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Cubic-phase sulfide and preparation method thereof

A sulfide, cubic phase technology, applied in chemical instruments and methods, lithium compounds, aluminum compounds, etc., can solve problems such as hindering preparation and use, and achieve the effect of saving production costs and simplifying preparation steps

Inactive Publication Date: 2018-07-03
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, the cubic phase argentite-type Li 7 P.S. 6 It has high ionic conductivity, but it only exists stably in the temperature range above 200°C; while the ionic conductivity of the orthorhombic phase structure is only ~10 -6 S cm -1 ; To obtain a cubic phase with high ionic conductivity, quenching treatment is often required, which greatly hinders the high ionic conductivity of Li 7 P.S. 6 preparation and use

Method used

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  • Cubic-phase sulfide and preparation method thereof
  • Cubic-phase sulfide and preparation method thereof
  • Cubic-phase sulfide and preparation method thereof

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preparation example Construction

[0034] The preparation method of above-mentioned cubic phase sulfide is: Li 2 S, M 2 S a ,P 2 S 5 Weigh under an inert atmosphere with a molar ratio of y:x:(1-x), and mix them evenly, and carry out solid-phase synthesis of raw materials under anaerobic conditions at 400°C to 650°C for 8h to 18h, so as to prevent reactants from being mixed with air Oxygen or moisture in the reaction to generate impurities, until complete reaction to generate Li y m x P 1－x S 6 ; The oxygen-free condition can be a vacuum less than 100Pa, or an inert gas such as nitrogen or argon.

[0035] And in the raw material Li 2 S-M 2 S a -P 2 S 5 There are crystal phases with various structures in the system, uniform mixing is very important, uneven mixing will cause inconsistency of components, and impurities are likely to be generated; at the same time, the mixing process is also accompanied by the refinement process of raw materials, which is conducive to later vulcanization The synthesis of ...

Embodiment 1

[0037] In an argon-protected glove box, the Li 2 S, M 2 S a ,P 2 S 5 Weigh at the molar ratio of (7+5x-ax):x:(1-x), and mix them as raw materials; in this example, a is the valence of M, M is B, and x is 0.1;

[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 220 r / min, and obtain a mixed powder after 24 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-state reaction is carried out at 400°C for 18 hours, and the temperature is naturally cooled to obtain the product Li (7+5x－ax) m x P 1－x S 6 , in this example, the product is Li 7.2 B 0.1 P 0.9 S 6 .

[004...

Embodiment 21

[0045] First, in an argon-protected glove box, the Li 2 S, B 2 S 3 、Al 2 S 3 ,P 2 S 5 Weigh with the molar ratio of 7.4:0.1:0.1:0.9, and mix as raw material;

[0046] Put the raw materials and zirconia balls into a zirconia-substrated ball mill tank with a capacity, seal the container, perform ball mill mixing at a speed of 300r / min, and obtain a mixed powder after 18 hours;

[0047] Put the mixed powder in the glove box, take it out, shape it under the 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-state reaction is carried out at 400°C for 18 hours, and the temperature is naturally cooled to obtain the product Li 7.4 B 0.1 Al 0.1 P 0.8 S 6 .

[0048] In the glove box, the product was taken out from the sealed glass tube, crushed and ground in a mortar, and a powder sample with a...

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Abstract

The invention discloses a cubic-phase sulfide and a preparation method thereof. The chemical formula of the cubic-phase sulfide is LiyMxP(1-x)S6, where M is an element of the group IIIA or IVA, with avalence of +a; x is greater than 0 and less than or equal to 0.4; and y=7+5x-ax. In the invention, by replacing partial P2S5 in the raw material with the sulfide of the group IIIA or IVA, the prepared sulfide solid electrolyte still can be kept in a cubic phase at room temperature while having an ionic conductivity over 0.31mS / cm; the preparation method does not need shock cooling, thus the preparation steps are simplified, and the production cost is saved; and the preparation method is more suitable for an all-solid-state battery.

Description

technical field [0001] The invention belongs to the field of all-solid-state lithium batteries, and more specifically relates to a cubic phase sulfide and a preparation method thereof. Background technique [0002] In recent years, with the rapid popularization of information devices and communication devices such as computers, cameras and mobile phones, the development of batteries used as power sources for these devices has attracted more and more attention from the industry. In addition, in the automotive industry, batteries with high power density and high capacity required for pure electric vehicles or hybrid electric vehicles are also being vigorously developed. Among the current various battery systems, lithium-ion batteries have attracted much attention due to their high energy density. [0003] Lithium-ion batteries currently on the market use a flammable organic solution as the electrolyte, which requires the installation of devices to deal with temperature rise c...

Claims

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Application Information

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IPC IPC(8): C01D15/00C01G17/00C01F7/00H01M10/0562H01M10/0525
CPCH01M10/0525H01M10/0562C01D15/00C01G17/006C01P2002/72C01P2002/30C01P2006/40C01F7/78Y02E60/10
Inventor 谢佳孙玉龙彭林峰
Owner HUAZHONG UNIV OF SCI & TECH
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