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A NASICON-type Li 1+x Al x Ti 2-x(PO 4) 3 (LATP) cold-sintered solid electrolyte is reported with a dense structure, as a possible alternative the commonly recognized liquid organic electrolytes. A low-temperature sintering technology (below 200 °C) with a sintering additive, aid of acid solvent and high pressure is originally developed for preparing the solid electrolyte. In addition, the setup has been designed using in operando impedance technique simultaneously, the Cold Sintering Process (CSP) is monitored in order to explore the mechanism are taking place during the densification. As a result, an ionic conductivity as high as 4.48·10−5 S·cm−1, with a relative density of ∼82% has been achieved for 2 wt% Bi 2 O 3 and 25 wt% 3 m acid acetic solution, LATP powder, and sintered under 700 MPa and at 150 °C, reaching the highest value in published peer-reviewed literature. The cold-sintered ceramics without post-annealing high temperature treatments present kinetics limitations due to intergranular regions. Therefore, this bottleneck must be studied and overcome to achieve higher ionic conductivities at low temperatures. [Display omitted] • Modification strategies of ceramic electrolytes sintering are focused on. • Cold Sintering Process method to sinter x-Bi2O3:LATP solid electrolyte. • Combination of 3 cornerstones: sintering aid, CSP and in operando impedance. [ABSTRACT FROM AUTHOR]

In the present work, a Polymer-In-Ceramics (PIC) solid electrolyte based on Li 1.3 Al 0.3 Ti 1.7 (PO 4) 3 (LATP) and PEO n -LiTFSI (poly(ethylene oxide) - lithium bis(trifluoromethanesulfonyl)imide) is obtained via Cold Sintering Process (CSP), at a temperature of 150 °C without any post-heat treatment, this is 900 °C below the traditional sintering temperature. This novel study demonstrates the effect of the Transient Liquid Phase content (TLP) and the composition of the polymeric active filler on the final Composite Solid Electrolyte (CSE) properties, with the sintering process being monitored by in-operando Electrochemical Impedance Spectroscopy (EIS). Firstly, the 15 wt% of TLP is stated as the optimal liquid content based on the electrical answer and workability. Then, the (EO:Li+) molar ratio is studied from (1:1) to (8:1). The highest ionic conductivity of 1.04·10−4 S cm−1 and a relative density above 98% are achieved at room temperature when the TLP content is 15 wt% and the molar ratio (2:1), with the LATP content set in 90 wt%. Moreover, the activation energy (Ea) is drastically reduced, from 0.388 eV (LATP ceramic electrolyte) to 0.298 eV (PIC electrolyte), with a lithium transference number (t Li +) close to 1. Therefore, this research work proposes a potential solid electrolyte to substitute the traditional liquid electrolytes. • Modification strategies of ceramic electrolytes sintering are focused on. • Cold Sintering Process method to sinter LATP-based Composite Solid Electrolyte. • The future of ASSLBs using Polymer-in-Ceramic electrolytes is discussed. • PEO n -LiTFSI doping of ceramic electrolytes to improve the ionic conductivity. [ABSTRACT FROM AUTHOR]