Atomic structure of sensitive battery materials and interfaces revealed by cryo–electron microscopy by Yuzhang Li, Yanbin Li, Allen Pei, Kai Yan, Yongming.

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Presentation transcript:

Atomic structure of sensitive battery materials and interfaces revealed by cryo–electron microscopy by Yuzhang Li, Yanbin Li, Allen Pei, Kai Yan, Yongming Sun, Chun-Lan Wu, Lydia-Marie Joubert, Richard Chin, Ai Leen Koh, Yi Yu, John Perrino, Benjamin Butz, Steven Chu, and Yi Cui Science Volume 358(6362):506-510 October 27, 2017 Copyright © 2017 The Authors, some rights reserved; exclusive licensee American Association for the Advancement of Science. No claim to original U.S. Government Works

Fig. 1 Preserving and stabilizing Li metal by cryo-EM. Preserving and stabilizing Li metal by cryo-EM. (A) Li metal dendrites are electrochemically deposited directly onto a Cu TEM grid and then plunged into liquid nitrogen after battery disassembly. (B) The specimen is then placed onto the cryo-TEM holder while still immersed in liquid nitrogen and isolated from the environment by a closed shutter. During insertion into the TEM column, temperatures do not increase above –170°C, and the shutter prevents air exposure to the Li metal. Yuzhang Li et al. Science 2017;358:506-510 Copyright © 2017 The Authors, some rights reserved; exclusive licensee American Association for the Advancement of Science. No claim to original U.S. Government Works

Fig. 2 Atomic-resolution TEM of Li metal dendrites. Atomic-resolution TEM of Li metal dendrites. (A) Cryo-EM image of Li metal dendrites. Electron dose rate <1 e Å–2 s–. (B) Standard TEM image of Li metal dendrite with ~1 s air exposure at room temperature. Inset, corresponding SAED pattern. (C) Standard TEM image of the dendrite from (B) after exposure to electron dose rate of ~500 e Å–2 s–1 for ~1 s. The three holes were formed immediately after this exposure. (D) Time-lapse images of Li dendrite from the green-outlined area in (A) after continuous electron-beam irradiation at a dose rate of ~50 e Å–2 s–1. (E and H) TEM images of Li metal dendrites growing along the <211> (E) and <110> (H) directions. Inset, corresponding SAED pattern showing that the dendrites are single-crystalline. Electron dose rate <1 e Å–2 s–1 for ~30 s. (F and I) Magnified image of boxed regions in red (F) and blue (I) from (E) and (H), respectively, showing the Li metal lattice at high resolution. Electron dose rate ~1000 e Å–2 s–1 for ~30 s. (G and J) Atomic-resolution TEM images resolving individual Li atoms along the [111] (G) and [001] (J) zone axes. Electron dose rate ~1000 e Å–2 s–1 for ~30 s. Yuzhang Li et al. Science 2017;358:506-510 Copyright © 2017 The Authors, some rights reserved; exclusive licensee American Association for the Advancement of Science. No claim to original U.S. Government Works

Fig. 3 Faceting behavior of Li metal dendrites. Faceting behavior of Li metal dendrites. (A to C) Li metal dendrites and their corresponding SAED patterns (insets) growing along <111> (A), <110> (B), and <211> (C). Electron dose rate <1 e Å–2 s–1 for ~30 s. (D) Statistics showing preferred growth direction is along <111>. (E) Standard SEM image of Li metal dendrites after brief exposure to air. Facets cannot be observed because of corrosion in air. (F) Cryo-SEM image of Li metal dendrites. Facet morphology is preserved by the cryo-transfer method. (G to I) Diagram of triangular (G), hexagonal (H), and rectangular (I) cross-sectional structures for dendrites, exhibiting clear faceting behavior. The low-energy (110) facet should be exposed according to thermodynamic considerations. Insets, diagrams of atomic projections from various zone axes. The shapes correspond to the cross-sectional structures observed in cryo-SEM. Yuzhang Li et al. Science 2017;358:506-510 Copyright © 2017 The Authors, some rights reserved; exclusive licensee American Association for the Advancement of Science. No claim to original U.S. Government Works

Fig. 4 Atomic-resolution TEM of kinked Li metal dendrite and SEI interface. Atomic-resolution TEM of kinked Li metal dendrite and SEI interface. (A) TEM image of kinked Li metal dendrite that changes from a <211> to <110> and back to <211> growth direction. Inset shows corresponding SAED pattern. Electron dose rate <1 e Å–2 s–1 for ~30 s. The dashed yellow lines indicate change in growth direction. (B and C) Magnified images of red region I (B) and blue region II (C) outlined in (A) showing both kinks at high resolution. Electron dose rate ~1000 e Å–2 s–1 for ~30 s. (D) Schematic of the single-crystalline nature of the kink. (E) Atomic-resolution image of green region III outlined in (A) revealing the interface between Li metal and the SEI. The lattice spacings of small crystalline grains of inorganic material dispersed throughout the amorphous film can be matched to Li carbonate (Li2CO3, orange circles) and Li oxide (Li2O, red circles). Electron dose rate ~1000 e Å–2 s–1 for ~30 s. (F) Schematic of the observed mosaic-type structure formed on Li dendrites in EC-DEC electrolyte. (G) Integrated pixel intensities of Li oxide (red) and Li carbonate (orange) lattice. The peaks and valleys represent rows of atoms and the gaps, respectively. a.u., arbitrary units. (H) Atomic-resolution image of the SEI formed in FEC electrolyte. Electron dose rate ~1000 e Å–2 s–1 for ~30 s. (I) Schematic of the observed multilayered structure formed on Li dendrites in FEC electrolyte. Yuzhang Li et al. Science 2017;358:506-510 Copyright © 2017 The Authors, some rights reserved; exclusive licensee American Association for the Advancement of Science. No claim to original U.S. Government Works