Synthesis of a Li1.3Al0.3Ti1.7(PO4)3 Solid Electrolyte from Oxalate Precursor

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Abstract

A new efficient method of synthesis of solid electrolyte with high lithium-ion conductivity with NASICON structure of Li1.3Al0.3Ti1.7(PO4)3 (LATP) composition is proposed. The advantage of the developed method is the use of liquid-phase precursor based on titanium oxalate complex. It was found that at 750°C a single phase well crystallized LATP is formed. The total ionic conductivity value of LATP after sintering at 900°C measured by impedance spectroscopy was 2.6 × 10−4 S/cm at room temperature and the activation energy of conductivity was 0.28 eV. The presented synthesis method is promising for scale-up and mass production.

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About the authors

G. B. Kunshina

Tananaev Institute of Chemistry of the Kola Science Centre of the Russian Academy of Sciences

Author for correspondence.
Email: g.kunshina@ksc.ru
Russian Federation, 26a, Akademgorodok, Apatity, 184209

I. V. Bocharova

Tananaev Institute of Chemistry of the Kola Science Centre of the Russian Academy of Sciences

Email: g.kunshina@ksc.ru
Russian Federation, 26a, Akademgorodok, Apatity, 184209

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Supplementary files

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2. Fig. 1. Results of thermal analysis of oxalate precursor LATP (a) and crystalline LATP (b).

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3. Fig. 2. LATP diffractograms after annealing the oxalate precursor at temperatures of 300-750°C and after sintering in tablets between 850-1100°C. The asterisk indicates the impurity phase AlPO4.

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4. Fig. 3. SEM images of monophasic LATP powder obtained from oxalate precursor at 750°C after grinding on a KM1 ball mill.

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5. Fig. 4. IR spectrum of LATP after 300 (1), 750 (2) and 900°C (3).

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6. Fig. 5. Electrochemical impedance spectra after LATP sintering at 900°C (1) and 1000°C (2) measured at room temperature.

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7. Fig. 6. Temperature dependence of the ionic conductivity of LATP after sintering at 900°C.

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8. Fig. 7. Chronoamperometric curve (a) and linear voltammetry curve (b) of LATP.

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