A method of production of a solid electrolyte, which comprises: a step of obtaining a mixture comprising a sulfide solid electrolyte and a tertiary alcohol including 9 or less carbon atoms, and a step of removing the tertiary alcohol from the mixture.

A method of production of a solid electrolyte, which comprises: a step of obtaining a mixture comprising a sulfide solid electrolyte and a tertiary alcohol including 9 or less carbon atoms, and a step of removing the tertiary alcohol from the mixture.

The invention relates to a highly reactive, high-purity, free-flowing and dust-free lithium sulfide powder having an average particle size between 250 and 1,500 m and BET surface areas between 1 and 100 m.sup.2/g. The invention, furthermore, relates to a process for its preparation, wherein in a first step, lithium hydroxide monohydrate is heated in a temperature-controlled unit to a reaction temperature between 150 C. and 450 C. in the absence of air, and an inert gas is passed over or through it, until the residual water of crystallization content of the formed lithium hydroxide is less than 5 wt. % and in a second step, the anhydrous lithium hydroxide formed in the first step is mixed, overflowed or traversed by a gaseous sulfur source from the group consisting of hydrogen sulfide, elemental sulfur, carbon disulfide, mercaptans or sulfur nitrides.

The invention relates to a highly reactive, high-purity, free-flowing and dust-free lithium sulfide powder having an average particle size between 250 and 1,500 m and BET surface areas between 1 and 100 m.sup.2/g. The invention, furthermore, relates to a process for its preparation, wherein in a first step, lithium hydroxide monohydrate is heated in a temperature-controlled unit to a reaction temperature between 150 C. and 450 C. in the absence of air, and an inert gas is passed over or through it, until the residual water of crystallization content of the formed lithium hydroxide is less than 5 wt. % and in a second step, the anhydrous lithium hydroxide formed in the first step is mixed, overflowed or traversed by a gaseous sulfur source from the group consisting of hydrogen sulfide, elemental sulfur, carbon disulfide, mercaptans or sulfur nitrides.

A main object of the present disclosure is to provide a method for producing a sulfide solid electrolyte material, the method that allows a concentration of lithium halide to increase and that allows drying at a low temperature. The present disclosure achieves the object by providing a method for producing a sulfide solid electrolyte material, the method comprising: a drying step of drying a precursor aqueous solution containing LiI, LiBr, and LiOH to remove water and obtain a precursor mixture; and an electrolyte synthesizing step including a sulfidization treatment to sulfurize the LiOH in the precursor mixture and obtain LiHS, a de-sulfide-hydrogenating treatment to desorb a hydrogen sulfide from the LiHS and obtain Li.sub.2S, and a synthesizing treatment to make the Li.sub.2S to react with an auxiliary material; wherein a molar ratio of the LiOH with respect to the LiI and the LiBr, LiOH/(LiI+LiBr), in the precursor aqueous solution is 3 or more and less than 6.

A main object of the present disclosure is to provide a method for producing a sulfide solid electrolyte material, the method that allows a concentration of lithium halide to increase and that allows drying at a low temperature. The present disclosure achieves the object by providing a method for producing a sulfide solid electrolyte material, the method comprising: a drying step of drying a precursor aqueous solution containing LiI, LiBr, and LiOH to remove water and obtain a precursor mixture; and an electrolyte synthesizing step including a sulfidization treatment to sulfurize the LiOH in the precursor mixture and obtain LiHS, a de-sulfide-hydrogenating treatment to desorb a hydrogen sulfide from the LiHS and obtain Li.sub.2S, and a synthesizing treatment to make the Li.sub.2S to react with an auxiliary material; wherein a molar ratio of the LiOH with respect to the LiI and the LiBr, LiOH/(LiI+LiBr), in the precursor aqueous solution is 3 or more and less than 6.

A main object of the present disclosure is to provide a method for producing a sulfide solid electrolyte material, the method that allows a concentration of lithium halide to increase and that allows drying at a low temperature. The present disclosure achieves the object by providing a method for producing a sulfide solid electrolyte material, the method comprising: a drying step of drying a precursor aqueous solution containing LiI, LiBr, and LiOH to remove water and obtain a precursor mixture; and an electrolyte synthesizing step including a sulfidization treatment to sulfurize the LiOH in the precursor mixture and obtain LiHS, a de-sulfide-hydrogenating treatment to desorb a hydrogen sulfide from the LiHS and obtain Li.sub.2S, and a synthesizing treatment to make the Li.sub.2S to react with an auxiliary material; wherein a molar ratio of the LiOH with respect to the LiI and the LiBr, LiOH/(LiI+LiBr), in the precursor aqueous solution is 3 or more and less than 6.

A main object of the present disclosure is to provide a method for producing a sulfide solid electrolyte material, the method that allows a concentration of lithium halide to increase and that allows drying at a low temperature. The present disclosure achieves the object by providing a method for producing a sulfide solid electrolyte material, the method comprising: a drying step of drying a precursor aqueous solution containing LiI, LiBr, and LiOH to remove water and obtain a precursor mixture; and an electrolyte synthesizing step including a sulfidization treatment to sulfurize the LiOH in the precursor mixture and obtain LiHS, a de-sulfide-hydrogenating treatment to desorb a hydrogen sulfide from the LiHS and obtain Li.sub.2S, and a synthesizing treatment to make the Li.sub.2S to react with an auxiliary material; wherein a molar ratio of the LiOH with respect to the LiI and the LiBr, LiOH/(LiI+LiBr), in the precursor aqueous solution is 3 or more and less than 6.

A method for preparing high-purity lithium sulfide by using industrial-grade butyllithium includes the following steps: step A: under an inert gas condition, thoroughly mixing 1.5-2.5 g of lithium chloride, 0.5 L of an industrial-grade n-butyllithium solution (2.5 mol/L) and 1.5-2.5 L of n-hexane to obtain a mixed solution, and charging the mixed solution into a sealed container; step B: under the sealed condition, firstly introducing H.sub.2S gas into a gas-washing bottle through a submerged pipe at a rate of 10.5 L/h, then introducing into the mixed solution through the submerged pipe, controlling the reaction temperature at 25-40 C., and continuously stirring for reaction for 4-6 h to obtain a reaction slurry; and step C: under an inert gas condition, filtering the reaction slurry with a G3 sand core funnel to obtain a crude lithium sulfide solid wet material.

A method for preparing high-purity lithium sulfide by using industrial-grade butyllithium includes the following steps: step A: under an inert gas condition, thoroughly mixing 1.5-2.5 g of lithium chloride, 0.5 L of an industrial-grade n-butyllithium solution (2.5 mol/L) and 1.5-2.5 L of n-hexane to obtain a mixed solution, and charging the mixed solution into a sealed container; step B: under the sealed condition, firstly introducing H.sub.2S gas into a gas-washing bottle through a submerged pipe at a rate of 10.5 L/h, then introducing into the mixed solution through the submerged pipe, controlling the reaction temperature at 25-40 C., and continuously stirring for reaction for 4-6 h to obtain a reaction slurry; and step C: under an inert gas condition, filtering the reaction slurry with a G3 sand core funnel to obtain a crude lithium sulfide solid wet material.