In situ transmission electron microscopy and spectroscopy studies of rechargeable batteries under dynamic operating conditions: A retrospective and perspective view

Journal of Materials Research

Volumn 30, Issue 3, 2015, Pages 326-339

  Wang, Chong Min ^a  

^a PACIFIC NORTHWEST NATIONAL LABORATORY   (United States)

Author keywords

energy storage; In situ TEM; lithium ion battery; rechargeable battery

Indexed keywords

ELECTRIC BATTERIES; ENERGY STORAGE; HIGH RESOLUTION TRANSMISSION ELECTRON MICROSCOPY; IN SITU PROCESSING; LITHIUM ALLOYS; LITHIUM-ION BATTERIES; TRANSMISSION ELECTRON MICROSCOPY;

ABERRATION CORRECTED TEM; IMAGING RESOLUTIONS; IN-SITU TEM; IN-SITU TRANSMISSION ELECTRON MICROSCOPIES; MICRO-FABRICATION TECHNIQUES; NANO-SCALE OBJECTS; OPERATING CONDITION; SCIENTIFIC DISCOVERY;

SECONDARY BATTERIES;

EID: 85027944510     PISSN: 08842914     EISSN: 20445326     Source Type: Journal    
DOI: 10.1557/jmr.2014.281     Document Type: Review

References (131)

1. M. Haider, S. Uhlemann, E. Schwan, H. Rose, B. Kabius, and K. Urban: Electron microscopy image enhanced. Nature 392 (6678), 768 (1998).
2. O. L. Krivanek, N. Dellby, and A. R. Lupini: Towards sub-angstrom electron beams. Ultramicroscopy 78, 1 (1999).
3. O. L. Krivanek, P. D. Nellist, N. Dellby, M. F. Murfitt, and Z. Szilagyi: Towards sub-0. 5 Å electron beams. Ultramicroscopy 96, 229 (2003).
4. H. Mueller, S. Uhlemann, P. Hartel, and M. Haider: Advancing the hexapole Cs-corrector for the scanning transmission electron microscope. Microsc. Microanal. 12, 442 (2006).
5. P. E. Batson, N. Dellby, and O. L. Krivanek: Sub-ångstrom resolution using aberration corrected electron optics. Nature 418, 617 (2002).
6. C. Kisielowskia, B. Freitaga, M. Bischoffa, H. van Lina, S. Lazara, G. Knippelsa, P. Tiemeijera, M. van der Stama, S. von Harracha, M. Stekelenburga, M. Haidera, S. Uhlemanna, H. Müllera, P. Hartela, B. Kabiusa, D. Millera, I. Petrova, E. A. Olsona, T. Doncheva, E. A. Kenika, A. R. Lupinia, J. Bentleya, S. J. Pennycooka, I. M. Andersona, A. M. Minora, A. K. Schmida, T. Dudena, V. Radmilovica, Q. M. Ramassea, M. Watanabea, R. Ernia, E. A. Stacha, P. Denesa, and U. Dahme: Detection of single atoms and buried defects in three dimensions by aberration-corrected electron microscope with 0. 5-Å information limit. Microsc. Microanal. 14, 469 (2008).
7. H. Sawada, F. Hosokawa, T. Kaneyama, T. Ishizawa, M. Terao, M. Kawazoe, T. Sannomiya, T. Tomita, Y. Kondo, T. Tanaka, Y. Oshima, Y. Tanishiro, N. Yamamoto, and K. Takayanagi: Achieving 63 pm resolution in scanning transmission electron microscope with spherical aberration corrector. Jpn. J. Appl. Phys. 46, L568 (2007).
8. K. W. Urban: Is science prepared for atomic resolution electron microscopy? Nat. Mater. 8, 260 (2009).
9. O. L. Krivanek, G. J. Corbin, N. Dellby, B. F. Elston, R. J. Keyse, M. F. Murfitt, C. S. Own, Z. S. Szilagyi, and J. W. Woodruff: An electron microscope for the aberration-corrected era. Ultramicroscopy 108, 179 (2007).
10. D. A. Muller, L. Fitting Kourkoutis, M. F. Murfitt, J. H. Song, H. Y. Hwang, J. Silcox, N. Dellby, and O. L. Krivanek: Atomic-scale chemical imaging of composition and bonding by aberration-corrected microscopy. Science 319, 1073 (2008).
11. D. A. Muller: Structure and bonding at the atomic scale by scanning transmission electron microscopy. Nat. Mater. 8, 263 (2009).
12. C. L. Jia, M. Lentzen, and K. Urban: Atomic-resolution imaging of oxygen in perovskite ceramics. Science 299, 870 (2003).
13. P. D. Nellist and S. J. Pennycook: Direct imaging of the atomic configuration of ultradispersed catalysts. Science 274, 413 (1996).
14. C-L. Jia, S-B. Mi, K. Urban, I. Vrejoiu, M. Alexe, and D. Hesse: Atomic-scale study of electric dipoles near charged and uncharged domain walls in ferroelectric films. Nat. Mater. 7, 57 (2008).
15. A. R. Harutyunyan, G. G. Chen, T. M. Paronyan, E. M. Pigos, O. A. Kuznetsov, K. Hewaparakrama, S. M. Kim, D. Zakharov, E. A. Stach, and G. U. Sumanasekera: Preferential growth of single-walled carbon nanotubes with metallic conductivity. Science 326, 116 (2009).
16. B. J. Kim, J. Tersoff, S. Kodambaka, M. C. Reuter, E. A. Stach, and F. M. Ross: Kinetics of individual nucleation events observed in nanoscale vapor-liquid-solid growth. Science 322, 1070 (2008).
17. P. L. Hansen, J. B. Wagner, S. Helveg, J. R. Rostrup-Nielsen, B. S. Clausen, and H. Topsoe: Atom-resolved imaging of dynamic shape changes in supported copper nanocrystals. Science 295, 2053 (2002).
18. P. Nolte, A. Stierle, N. Y. Jin-Phillipp, N. Kasper, T. U. Schulli, and H. Dosch: Shape changes of supported Rh nanoparticles during oxidation and reduction cycles. Science 321, 1654 (2008).
19. H. Yoshida, Y. Kuwauchi, J. R. Jinschek, K. Sun, S. Tanaka, M. Kohyama, S. Shimada, M. Haruta, and S. Takeda: Visualizing gas molecules interacting with supported nanoparticulate catalysts at reaction conditions. Science 335, 317 (2012).
20. Z. W. Shan, R. K. Mishra, S. A. S. Asif, O. L. Warren, and A. M. Minor: Mechanical annealing and source-limited deformation in submicrometre-diameter Ni crystals. Nat. Mater. 7, 115 (2008).
21. A. M. Minor, S. A. S. Asif, Z. W. Shan, E. A. Stach, E. Cyrankowski, T. J. Wyrobek, and O. L. Warren: A new view of the onset of plasticity during the nanoindentation of aluminium. Nat. Mater. 5, 697 (2006).
22. H. M. Zheng, R. K. Smith, Y. W. Jun, C. Kisielowski, U. Dahmen, and A. P. Alivisatos: Observation of single colloidal platinum nanocrystal growth trajectories. Science 324, 1309 (2009).
23. H. G. Liao, L. K. Cui, S. Whitelam, and H. M. Zheng: Real-time imaging of Pt3Fe nanorod growth in solution. Science 336, 1011 (2012).
24. D. Li, M. H. Nielsen, J. R. I. Lee, C. Frandsen, J. F. Banfield, and J. J. De Yoreo: Direction-specific interactions control crystal growth by oriented attachment. Science 336, 1014 (2012).
25. M. J. Williamson, R. M. Tromp, P. M. Vereecken, R. Hull, and F. M. Ross: Dynamic microscopy of nanoscale cluster growth at the solid-liquid interface. Nat. Mater. 2, 532 (2003).
26. N. de Jonge, D. B. Peckys, G. J. Kremers, and D. W. Piston: Electron microscopy of whole cells in liquid with nanometer resolution. Proc. Natl. Acad. Sci. 106, 2159 (2009).
27. B. Kang and G. Ceder: Battery materials for ultrafast charging and discharging. Nature 458, 190 (2009).
28. P. Poizot, S. Laruelle, S. Grugeon, L. Dupont, and J. M. Tarascon: Nano-sized transition-metal oxides as negative-electrode materials for lithium-ion batteries. Nature 407, 496 (2000).
29. B. Scrosati: Challenge of portable power. Nature 373, 557 (1995).
30. J. M. Tarascon and M. Armand: Issues and challenges facing rechargeable lithium batteries. Nature 414, 359 (2001).
31. M. Gu, I. Belharouak, A. Genc, Z. Wang, D. Wang, K. Amine, F. Gao, G. Zhou, S. Thevuthasan, D. R. Baer, J-G. Zhang, N. D. Browning, J. Liu, and C. Wang: Conflicting roles of nickel in controlling cathode performance in lithium ion batteries. Nano Lett. 12, 5186 (2012).
32. R. Retoux, T. Brousse, and D. M. Schleich: High-resolution electron microscopy investigation of capacity fade in SnO2 electrodes for lithium-ion batteries. J. Electrochem. Soc. 146, 2472 (1999).
33. C. Delmas, M. Maccario, L. Croguennec, F. L. Cras, and F. Weill: Lithium deintercalation in LiFePO4 nanoparticles via a domino-cascade model. Nat. Mater. 7, 665 (2008).
34. P. Gibot, M. Casas-Cabanas, L. Laffont, S. Levasseur, P. Carlach, S. Hamelet, J. M. Tarascon, and C. Masquelier: Room-temperature single-phase li insertion/extraction in nanoscale LixFePO4. Nat. Mater. 77, 741 (2008).
35. G. Y. Chen, X. Y. Song, and T. J. Richardson: Electron microscopy study of the LiFePO4 to FePO4 phase transition. Electrochem. Solid State Lett. 9, A295 (2006).
36. L. Laffont, C. Delacourt, P. Gibot, M. Y. Wu, P. Kooyman, C. Masquelier, and J. Marie Tarascon: Study of the LiFePO4/FePO4 two-phase system by high-resolution electron energy loss spectroscopy. Chem. Mater. 18, 5520 (2006).
37. H. Gabrisch, R. Yazami, and B. Fultz: A transmission electron microscopy study of cycled LiCoO2. J. Power Sources 119, 675 (2003).
38. J. Graetz, C. C. Ahn, R. Yazami, and B. Fultz: An electron energy-loss spectroscopy study of charge compensation in LiNi0. 8Co0. 2O2. J. Phys. Chem. B 107, 2887 (2003).
39. Y. S. Meng, G. Ceder, C. P. Grey, W. S. Yoon, M. Jiang, J. Greger, and Y. Shao-Horn: Cation ordering in layered O3 Li [NixLi1/3-2x/3Mn2/3-x/3]O2 (0 5 x 5 1/2) compounds. Chem. Mater. 17, 2386 (2005).
40. M. T. McDowell and Y. Cui: Single nanostructure electrochemical devices for studying electronic properties and structural changes in lithiated Si nanowires. Adv. Energy Mater. 7, 894 (2011).
41. S. W. Lee, M. T. McDowell, J. W. Choi, and Y. Cui: Anomalous shape changes of silicon nanopillars by electrochemical lithiation. Nano Lett. 11, 3034 (2011).
42. H. Bryngelsson, M. Stjerndahl, T. Gustafsson, and K. Edstrom: How dynamic is the SEI?. J. Power Sources 174, 970 (2007).
43. F. Kong, R. Kostecki, G. Nadeau, X. Song, K. Zaghib, K. Kinoshita, and F. McLarnon: In situ studies of SEI formation. J. Power Sources 97-98, 58 (2001).
44. H. Gabrisch, R. Yazami, and B. Fultz: Charge/discharge simulation of an all-solid-state thin-film battery using a one-dimensional model. Electrochem. Solid State Lett. 56, A111 (2002).
45. S. K. Eswaramoorthy, J. M. Howe, and G. Muralidharan: In-situ determination of the nanoscale chemistry and behavior of solidliquid systems. Science 318, 1437 (2007).
46. R. Dedryvere, H. Martinez, S. Leroy, D. Lemordant, F. Bonhomme, P. Biensan, and D. Gonbeau: Surface film formation on electrodes in a LiCoO2/graphite gell: A step by step XPS study. J. Power Sources 174, 462 (2007).
47. S. I. Nishimura, G. Kobayashi, K. Ohoyama, R. Kanno, M. Yashima, and A. Yamada: Experimental visualization of lithium diffusion in LixFePO4. Nat. Mater. 7, 707 (2008).
48. V. Mauchamp, P. Moreau, L. Moncondut, M. L. Doublet, F. Boucher, and G. Ouvrard: Determination of lithium insertion sites in LixTiP4 (x5 2-11) by electron energy-loss spectroscopy. J. Phys. Chem. C 111, 3996 (2007).
49. A. Brazier, L. Dupont, L. Dantras-Laffront, N. Kuwata, J. Kawamura, and J. M. Tarascon: First cross-section observation of an all solid-state lithium-ion "nanobattery" by transmission electron microscopy. Chem. Mater. 20, 2352 (2008).
50. S. F. Lux, M. Schmuck, B. Rupp, W. Kern, G. B. Appetecchi, S. Passerini, M. Winter, and A. Balducci: Mixtures of ionic liquids in combination with graphite electrodes: The role of Li-salt. ECS Trans. 16, 45 (2009).
51. A. Lewandowski and A. Widerska-Mocek: Properties of the graphite-lithium anode in N-methyl-N-propylpiperidinium bis (trifluoromethanesulfonyl)imide as an electrolyte. J. Power Sources 171, 938 (2007).
52. K. Yamamoto, Y. Iriyama, T. Asaka, T. Hirayama, H. Fujita, C. A. J. Fisher, K. Nonaka, Y. Sugita, and Z. Ogumi: Dynamic visualization of the electric potential in an all-solid-state rechargeable lithium battery. Angew. Chem. , Int. Ed. 49, 4414 (2010).
53. C. M. Wang, W. Xu, J. Liu, D. W. Choi, B. Arey, L. V. Saraf, J. G. Zhang, Z. G. Yang, S. Thevuthasan, D. R. Baer, and N. Salmon: In situ transmission electron microscopy and spectroscopy studies of interfaces in Li ion batteries: Challenges and opportunities. J. Mater. Res. 25, 1541 (2010).
54. C. M. Wang, W. Xu, J. Liu, J. G. Zhang, L. V. Saraf, B. W. Arey, D. W. Choi, Z. G. Yang, J. Xiao, S. Thevuthasan, and D. R. Baer: In situ transmission electron microscopy observation of microstructure and phase evolution in a SnO2 nanowire during lithium intercalation. Nano Lett. 11, 1874 (2011).
55. M. Klett, M. Giesecke, A. Nyman, F. Hallberg, R. W. Lindstrom, G. Lindbergh, and I. Furo: Quantifying mass transport during polarization in a li ion battery electrolyte by in situ Li-7 NMR imaging. J. Am. Chem. Soc. 134, 14654 (2012).
56. J. Wang, Y-C. K. Chen-Wiegart, and J. Wang: In situ chemical mapping of a lithium-ion battery using full-field hard X-ray spectroscopic imaging. Chem. Commun. 49, 6480 (2013).
57. I. T. Lucas, E. Pollak, and R. Kostecki: In situ AFM studies of SEI formation at a Sn electrode. Electrochem. Commun. 11, 2157 (2009).
58. S. F. Lux, I. T. Lucas, E. Pollak, S. Passerini, M. Winter, and R. Kostecki: The mechanism of HF formation in LiPF6 based organic carbonate electrolytes. Electrochem. Commun. 14, 47 (2012).
59. P. Novak, D. Goers, L. Hardwick, M. Holzapfel, W. Scheifele, J. Ufhiel, and A. Wursig: Advanced in situ characterization methods applied to carbonaceous materials. J. Power Sources 146, 15 (2005).
60. J. Y. Huang, L. Zhong, C. M. Wang, J. P. Sullivan, W. Xu, L. Q. Zhang, S. X. Mao, N. S. Hudak, X. H. Liu, A. Subramanian, H. Y. Fan, L. A. Qi, A. Kushima, and J. Li: In situ observation of the electrochemical lithiation of a single SnO2 nanowire electrode. Science 330, 1515 (2010).
61. M. T. McDowell, I. Ryu, S. W. Lee, C. Wang, W. D. Nix, and Y. Cui: Studying the kinetics of crystalline silicon nanoparticle lithiation with in situ transmission electron microscopy. Adv. Mater. 24, 6034 (2012).
62. X. H. Liu, J. W. Wang, S. Huang, F. Fan, X. Huang, Y. Liu, S. Krylyuk, J. Yoo, S. A. Dayeh, A. V. Davydov, S. X. Mao, S. T. Picraux, S. Zhang, J. Li, T. Zhu, and J. Y. Huang: In situ atomic-scale imaging of electrochemical lithiation in silicon. Nat. Nanotechnol. 7, 749 (2012).
63. X. H. Liu, L. Q. Zhang, L. Zhong, Y. Liu, H. Zheng, J. W. Wang, J-H. Cho, S. A. Dayeh, S. T. Picraux, J. P. Sullivan, S. X. Mao, Z. Z. Ye, and J. Y. Huang: Ultrafast electrochemical lithiation of individual Si nanowire anodes. Nano Lett. 11, 2251 (2011).
64. C-M. Wang, X. Li, Z. Wang, W. Xu, J. Liu, F. Gao, L. Kovarik, J-G. Zhang, J. Howe, D. J. Burton, Z. Liu, X. Xiao, S. Thevuthasan, and D. R. Baer: In situ TEM investigation of congruent phase transition and structural evolution of nanostructured silicon/carbon anode for lithium ion batteries. Nano Lett. 12, 1624 (2012).
65. H. Ghassemi, M. Au, N. Chen, P. A. Heiden, and R. S. Yassar: In-situ electrochemical lithiation/delithiation observation of individual amorphous Si nanorods. ACS Nano 5, 7805 (2011).
66. D. J. Miller, C. Proff, J. G. Wen, D. P. Abraham, and J. Barenõ: Observation of microstructural evolution in Li battery cathode oxide particles by in situ electron microscopy. Adv. Energy Mater. 3, 1098 (2013).
67. F. Wang, H-C. Yu, M-H. Chen, L. Wu, N. Pereira, K. Thornton, A. Van der Ven, Y. Zhu, G. G. Amatucci, and J. Graetz: Tracking lithium transport and electrochemical reactions in nanoparticles. Nat. Commun. 3, 1201 (2012).
68. Y. S. Meng, T. McGilvray, M-C. Yang, D. Gostovic, F. Wang, D. Zeng, Y. Zhu, and J. Graetz: In situ analytical electron microscopy for probing nanoscale electrochemistry. Electrochem. Soc. Interface 20, 49 (2011).
69. L. Q. Mai, Y. J. Dong, L. Xu, and C. H. Han: Single nanowire electrochemical devices. Nano Lett. 10, 4273 (2010).
70. H. Ghassemi, M. Au, N. Chen, P. A. Heiden, and R. S. Yassar: Real-time observation of lithium fibers growth inside a nanoscale lithium-ion battery. Appl. Phys. Lett. 99, 123113 (2011).
71. M. Gu, Y. Li, X. Li, S. Hu, X. Zhang, W. Xu, S. Thevuthasan, D. R. Baer, J-G. Zhang, J. Liu, and C. Wang: In situ TEM study of lithiation behavior of silicon nanoparticles attached to and embedded in a carbon matrix. ACS Nano 6, 8439 (2012).
72. A. Nie, L-Y. Gan, Y. Cheng, H. Asayesh-Ardakani, Q. Li, C. Dong, R. Tao, F. Mashayek, H-T. Wang, U. Schwingenschlögl, R. F. Klie, and R. S. Yassar: Atomic-scale observation of lithiation reaction front in nanoscale SnO2 materials. ACS Nano 23, 6203 (2013).
73. H. Yang, S. Huang, X. Huang, F. Fan, W. Liang, X. H. Liu, L-Q. Chen, J. Y. Huang, J. Li, T. Zhu, and S. Zhang: Orientationdependent interfacial mobility governs the anisotropic swelling in lithiated silicon nanowires. Nano Lett. 12, 1953 (2012).
74. X. H. Liu, L. Zhong, S. Huang, S. X. Mao, T. Zhu, and J. Y. Huang: Size-dependent fracture of silicon nanoparticles during lithiation. ACS Nano 6, 1522 (2012).
75. X. H. Liu, S. Huang, S. T. Picraux, J. Li, T. Zhu, and J. Y. Huang: Reversible nanopore formation in Ge nanowires during lithiation-delithiation cycling: An in situ transmission electron microscopy study. Nano Lett. 11, 3991 (2011).
76. Y. Liu, N. S. Hudak, D. L. Huber, S. J. Limmer, J. P. Sullivan, and J. Y. Huang: In situ transmission electron microscopy observation of pulverization of aluminum nanowires and evolution of the thin surface Al2O3 layers during lithiation-delithiation cycles. Nano Lett. 11, 4188 (2011).
77. L. Q. Zhang, X. H. Liu, Y-C. Perng, J. Cho, J. P. Chang, S. X. Mao, Z. Z. Ye, and J. Y. Huang: Direct observation of Sn crystal growth during the lithiation and delithiation processes of SnO2 nanowires. Micron 43, 1127 (2012).
78. L. Zhong, X. H. Liu, G. F. Wang, S. X. Mao, and J. Y. Huang: Multiple-stripe lithiation mechanism of individual SnO2 nanowires in a flooding geometry. Phys. Rev. Lett. 106, 248302 (2011).
79. A. Kushima, X. H. Liu, G. Zhu, Z. L. Wang, J. Y. Huang, and J. Li: Leapfrog cracking and nanoamorphization of ZnO nanowires during in situ electrochemical lithiation. Nano Lett. 11, 4535 (2011).
80. X. H. Liu, J. W. Wang, Y. Liu, H. Zheng, A. Kushima, S. Huang, T. Zhu, S. X. Mao, J. Li, S. Zhang, W. Lu, J. M. Tour, and J. Y. Huang: In situ transmission electron microscopy of electrochemical lithiation, delithiation and deformation of individual graphene nanoribbons. Carbon 50, 3836 (2012).
81. Q. Q. Li, P. Wang, Q. Feng, M. M. Mao, J. B. Liu, S. X. Mao, and H. T. Wang: In situ TEM on the reversibility of nanosized Sn anodes during the electrochemical reaction. Chem. Mater. 26, 4102 (2014).
82. Y. Liu, H. Zheng, X. H. Liu, S. Huang, T. Zhu, J. Wang, A. Kushima, N. S. Hudak, X. Huang, S. Zhang, S. X. Mao, X. Qian, J. Li, and J. Y. Huang: Lithiation-induced embrittlement of multiwalled carbon nanotubes. ACS Nano 5, 7245 (2011).
83. M. M. Islam and T. Bredow: Density functional theory study for the stability and ionic conductivity of Li2O surfaces. J. Phys. Chem. C 113, 672 (2009).
84. X. H. Liu, H. Zheng, L. Zhong, S. Huang, K. Karki, L. Q. Zhang, Y. Liu, A. Kushima, W. T. Liang, J. W. Wang, J-H. Cho, E. Epstein, S. A. Dayeh, S. T. Picraux, T. Zhu, J. Li, J. P. Sullivan, J. Cumings, C. Wang, S. X. Mao, Z. Z. Ye, S. Zhang, and J. Y. Huang: Anisotropic swelling and fracture of silicon nanowires during lithiation. Nano Lett. 11, 3312 (2011).
85. M. Meng Gu, A. Kushima, Y. Shao, J-G. Zhang, J. Liu, N. D. Browning, J. Li, and C-M. Wang: Probing the failure mechanism of SnO2 nanowires for sodium-ion batteries. Nano Lett. 13, 5203-5211 (2013).
86. J. E. Evans, K. L. Jungjohann, N. D. Browning, and I. Arslan: Controlled growth of nanoparticles from solution with in situ liquid transmission electron microscopy. Nano Lett. 11, 2809 (2011).
87. L. R. Parent, D. B. Robinson, T. J. Woehl, W. D. Ristenpart, J. E. Evans, N. D. Browning, and I. Arslan: Direct in situ observation of nanoparticle synthesis in a liquid crystal surfactant template. ACS Nano 6, 3589 (2012).
88. K. L. Jungjohann, S. Bliznakov, P. W. Sutter, E. A. Stach, and E. A. Sutter: In situ liquid cell electron microscopy of the solution growth of Au-Pd core-shell nanostructures. Nano Lett. 13, 2964 (2013).
89. T. J. Woehl, J. E. Evans, I. Arslan, W. D. Ristenpart, and N. D. Browning: Direct in situ determination of the mechanisms controlling nanoparticle nucleation and growth. ACS Nano 6, 8599 (2012).
90. N. de Jonge and F. M. Ross: Electron microscopy of specimens in liquid. Nat. Nanotechnol. 6, 695 (2011).
91. T. J. Woehl, C. Park, J. E. Evans, I. Arslan, W. D. Ristenpart, and N. D. Browning: Direct observation of aggregative nanoparticle growth: Kinetic modeling of the size distribution and growth rate. Nano Lett. 14, 373 (2013).
92. X. Chen, K. W. Noh, J. G. Wen, and S. J. Dillon: In situ electrochemical wet cell transmission electron microscopy characterization of solid-liquid interactions between Ni and aqueous NiCl. Acta Mater. 60, 192 (2012).
93. J. E. Evans, K. L. Jungjohann, P. C. K. Wong, P-L. Chiu, G. H. Dutrow, I. Arslan, and N. D. Browning: Visualizing macromolecular complexes with in situ liquid scanning transmission electron microscopy. Micron 43, 1085 (2012).
94. U. M. Mirsaidov, H. M. Zheng, Y. Casana, and P. Matsudaira: Imaging protein structure in water at 2. 7 nm resolution by transmission electron microscopy. Biophys. J. 102, L15 (2012).
95. T. W. Huang, S. Y. Liu, Y. J. Chuang, H. Y. Hsieh, C. Y. Tsai, W. J. Wu, C. T. Tsai, U. Mirsaidov, P. Matsudaira, C. S. Chang, F. G. Tseng, and F. R. Chen: Dynamics of hydrogen nanobubbles in KLH protein solution studied with in situ wet-TEM. Soft Matter 9, 8856 (2013).
96. M. T. Proetto, A. M. Rush, M-P. Chien, P. Abellan Baeza, J. P. Patterson, M. P. Thompson, N. H. Olson, C. E. Moore, A. L. Rheingold, C. Andolina, J. Millstone, S. B. Howell, N. D. Browning, J. E. Evans, and N. C. Gianneschi: Dynamics of soft nanomaterials captured by transmission electron microscopy in liquid water. J. Am. Chem. Soc. 136, 1162 (2014).
97. E. R. White, S. B. Singer, V. Augustyn, W. A. Hubbard, M. Mecklenburg, B. Dunn, and B. C. Regan: In situ transmission electron microscopy of lead dendrites and lead ions in aqueous solution. ACS Nano 6, 6308 (2012).
98. H. M. Zheng, S. A. Claridge, A. M. Minor, A. P. Alivisatos, and U. Dahmen: Nanocrystal diffusion in a liquid thin film observed by in situ transmission electron microscopy. Nano Lett. 9, 2460 (2009).
99. L. R. Parent, D. B. Robinson, P. J. Cappillino, R. J. Hartnett, P. Abellán, J. E. Evans, N. D. Browning, and I. Arslan: In situ observation of directed nanoparticle aggregation during the synthesis of ordered nanoporous metal in soft templates. Chem. Mater. 26, 1426 (2014).
100. M. Gu, L. R. Parent, B. L. Mehdi, R. R. Unocic, M. T. McDowell, R. L. Sacci, W. Xu, J. G. Connell, P. Xu, P. Abellan, X. Chen, Y. Zhang, D. E. Perea, J. E. Evans, L. J. Lauhon, J-G. Zhang, J. Liu, N. D. Browning, Y. Cui, I. Arslan, and C-M. Wang: Demonstration of an electrochemical liquid cell for operando transmission electron microscopy observation of the lithiation/delithiation behavior of Si nanowire battery anodes. Nano Lett. 13, 6106 (2013).
101. M. E. Holtz, Y. Yu, D. Gunceler, J. Gao, R. Sundararaman, K. A. Schwarz, T. A. Arias, H. D. Abrun?a, and D. A. Muller: Nanoscale imaging of lithium ion distribution during in situ operation of battery electrode and electrolyte. Nano Lett. 14, 1453 (2014).
102. R. L. Sacci, N. J. Dudney, K. L. More, L. R. Parent, I. Arslan, N. D. Browning, and R. R. Unocic: Direct visualization of initial SEI morphology and growth kinetics during lithium deposition by in situ electrochemical transmission electron microscopy. Chem. Commun. 50, 2104 (2014).
103. Z. Zeng, W-I. Liang, H-G. Liao, H. L. Xin, Y-H. Chu, and H. Zheng: Visualization of electrode-electrolyte interfaces in LiPF6/EC/DEC electrolyte for lithium ion batteries via in situ TEM. Nano Lett. 14, 1745 (2014).
104. R. R. Unocic, R. L. Sacci, G. M. Brown, G. M. Veith, N. J. Dudney, K. L. More, F. S. Walden, II. , D. S. Gardiner, J. Damiano, and D. P. Nackashi: Quantitative electrochemical measurements using in situ ec-S/TEM devices. Microsc. Microanal. 20, 452 (2014).
105. X. H. Liu, F. Fan, H. Yang, S. Zhang, J. Y. Huang, and T. Zhu: Self-limiting lithiation in silicon nanowires. ACS Nano 7, 1495 (2012).
106. Y. Yang, C. Xie, R. Ruffo, H. Peng, D. K. Kim, and Y. Cui: Single nanorod devices for battery diagnostics: A case study on LiMn2O4. Nano Lett. 9, 4109 (2009).
107. F. Lin, D. Nordlund, T-C. Weng, Y. Zhu, C. Ban, R. M. Richards, and H. L. Xin: Phase evolution for conversion reaction electrodes in lithium-ion batteries. Nat. Commun. 5, 3358 (2014).
108. F. Wang, J. Graetz, M. S. Moreno, C. Ma, L. Wu, V. Volkov, and Y. Zhu: Chemical distribution and bonding of lithium in intercalated graphite: Identification with optimized electron energy loss spectroscopy. ACS Nano 5, 1190 (2011).
109. X. H. Liu, Y. Liu, A. Kushima, S. Zhang, T. Zhu, J. Li, and J. Y. Huang: In situ TEM experiments of electrochemical lithiation and delithiation of individual nanostructures. Adv. Energy Mater. 2, 722 (2012).
110. P. Vajda and F. Beuneu: Electron radiation damage and Li-colloid creation in Li2O. Phys. Rev. B 53, 5335 (1996).
111. G. Krexner, M. Prem, F. Beuneu, and P. Vajda: Nanocluster formation in electron-irradiated Li2O crystals observed by elastic diffuse neutron scattering. Phys. Rev. Lett. 91, 135502 (2003).
112. C. M. Wang, D. R. Baer, J. E. Amonettea, M. H. Engelharda, J. J. Antony, and Y. Qiang: Electron beam-induced thickening of the protective oxide layer around Fe nanoparticles. Ultramicroscopy 108, 43 (2007).
113. F. Wang, M. Malac, and R. F. Egerton: Energy-loss near-edge fine structures of iron nanoparticles. Micron 37, 316 (2006).
114. M. den Heijer, I. Shao, A. Radisic, M. C. Reuter, and F. M. Ross: Patterned electrochemical deposition of copper using an electron beam. APL Mater. 2, 022101 (2014).
115. J. M. Grogan, N. M. Schneider, F. M. Ross, and H. H. Bau: Bubble and pattern formation in liquid induced by an electron beam. Nano Lett. 14, 359 (2014).
116. P. Abellan, B. L. Mehdi, L. R. Parent, M. Gu, C. Park, W. Xu, Y. Zhang, I. Arslan, J-G. Zhang, C-M. Wang, J. E. Evans, and N. D. Browning: Probing the degradation mechanisms in electrolyte solutions for Li-ion batteries by in situ transmission electron microscopy. Nano Lett. 14, 1293 (2014).
117. K. Xu: Nonaqueous liquid electrolytes for lithium-based rechargeable batteries. Chem. Rev. 104(10), 4303 (2004).
118. E. Nasybulin, W. Xu, M. H. Engelhard, Z. M. Nie, S. D. Burton, L. Cosimbescu, M. E. Gross, and J. G. Zhang: Effects of electrolyte salts on the performance of Li-O2 batteries. J. Phys. Chem. C 117, 2635 (2013).
119. Y. Gofer, M. Ben-Zion, and D. Aurbach: Solutions of LiAsF6 in 1,3-dioxolane for secondary lithium batteries. J. Power Sources 39, 163 (1992).
120. C. Nanjundiah, J. L. Goldman, L. A. Dominey, and V. R. Koch: Electrochemical stability of LiMF6 (M5P, As, Sb) in tetrahydrofuran and sulfolane. J. Electrochem. Soc. 135, 2914 (1988).
121. J. Belloni, M. Mostafavi, H. Remita, J. L. Marignier, and M. O. Delcourt: Radiation-induced synthesis of mono-and multi-metallic clusters and nanocolloids. New J. Chem. 22, 1239 (1998).
122. J. Belloni: Nucleation, growth and properties of nanoclusters studied by radiation chemistry-Application to catalysis. Catal. Today 113, 141 (2006).
123. E. Peled, D. Golodnitsky, C. Menachem, and D. Bar-Tow: An advanced tool for the selection of electrolyte components for rechargeable lithium batteries. J. Electrochem. Soc. 145, 3482 (1998).
124. P. Verma, P. Maire, and P. Novak: A review of the features and analyses of the solid electrolyte interphase in Li-ion batteries. Electrochim. Acta 55, 6332 (2010).
125. R. F. Egerton: Control of radiation damage in the TEM. Ultramicroscopy 127, 100 (2013).
126. T. J. Woehl, K. L. Jungjohann, J. E. Evans, I. Arslan,W. D. Ristenpart, and N. D. Browning: Experimental procedures to mitigate electron beam induced artifacts during in situ fluid imaging of nanomaterials. Ultramicroscopy 127, 53 (2013).
127. K. L. Jungjohann, J. E. Evans, J. A. Aguiar, I. Arslan, and N. D. Browning: Atomic-scale imaging and spectroscopy for in situ liquid scanning transmission electron microscopy. Microsc. Microanal. 18, 621 (2012).
128. D. A. Welch, R. Faller, J. E. Evans, and N. D. Browning: Simulating realistic imaging conditions for in situ liquid microscopy. Ultramicroscopy 135, 36 (2013).
129. R. F. Egerton: Electron Energy-Loss Spectroscopy in the Electron Microscope, 3rd ed. (Springer, New York, NY, 2011).
130. M. E. Holtz, Y. Yu, J. Gao, H. D. Abrunã, and D. A. Muller: In situ electron energy-loss spectroscopy in liquids. Microsc. Microanal. 19, 1027 (2013).
131. F. A. Stevie, R. B. Irwin, T. L. Shofner, S. R. Brown, J. L. Drown, and L. A. Giannuzzi: Plan view TEM sample preparation using the focused ion beam lift-out technique. AIP Conf. Proc. 449, 868 (1998).