TEM observation of the morphological evolution of the reaction product upon discharging/charging of the Li-O2 battery, featuring the formation of hollow spherical particle during discharging (oxygen reduction reaction (ORR)) and shrinkage of the hollow sphere upon charging (oxygen evolution reaction). The frame speed is 16 times fast of the real time. Supplementary Video S3. In situ TEM observation illustrating the growth and decomposition of the discharging product as conformal coatings on the carbon nanotube surface. The frame speed is 16 times fast of the real time. Supplementary Video S4. In situ STEM observation of the decomposition process of the discharging product formed as a conformal coating on carbon nanotube surface, revealing the decomposition of Li 2 O 2 proceeds through nucleation of smaller particles accompanying O 2 release. The frame speed is 16 times fast of the real time. NATURE NANOTECHNOLOGY 1

2 2. Supplementary Figures Figure S1. Morphology of RuO 2 decorated CNTs as cathode in Li-O 2 battery. HRTEM images shows the structure of RuO 2 decorated CNTs. The RuO 2 has both well crystalline structure (inset) and quasi-amorphous structure. NATURE NANOTECHNOLOGY 2

3 Figure S2. Spatial correlation of Li 2 O and Li 2 O 2 phases in one hollow spherical particle. a, SAED pattern of a hollow sphere and b, corresponded dark-field TEM image by choosing only the spot of Li 2 O 2 phase circulated in a shows the Li 2 O 2 phase is presented in center part (brighter contrast) of the hollow sphere while coated by surface Li 2 O layer (dark contrast). c, SAED pattern of a hollow sphere (inset) during discharge shows Li 2 O+Li 2 O 2 phases while d, a decomposed hollow sphere (inset) during charge shows only Li 2 O phase. NATURE NANOTECHNOLOGY 3

4 Figure S3. Formation of hollow spherical particles in various sites on CNTs/RuO 2 cathode. Bright-field TEM images taken during discharging Li-O 2 nano-battery show different formation sites of discharging product: a. at both of the three-phase boundary (lower right) and the CNTs/current collector interface (upper left); b. at the junction of two CNTs without RuO 2 ; c. at the middle of RuO 2 decorated CNT. NATURE NANOTECHNOLOGY 4

5 3. Evaluation of beam effect The beam dose rate for TEM is in the range of 10-4 A/cm 2 to 10-3 A/cm 2, which is typically in the low dose range of imaging. Further, to evaluate the beam effect, we have done control experiment that blanking the beam during the reaction, and found there is no observable effect of beam on the discharging/charging process. NATURE NANOTECHNOLOGY 5

6 4. Electrochemical lithiation of RuO 2 Upon discharging, a negative bias was applied to drive Li + to react with O 2 on CNTs/RuO 2 surface. Before the formation of Li-O reaction product (e.g. hollow spherical particles and conformal coatings), the RuO 2 was electrochemically lithiated and converted to ultrafine Ru NPs embedded in Li 2 O matrix as shown in the image of 40s in Fig. 2, which is the working morphology of the electrocatalyst during the following charging/discharging reactions. Prelithiation has been used to prepare cathode for high performance Li-O 2 battery 1. Figure S4. Electrochemical lithiation of RuO 2 on CNTs. Time-lapse HRTEM images show the initial electrochemical lithiation of RuO 2 during the Li-O 2 reaction. Through conversion reaction: RuO Li + + 4e - Ru + 2Li 2 O, the RuO 2 phase has been converted to ultrafine Ru nanoparticles embedded in Li 2 O matrix as shown in the image of 40s with the inset of SAD pattern. NATURE NANOTECHNOLOGY 6

7 5. Phase identification of discharging product during Li-O 2 reaction In situ SAED analysis monitors the phase change of the growing reaction product during discharging process. Hence, the orientation and size of the selected area were rapidly changing, leading to cases of missing and/or rotation of diffraction spots as well as the overlay of two or more diffraction patterns from multiple particles. However, the lattice space of each plane can be accurtately measured and correlated to each phase. Fig. 5a and b show the simulated single crystal LiO 2 and polycrystalline Li 2 O 2 and Li 2 O phases, respectively. Fig. 5c-f show a series of time-lapse in situ SAED patterns taken during discharing process of the Li-O 2 battery and detailed indexing of the diffraction patterns were given. It is noted that Fig. 5d-f were also shown in Fig. 3 in main text but without detailed indexing. NATURE NANOTECHNOLOGY 7

8 Figure S5. Phase identification of LiO 2 and Li 2 O 2. a. simulated single crystal diffraction pattern of LiO 2 from zone axis (001). b. rotational average of Li 2 O 2 and Li 2 O phase. c-f. Timelapse in situ SAED patterns of the growing discharging product show the phase evolution of LiO 2, Li 2 O 2 and Li 2 O. NATURE NANOTECHNOLOGY 8

9 6. Control experiment of Li-O 2 reaction on bare CNT We use pure CNTs without catalyst as cathode for in situ battery experiments to compare with the case of CNTs/RuO 2 cathode. Fig. 6a shows the typical morphology of both hollow spherical particles and conformal coating as discharging product. The inset of SAED pattern confirms the Li 2 O 2 and Li 2 O as the final phase of these hollow spheres. It is noted that hollow spheres were presented on both three-phase point and the cathode/current collector interface as described in the main text. Fig. 6b and c show typical morphology of conformal coating on the surface of CNTs after discharging and charging process. The thickness of this layer of discharging product slightly decreased after charging as indicated by white arrows. Fig. 6d-f show the SAED patterns of phase evolution on the surface of CNTs, i.e. pristine CNTs, CNTs after 1 st discharging and 1 st charging, respectively. Similar as the case of Li-O 2 reaction on CNTs/RuO 2, the discharging product has Li 2 O 2 and Li 2 O phase in conformal coating layer. As shown above, the catalyst RuO 2 has little effect on the formation of large hollow spherical particles during discharging. NATURE NANOTECHNOLOGY 9

10 Figure S6. Controlled Experiments on bare CNTs. a. Overall typical morphology of discharging product on the surface of bare CNTs. The inset is the SAED pattern from the hollow spheres. b and c. Morphology of the conformal layer of discharging product on CNT surface during discharging and charging process, respectively. d-f, SAED patterns show phase evolution on the CNTs surface, i.e. pristine CNTs, CNTs after 1 st discharging and 1 st charging, respectively. NATURE NANOTECHNOLOGY 10

11 7. Control experiment of Li-H 2 O reaction on CNT/RuO 2 To confirm the right Li-O chemistry in the nano-battery built in ETEM, we switched gas environment from pure O 2 to H 2 O to see the change of discharging product. Meanwhile, Li-H 2 O chemistry is critical for aqueous Li-O 2 battery. With the environment of water vapor (0.01mbar), we have found no hollow spherical particles formation but only conformal coatings deposited on the surface of CNTs. Fig. 7a shows typical morphology of the conformal coating with a thickness of ~11.2 nm and the lattice of the CNT is clearly seen. SAED pattern in Fig. 7b reveals the phase of this conformal coating that the final discharging product changed from Li 2 O+Li 2 O 2 to Li 2 O+Li 2 CO 3 +LiOH as labeled. These observations indicate that the typical hollow spheres only form in the O 2 environment as a result of O 2 releasing through disproportion reaction, which justifies our proposed mechanism. NATURE NANOTECHNOLOGY 11

12 Figure S7. Controlled Experiments in H 2 O environment. a. Typical morphology of the conformal coating on CNTs/RuO 2 as discharging product. b. SAED analysis of the discharging product shows the presence of Li 2 O, Li 2 CO 3 and LiOH phases. NATURE NANOTECHNOLOGY 12

13 8. Calculation of O 2 volume during disproportionation reaction Assume a LiO 2 nucleus has a dimension of nm, it has 1000 nm 3 ~ 10 6 A 3 / A 3 = unit cell. 1 unit cell has 2Li and 4O, then it is /N A = mol 2 mol LiO 2 generate 1 mol O 2 gas, that is mol O 2 gas, the O 2 density is g/l, O 2 released has a volume of /1.429= L= nm 3 = nm 3, equivalent to a sphere of d=107.2 nm. NATURE NANOTECHNOLOGY 13

14 9. Ex-situ Electrochemical test of CNTs/RuO 2 air electrode We have assembled a Li-O 2 cell using CNTs/RuO 2 as air electrode same as our in situ TEM tests. The electrolyte used is 200 ul of 1M LiTf-TEGDME and the mass loading of RuO 2 /CNTs is 0.45 mg cm -2. First two cycles discharge/charge profiles of CNTs/RuO 2 air electrode with a current density of 0.1 macm -2 are shown below. Figure S8. Ex-situ Electrochemical test of CNTs/RuO 2 air electrode. First two cycles discharge/charge profiles of CNTs/RuO 2 air electrode with a current density of 0.1 macm -2. The electrolyte used is 200 ul of 1M LiTf-TEGDME and the mass loading of RuO 2 /CNTs is 0.45 mg cm -2. References 1 Liu, B. et al. Electrochemically Formed Ultrafine Metal Oxide Nanocatalysts for High- Performance Lithium Oxygen Batteries. Nano Lett. 16, (2016). NATURE NANOTECHNOLOGY 14

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