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Instruments / Technical Area	Publication Details	Published
B18-Core EXAFS	Rapid sintering of Li6.5La3Zr1Nb0.5Ce0.25Ti0.25O12 for high density lithium garnet electrolytes with current induced in-situ interfacial resistance reduction Mark P. Stockham , Bo Dong , Matthew S. James , Pengcheng Zhu , Emma Kendrick , Peter R. Slater Energy Advances DOI: 10.1039/D3YA00123G Diamond Proposal Number(s): [14239] Open Access Show Abstract ▼ Abstract: A primary target of energy storage is the all solid state battery, however finding a suitable solid state electrolyte has proven troublesome. Lithium garnet materials are promising solid state electrolytes with high room temperature conductivity, a wide electrochemical window, high chemical stability with Li metal and have minimal hazards. However, lithium garnets suffer from slow, energy demanding synthesis, rapid proton exchange (leading to high interfacial resistance between the garnet and electrodes), mechanical instabilities with Li metal and require specific handling methods to achieve the highest performing materials (such as full processing under Ar). Here we report a Ti/Ce co-doped high entropy lithium garnet material with four B site dopants, with the formula Li6.5La3Zr1Nb0.5Ce0.25Ti0.25O12. This material benefits from rapid simultaneous sintering and densification directly from the starting materials, allowing formation of dense pellets in <1hr at 1100°C using only a standard, cheap, muffle furnace. Li6.5La3Zr1Nb0.5Ce0.25Ti0.25O12 also has high conductivity (0.5 mS cm-1 at 25°C), scalability and insensitivity to both rapid furnace ramp rates and long dwell times. There is also an indication of unusual behaviour towards limiting lithium dendrite propagation, which is also discussed.	Aug 2023
I15-1-X-ray Pair Distribution Function (XPDF)	X-ray pair distribution function analysis and electrical and electrochemical properties of cerium doped Li5La3Nb2O12 garnet solid-state electrolyte Bo Dong , Mark P. Stockham , Philip A. Chater , Peter R. Slater Dalton Transactions 414 DOI: 10.1039/D0DT02112A Diamond Proposal Number(s): [20877] Open Access Show Abstract ▼ Abstract: Garnet solid state electrolytes have been considered as potential candidates to enable next generation all solid state batteries (ASSBs). To facilitate the practical application of ASSBs, a high room temperature ionic conductivity and a low interfacial resistance between solid state electrolyte and electrodes are essential. In this work, we report a study of cerium doped Li5La3Nb2O12 through X-ray pair distribution function analysis, impedance spectroscopy and electrochemical testing. The successful cerium incorporation was confirmed by both X-ray diffraction refinement and X-ray pair distribution function analysis, showing the formation of an extensive solid solution. The local bond distances for Ce and Nb on the octahedral site were determined using X-ray pair distribution function analysis, illustrating the longer bond distances around Ce. This Ce doping strategy was shown to give a significant enhancement in conductivity (1.4 × 10−4 S cm−1 for Li5.75La3Nb1.25Ce0.75O12, which represents one of the highest conductivities for a garnet with less than 6 Li) as well as a dramatically decreased interfacial resistance (488 Ω cm2 for Li5.75La3Nb1.25Ce0.75O12). In order to demonstrate the potential of this doped system for use in ASSBs, the long term cycling of a Li//garnet//Li symmetric cell over 380 h has been demonstrated.	Aug 2020
B18-Core EXAFS	Evaluation of the effect of site substitution of Pr doping in the Lithium garnet system Li5La3Nb2O12 Mark P. Stockham , Bo Dong , Yongliang Li , Yulong Ding , Peter Slater Dalton Transactions DOI: 10.1039/D0DT01497D Diamond Proposal Number(s): [14239] Open Access Show Abstract ▼ Abstract: Li ion conducting garnets have been attracting considerable interest for use as the electrolyte in all solid-state batteries, due to their high ionic conductivity and wide electrochemical stability window. Consequently, there have been a number of doping studies aimed at optimising the conductivity, focusing on both doping in Li7La3Zr2O12 and Li5La3(Nb/Ta)2O12 systems. In this paper, we report a detailed study of Pr doping in Li5La3Nb2O12, and show that this is a rare example of an ambi-site dopant, being able to be doped onto either the La or Nb site. Interestingly the resultant Pr oxidation state is determined by the site substitution, with oxidation states of 3+ for the La site, and 4+ for the Nb site. While the conductivity is essentially unchanged for the La site substitution, Pr4+ substitution on the Nb site leads to a large increase in the conductivity associated with the increase in Li content (Li5+xLa3Nb2-xPrxO12) up to 0.56 mScm-1 (at 50˚C) for x=0.8. Overall, this work highlights the flexibility of these garnet materials to doping, and suggests that further consideration of site substitution be considered for other dopants.	May 2020

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