Solid electrolyte and method for producing solid electrolyte
A technology of solid electrolyte and manufacturing method, which is applied in the direction of solid electrolyte, non-aqueous electrolyte battery, electrolyte, etc., can solve the problems of reduced ion conductivity and inability to obtain solid electrolyte, and achieve the effect of simplifying the manufacturing process
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Embodiment 1A
[0188] A planetary ball mill (trade name: CLASSIC LINE P-7, manufactured by Fritsch Corporation) was installed. Weigh 0.598g of lithium sulfide, 0.867g of phosphorus pentasulfide, 0.271g of lithium bromide, and 0.264g of iodine, and put them into a container (45cc, made of zirconia) for a planetary ball mill, then put in 4g of dehydrated toluene (moisture content: 10ppm or less), and put the container Completely airtight. This container was attached to the above-mentioned planetary ball mill, and the mixing, stirring, and pulverization were performed simultaneously for 40 hours at a chassis rotation speed of 500 rpm to prepare a sulfide-based solid electrolyte.
[0189] In the glove box, 5 ml of dehydrated toluene was added to the obtained slurry-like product containing an amorphous sulfide-based solid electrolyte and a solvent, and it was collected in a metal tank (butter), and the powder (solid electrolyte) was precipitated, and then removed. as a solvent for the supernatan...
Embodiment 2A
[0200] use image 3 The device shown is used to manufacture sulfide-based solid electrolytes. right image 3 The device shown is described. image 3 The illustrated apparatus includes a bead mill 10 for reacting raw materials by mixing, stirring, pulverizing, or combining them, and a reaction tank 20 . The reaction tank 20 is equipped with the container 22 and the stirring blade 24, and the stirring blade 24 is driven by the motor (M).
[0201] The bead mill 10 is provided with a heater 30 capable of feeding warm water (HW) around the mill 10, and heat is supplied to the warm water (HW) by the heater 30, and the warm water (RHW) discharged from the outlet of the heater 30 is ) is externally circulated to the heater 30 in the form of warm water (HW) after heating. The reaction tank 20 enters the oil bath 40 . The oil bath 40 heats the raw materials and the solvent in the container 22 to a predetermined temperature. For the reaction tank 20, a cooling pipe 26 that cools an...
Embodiment 3A
[0208] In Example 2A, an amorphous sulfide-based solid electrolyte was obtained in the same manner as in Example 2A except that lithium sulfide was 35.64 g, phosphorus pentasulfide was 49.25 g, iodine was 14.06 g, and bromine was 8.85 g. The obtained sulfide-based solid electrolyte was subjected to powder X-ray analysis (XRD) measurement in the same manner as in Example 1A. As a result, it was found that there were no peaks other than those derived from the raw materials.
[0209] The obtained amorphous sulfide-based solid electrolyte was heated at 203° C. for 3 hours to obtain a crystalline sulfide-based solid electrolyte. As a result of powder X-ray analysis (XRD) measurement, crystallization peaks were detected at 2θ=19.9° and 23.6° similarly to Example 1, and it was confirmed that a crystalline sulfide-based solid electrolyte was obtained. The ion conductivity of the obtained crystalline sulfide-based solid electrolyte was measured and found to be 5.01×10 -3 (S / cm), confi...
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