Air-stable sulfide sodium ion solid electrolyte and preparation method thereof
A solid electrolyte, sodium ion technology, applied in solid electrolyte, electrolyte battery manufacturing, non-aqueous electrolyte and other directions, can solve the problems of solid electrolyte failure, sensitivity, and restrict the application of sulfide solid electrolyte, and achieve the effect of increasing the cost of making batteries
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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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