Sulfide composite solid electrolyte prepared by dry method and preparation method thereof
A technology of sulfide electrolyte and solid electrolyte, which is applied in the direction of solid electrolyte, non-aqueous electrolyte, circuit, etc., and can solve the problems affecting the ionic conductivity of sulfide electrolyte sheets, etc.
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[0028] The invention provides a preparation method of a sulfide composite solid electrolyte, comprising: a) freeze-grinding a polymer to obtain a polymer powder; b) mixing the polymer powder with a sulfide electrolyte powder, then performing shear kneading, The sulfide composite solid electrolyte is obtained through static pressure processing of a flat plate, and then densified under pressure.
[0029] The present invention has no special limitation on the sources of all raw materials, which can be commercially available or self-made.
[0030] In the present invention, the polymer is preferably styrene-ethylene-butylene-styrene copolymer, butadiene-styrene copolymer, polyvinylidene fluoride, polysulfone, polyethersulfone, polymethyl sulfone Acrylic-based, polyacrylonitrile-based, cellulose, polytetrafluoroethylene, polystyrene-based, polycarbonate-based, polyvinyl chloride-based, polyamide-based, polyimide-based, polyurethane-based, ethylene-vinyl acetate One or more of copol...
Embodiment 1
[0051] Styrene-ethylene-butylene-styrene copolymer (25 wt% styrene content) was ground into a powder with an average particle size of 55 μm in liquid nitrogen by a freeze grinder, and then 0.5 parts by mass of styrene-ethylene- Butylene-styrene copolymer powder and 99.5 parts by mass of sulfide electrolyte Li with an average particle size of 25 μm 10 sn 0.7 Si 0.3 P 2 S 12 The powder is uniformly mixed by mechanical stirring; the obtained electrolyte mixture is sheared and kneaded at 100°C by an internal mixer, and then the sheared and kneaded electrolyte mixture is processed into a sheet at 110°C by flat plate static pressure (50MPa, 10min) ; the resulting electrolyte sheet was densified by roll pressing to obtain a 146 μm monolayer Li 10 sn 0.7 Si 0.3 P 2 S 12 Composite solid electrolyte sheet.
[0052] At room temperature, for the prepared Li 10 sn 0.7 Si 0.3 P 2 S 12 The composite solid electrolyte sheet was tested by electrochemical impedance spectroscopy, u...
Embodiment 2
[0054] Grind polyimide (the tensile strength of pure polyimide is 110 MPa) in dry ice into a powder with an average particle size of 5 μm by a freeze grinder, then mix 10 parts by mass of polyimide powder with 90 parts by mass The sulfide electrolyte Li with an average particle size of 5 μm 3 P.S. 4 The powder is mixed evenly by hand grinding; the obtained electrolyte mixture is sheared and kneaded at 160°C by a kneader, and then the sheared and kneaded electrolyte mixture is processed into a sheet shape at 260°C by flat plate static pressure (500MPa, 50min); The resulting electrolyte sheet was densified by isostatic pressing to obtain a 10 μm monolayer Li 3 P.S. 4 Composite solid electrolyte sheet.
[0055] At room temperature, for the prepared Li 3 P.S. 4 The composite solid electrolyte sheet was tested by electrochemical impedance spectroscopy, using stainless steel as the electrode, and the obtained results were: lithium ion conductivity 9.7×10 -4 S / cm.
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