In situ transmission electron microscopy and spectroscopy studies of rechargeable batteries under dynamic operating cond
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In situ transmission electron microscopy and spectroscopy studies of rechargeable batteries under dynamic operating conditions: A retrospective and perspective view Chong-Min Wanga) Environmental Molecular Sciences Laboratory, Pacific Northwest National Laboratory, Richland, Washington 99354, USA (Received 11 June 2014; accepted 12 August 2014)
Since the advent of the transmission electron microscope (TEM), continuing efforts have been made to image material under native and reaction environments that typically involve liquids, gases, and external stimuli. With the advances of aberration-corrected TEM for improving the imaging resolution, steady progress has been made on developing methodologies that allow imaging under dynamic operating conditions, or in situ TEM imaging. The success of in situ TEM imaging is closely associated with advances in microfabrication techniques that enable manipulation of nanoscale objects around the objective lens of the TEM. This study summarizes and highlights recent progress involving in situ TEM studies of energy storage materials, especially rechargeable batteries. The study is organized to cover both the in situ TEM techniques and the scientific discoveries made possible by in situ TEM imaging.
I. INTRODUCTION
Over the last decade, tremendous progress has been made on the development of aberration-corrected scanning/transmission electron microscopy (S/TEM).1–8 As a result, atomic-scale imaging and spectroscopic probing of materials appear to be routine practice.9–14 Imaging materials at or near-realistic working conditions, or in situ S/TEM, is keeping pace with the progress of high-spatial, fast-temporal, and high-energy resolution, as exemplified by the in situ TEM observation of nanostructured materials growth, 15,16 the solid–gas reaction in a catalytic system,17–19 materials deformation behavior,20,21 particle nucleation and growth from a solution,22–24 the electrochemical deposition process,25 and cells in a liquid environment.26 This progress has benefited from both the development of a dedicated microscope that can handle certain gas pressure around the sample region, such as the environmental TEM, and the ability to manipulate and microfabricate materials at the nanoscale. Energy storage technologies, such as lithium-ion (Li-ion) batteries, now are indispensably used for portable electronics, electric vehicles, and renewable energies. 27–31 One of the fundamental challenges for battery research is direct observation of the structural and chemical evolution of the battery components and a)
Address all correspondence to this author. e-mail: [email protected] DOI: 10.1557/jmr.2014.281 J. Mater. Res., 2014
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how this directly correlates with battery properties. The ex situ method, based on electron beam imaging and spectroscopy, has been widely used for probing the structural features of a lithium battery system. 32–39 However, due to the dynamic nature of the process, the ex situ method cannot answer some of the qu
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