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Wilkening, H. M. R.
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article
Proton Bulk Diffusion in Cubic Li7La3Zr2O12 Garnets as Probed by Single X-ray Diffraction
Abstract
<p>Ceramic electrolytes, characterized by a very high ionic conductivity as it is the case for Al-stabilized cubic Li<sub>7</sub> La<sub>3</sub> Zr<sub>2</sub> O<sub>12</sub> (Al:LLZO), are of utmost interest to develop next-generation batteries that can efficiently store electrical energy from renewable sources. If envisaged not as a solid electrolyte but as a protecting layer in lithium-metal batteries with liquid electrolytes, the ceramic should allow Li<sup>+</sup> to pass through but block out other species such as H<sup>+</sup> . Protons, for example, originating from the decomposition of electrolyte solvent molecules, will form detrimental LiH that severely affects the performance and lifetime of such batteries. Although Li-ion dynamics in Al:LLZO has been the topic of many studies, until today, little information is available about macroscopic proton diffusion in LLZO. Here, we used single-crystal X-ray diffraction to study the Li<sup>+</sup> /H<sup>+</sup> exchange rate in AL:LLZO over a period of about 3 years. Rietveld refinements reveal that H solely exchanges on the 96h site. The Li/H portion significantly changes from the anhydrous pristine sample to Li<sub>4.21</sub> :H<sub>0.66</sub> after 17 days of altering in humid air and finally to Li<sub>2.55</sub> :H<sub>2.32</sub> after 960 days. Considering the change of the Li/H portion and the probing depth of X-rays into Al:LLZO, we applied a spherical diffusion model to estimate the proton diffusion coefficient of D<sub>0</sub> ≠10<sup>-17</sup> m<sup>2</sup> s<sup>-1</sup> . Such a proton diffusion coefficient value is sufficiently high to have significant impact on cell performance and safety if Al:LLZO is going to be used to protect the Li-metal anode from reaction with the liquid electrolyte. In particular, during Li plating, such a high H<sup>+</sup> penetration rate may accelerate the formation of LiH, giving rise to safety problems of these types of batteries.</p>