TY - JOUR

T1 - Foaming suppression during the solid-state synthesis of the Li1.3Al0.3Ti1.7(PO4)3 solid electrolyte

AU - Shindrov, Alexander A.

AU - Skachilova, Maria G.

AU - Gerasimov, Konstantin B.

AU - Kosova, Nina V.

N1 - This work was supported by the Russian Science Foundation, Project №22-43-02028.

PY - 2024/8

Y1 - 2024/8

N2 - In this work, the effect of carbon on the suppression of foaming during the solid-state synthesis of the Li1.3Al0.3Ti1.7(PO4)3 (LATP) solid electrolyte was studied. According to thermal analysis data, mechanically activated mixtures with and without carbon exhibit similar behavior. The presence of carbon does not affect the gas release process during decomposition, and foaming suppression occurs due to the change in viscosity of the melt created by NH4H2PO4. Slow LATP-S, medium LATP-M and fast LATP-F synthesis routes were used to evaluate the optimal conditions for LATP preparation. It was found that the use of carbon to suppress foaming eliminated the need for preheating and milling and reduced the synthesis time to 2.5 h (LATP-F). The effect of the synthesis route on the phase composition, morphology, conductive and electrochemical properties of LATP-S, LATP-M and LATP-F was investigated. No significant differences in studied properties were found for the synthesizer LATP samples excluding particle size distribution. Comparison of the granulometric curves showed that the fast synthesis method resulted in a decrease in particle size. The values of the ionic conductivity σion for LATP-S, LATP-M and LATP-F are equal to ∼10−4 S cm−1, while the electronic conductivity σe does not exeed∙10−9 S cm−1. The study of the electrochemical stability window of the synthesized LATP samples was showed that these solid electrolytes are stable up to 4.65–4.70 V.

AB - In this work, the effect of carbon on the suppression of foaming during the solid-state synthesis of the Li1.3Al0.3Ti1.7(PO4)3 (LATP) solid electrolyte was studied. According to thermal analysis data, mechanically activated mixtures with and without carbon exhibit similar behavior. The presence of carbon does not affect the gas release process during decomposition, and foaming suppression occurs due to the change in viscosity of the melt created by NH4H2PO4. Slow LATP-S, medium LATP-M and fast LATP-F synthesis routes were used to evaluate the optimal conditions for LATP preparation. It was found that the use of carbon to suppress foaming eliminated the need for preheating and milling and reduced the synthesis time to 2.5 h (LATP-F). The effect of the synthesis route on the phase composition, morphology, conductive and electrochemical properties of LATP-S, LATP-M and LATP-F was investigated. No significant differences in studied properties were found for the synthesizer LATP samples excluding particle size distribution. Comparison of the granulometric curves showed that the fast synthesis method resulted in a decrease in particle size. The values of the ionic conductivity σion for LATP-S, LATP-M and LATP-F are equal to ∼10−4 S cm−1, while the electronic conductivity σe does not exeed∙10−9 S cm−1. The study of the electrochemical stability window of the synthesized LATP samples was showed that these solid electrolytes are stable up to 4.65–4.70 V.

KW - Conductive properties

KW - Fast synthesis

KW - Foaming suppression

KW - Li1.3Al0.3Ti1.7(PO4)3

KW - Phase composition

KW - Super P

UR - https://www.scopus.com/record/display.uri?eid=2-s2.0-85196808993&origin=inward&txGid=cb32b07de3457045bbc1c9a3a42c721d

UR - https://www.webofscience.com/wos/woscc/full-record/WOS:001261926400001

UR - https://www.mendeley.com/catalogue/b72fa4a5-1f1e-3843-8a03-fbb284779554/

U2 - 10.1016/j.solidstatesciences.2024.107617

DO - 10.1016/j.solidstatesciences.2024.107617

M3 - Article

VL - 154

JO - Solid State Sciences

JF - Solid State Sciences

SN - 1293-2558

M1 - 107617

ER -