A kind of air stable sulfide sodium ion solid electrolyte and preparation method thereof
A solid electrolyte and sodium ion technology, applied in the direction of solid electrolyte, electrolyte battery manufacturing, non-aqueous electrolyte, etc., can solve the problems of limiting the application of sulfide solid electrolyte, sensitivity, solid electrolyte failure, etc.
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[0033] The preparation method of above-mentioned cubic phase sulfide is: Na 2 S, Na 2 O, SnS 2 ,P 2 S 5 、As 2 S 5 , Sb 2 S 5 Take Na 4-x sn 1- x m x S 4-y o y The molar ratio within is weighed under an inert atmosphere, and mixed uniformly, and then calcined at 400°C to 650°C for 8h to 24h under a vacuum degree of less than 100Pa, so as to prevent the reactants from reacting with oxygen or moisture in the air to form impurities;
[0034] In the Na-Sn-M-S-O system, there are crystal phases of various structures, and uniform mixing is very important. Uneven mixing causes inconsistencies in components and is prone to impurities; at the same time, the mixing process is also accompanied by the fineness of raw materials. The chemical process is beneficial to the synthesis of sulfide electrolyte in the later stage; the method of uniform mixing can choose mechanical grinding methods such as vibration mill, turbo mill, ball mill; for example, when mixing by ball mill metho...
Embodiment 1
[0037] Na in an argon-protected glove box 2 S, Sb 2 S 5 , SnS 2 Take Na 3.7 sn 0.7 Sb 0.3 S 4 The mol ratio is weighed and mixed as raw materials;
[0038] Put the raw materials and zirconia balls into a zirconia-substrate ball mill tank with a capacity of 100, seal the container, perform ball mill mixing at a speed of 350 r / min, and obtain a mixed powder after 15 hours;
[0039] Put the mixed powder in the glove box, take it out, and form it under 150MPa pressure in a powder tablet press, put it into a glass / quartz tube, evacuate it until the vacuum degree is less than 100Pa, seal it, and put it into a muffle furnace. The temperature rise rate of the muffle furnace is 100°C / hour, and then the solid phase reaction is carried out at 550°C for 24 hours, and the temperature is naturally cooled to obtain the product Na 4-x sn 1-x MxS 4-y o y , in this example, the product is Na 3.7 sn 0.7 Sb 0.3 S 4 .
[0040] In the glove box, the product was taken out from the se...
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