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Solid Interfaces in Electrochemical Devices T.A In situ and operando probing of solid– solid interfaces in electrochemical devices T.A. Wynn , J.Z. Lee , A. Banerjee , and Y.S. Meng Solid-state electrolytes can offer improved lithium-ion battery safety while potentially increasing the energy density by enabling alkali metal anodes. There have been signifi cant research efforts to improve the ionic conductivity of solid-state electrolytes and the electrochemical performance of all-solid-state batteries; however, the root causes of their poor performance— interfacial reaction and subsequent impedance growth—are poorly understood. This is due to the dearth of effective characterization techniques for probing these buried interfaces. In situ and operando methodologies are currently under development for solid-state interfaces, and they offer the potential to describe the dynamic interfacial processes that serve as performance bottlenecks. This article highlights state-of-the-art solid–solid interface probing methodologies, describes practical limitations, and describes a future for dynamic interfacial characterization. Introduction the importance of these interfaces in the functionality of next- The future of electrochemical energy storage depends on the generation solid-state devices, there are surprisingly few studies concurrent advancement of constituent component materials focused on characterization of their interfaces, and even fewer and their satisfactory interaction with one another. We primarily providing in situ and operando insights. look to increase the energy and power density of electrochem- In the past decade there have been signifi cant efforts in ical cells through increasing electrode capacity, and remove applying in situ and operando measurements to electrochemical the chemical energy available for release during device failure, systems, though most work is limited to liquid-electrolyte sys- as present in modern fl ammable organic liquid electrolytes tems. Development of intricate electrochemical testing cells used in lithium-ion batteries. 1 Solid-state electrolytes (SSEs) for synchrotron end stations have enabled in situ and operando may satisfy both these requirements, serving as a safe replace- x-ray diffraction (XRD), x-ray absorption spectroscopy, and ment for their organic liquid counterparts, while potentially x-ray photoelectron spectroscopy (XPS). 8 In situ holders for enabling alkali metal anodes. electron microscopy have similarly progressed, 9 – 12 aided by However, the introduction of SSEs into full cell batteries is the collaborative environment established by developers of accompanied by other constraints, both intrinsic and extrinsic. 2 transmission electron microscopy (TEM) holders. These Intrinsically, though many SSEs exhibit high bulk ionic methods have enabled dynamic observation of the complex conductivity, grain boundaries may ultimately reduce the changes within electrode materials during electrochemical effective ionic conductivity to unusable levels, as in the case cycling and have provided a variety of insights, including the of solid-oxide perovskite lithium lanthanum titanate (LLTO), 3 dynamics of lithiation, phase transformations, and the elusive and may serve as regions of mechanical susceptibility, aid- nature of the solid-electrolyte interface (SEI) formation. Such ing lithium dendrite nucleation and penetration. 4 Extrinsically, in situ electrochemical liquid testing methods are extensively questions of electrolyte/electrode interfacial impedance, resulting described in previous review articles. 8 – 12 from space charge 5 and chemical and electrochemical com- Attempts to observe similar processes in solid-state patibility 6 , 7 of solid–solid interfaces, come into play. Despite materials have added degrees of complexity due to their buried T.A. Wynn , University of California , San Diego , USA ; [email protected] J.Z. Lee , University of California , San Diego , USA ; [email protected] A. Banerjee , University of California , San Diego , USA ; [email protected] Y.S. Meng , University of California , San Diego , USA ; [email protected] doi:10.1557/mrs.2018.235 Downloaded768 MRSfrom BULLETIN https://www.cambridge.org/core • VOLUME 43 • OCTOBER .2018 Access • www.mrs.org/bulletin paid by the UC San Diego Library, on 11 Oct 2018 at 05:21:11, subject to the Cambridge Core © 2018 terms Materials of use, Research available Society at https://www.cambridge.org/core/terms. https://doi.org/10.1557/mrs.2018.235 IN SITU AND OPERANDO PROBING OF SOLId–solID INTERFACES IN ELECTROCHEMICAL DEVICES interfaces, often requiring the expansion of existing tech- interface was shown via XPS to modify lithium concentration, niques and the development of entirely new methodologies. an effect that was attributed to non-faradaic Li migration.19 This perspective aims to review advanced characterization A following body of computational research opened the ques- techniques applied to solid–solid interfaces, working toward tion as to the thermodynamic stability of these interfaces— in situ and operando characterization to elucidate the less- a fundamentally important step in interpreting the nature understood dynamic behavior and heterogeneous characteris- of these buried interfaces, providing potential explanations tics present at these interfaces. for the presence of interfacial resistances at solid−solid inter- faces.6,7,20 This work suggests that stable solid-state inter- Techniques to characterize buried solid–solid phases effectively bridge the electrochemical window in interfaces much the same way the SEI does in their liquid electrolyte Until recently, electrochemical techniques, primarily cyclic counterpart. voltammetry and electrochemical impedance spectroscopy, Thermodynamically driven decomposition is most clearly were the main methods of characterizing buried interface shown after applying high-temperature processing methods, resistances. These studies are prevalent in characterization of as in the case of spinel cathodes interfaced with LATP; here, all-solid-state batteries, such as LiCoO2 (LCO)/lithium phos- the increased temperature drives decomposition to a degree 13 phorus oxynitride (LiPON)/Li and LCO/Li1.5Al0.5Ti1.5(PO4)3 detectable by x-ray diffraction (XRD)—intuitively ruling (LATP)14 chemistries. Electrochemical testing of such cells out high-temperature co-sintering as a processing method.21 suggested growing interfacial impedance, vaguely attributed Combining results of electrochemical testing with ex situ to modified chemical bonding impacting charge-transfer evaluation has proven to be an effective technique for a more characteristics.13 Thermal annealing studies showed reduced comprehensive understanding of the stability of solid–solid interfacial resistances and improved cyclability of the LCO/ interfaces, and has yielded results consistent with computa- LiPON/Li cells, though physical interpretation was specu- tional predictions. lative, lacking further experimental evidence and simply For the case of LCO/LiPON, LCO was predicted to decom- attributing the change to modified bonding at the LCO/LiPON pose into a variety of constituents, dependent on the local interface.13 The LCO/LATP cell utilized in situ formation of bonding environment and lithiation state.20 Experimentally, the anode, showing low charge-transfer resistance, though it was observed that cycling LCO/LiPON/Li thin-film batter- the nature of the anode was unknown at the time of the ies at elevated temperatures resulted in increasing interfacial electrochemical testing.14 impedance values. When extracted by a focused ion beam Similar studies further evaluated the stability of an inter- (FIB) system and observed by scanning transmission electron face or interlayer, such as the insertion of a Nb interlayer microscopy coupled with electron energy-loss spectroscopy between LCO and lithium lanthanum zirconium oxide (LLZO) (STEM/EELS), the increased interfacial impedance was cor- electrolyte, observing reduced interfacial impedance without related with the growth of a structurally decomposed LCO 15 explicit mechanistic descriptions. That is not to say that elec- interlayer, exhibiting chemical signals consistent with Li2O 22 trochemical methods are insufficient methods of probing such and disordered rock-salt Co3O4. X-ray photoelectron spec- interfaces. In scenarios where constituents are expected to be troscopy (XPS) was similarly applied to explain growing kinetically stable, careful experimental design promotes iso- impedance in Na-metal/Na-sulfide symmetric cells; as pre- lation of such effects, as in the case of idealized solid-state dicted by computational modeling, Cl-doping was observed to interfaces such as some silver conductors.16 Control of materi- promote the formation of NaCl, which stabilized the interface, als selection can allow electrochemical methodologies to preventing further electrolyte decomposition.23 Similar to the effectively isolate sources of charge-transfer resistance to the case of LCO/LiPON, DFT modeling of phase diagrams is par- impact of lattice mismatch, defect chemistry, and equilibrium tially correct, yet it generally fails to differentiate the kinetics potentials.17 Indeed, an entire field has been based around this of phase formation. ideology—solid-state ionics/nanoionics—however, this will Though ex situ methods have proven convenient for be not be covered in this article to focus on adapting advanced interpreting interfacial behavior, they are ineffective for characterization techniques to more commercially relevant
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