Performance of Nano-porous β-Li3PS4 Prepared by Solvent Removing Method†

doi:10.7503/cjcu20160333

Abstract

Abstract:

Room temperature-stable and highly ionic conductive crystal electrolyte β-Li₃PS₄ was fabricated via solvent-removing method using Li₂S and P₂S₅ as reactants, tetrahydrofuran as solvent. Then β-Li₃PS₄ was analyzed through X-ray diffraction, differential thermal analysis and thermogravimetry analysis, Raman spectrometry, N₂ adsorption-desorption analysis and electrochemical impedance spectroscopy. Effects of heat treatment temperature on solvent removing, crystallization, specific surface area, porosity, and ionic conductivity were investigated. The results show that solvent-removing method successfully stabilizes β-Li₃PS₄ at room temperature. When heated at 160 ℃, Li₃PS₄ reaches its highest ionic conductivity, 7.44×10^-6 S/cm. During the heating treatment, tetrahydrofuran solvent was removed in 3 stages, generating numerous nanopores at both surface and interior of the Li₃PS₄ particles. Those nanopores increase surface energy, which helps new phase nucleate, expedites crystalline transition, reduces phase transition temperature, and stabilizes β-Li₃PS₄ to room temperature.

Key words: Solid electrolyte, Solvent-removing method, Nanoporous, β-Li3PS4

CLC Number:

TrendMD:

PAN Yizhen, LI Yujie, CHEN Yimin, ZHENG Chunman. Performance of Nano-porous β-Li₃PS₄ Prepared by Solvent Removing Method^†[J]. Chem. J. Chinese Universities, 2016, 37(7): 1232.

Figures/Tables 10

Fig.1 DTA-TGA curves of Li3PS4·xTHF

Fig.2 Raman spectra of Li3PS4·xTHF heated at 80 ℃(a), 100 ℃(b) and 160 ℃(c)

Fig.3 XRD patterns of Li3PS4·xTHF heated at different temperaturesTemperature/℃: a. 25; b. 80; c. 100; d. 120;

Table 1 XRD data of Li3PS4 heated at different temperatures

Heating temperature/℃	Crystal face	2θ/(°)	d/nm	Peak width of half height/(°)
200	(102)	30.22	0.2955	0.139
160		30.18	0.2959	0.186
140		29.96	0.2980	0.220
200	(210)	17.89	0.4954	0.120
160		17.81	0.4976	0.162
140		17.65	0.5021	0.201
200	(220)	26.36	0.3379	0.148
160		26.30	0.3386	0.173
140		26.15	0.3404	0.181

Fig.4 SEM images of Li3PS4·xTHF before(A, B) and after(C, D) 160 ℃ heat treatment

Fig.5 Relationship between heating temperature and specific surface area

Fig.6 Pore diameter distribution of 160 ℃-heated Li3PS4

Fig.7 Impedance plot from the symmetrical cell containing 160 ℃-heated Li3PS4

Fig.8 Impedance plots from the symmetrical cell containing 160 ℃-(a), 180 ℃-(b) and 200 ℃-(c) heated Li3PS4

Fig.9 Logarithmic relationship between ionic conductivity and heating temperature

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Performance of Nano-porous β-Li₃PS₄ Prepared by Solvent Removing Method^†

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