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Sulfide solid electrolyte based on oxygen doping and preparation method of sulfide solid electrolyt

A solid electrolyte, sulfide technology, applied in the direction of solid electrolyte, non-aqueous electrolyte, non-aqueous electrolyte battery, etc., can solve the problems of sensitivity, poor electrochemical stability of cathode and metal lithium, etc., to overcome instability, low price and stable performance Effect

Active Publication Date: 2018-09-04
YANSHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Among inorganic solid electrolytes, compared with oxide solid electrolytes, sulfide electrolytes have higher ionic conductivity and deformability, but sulfide solid electrolytes are more sensitive to air, and have poor electrochemical stability to positive electrodes and metal lithium.

Method used

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  • Sulfide solid electrolyte based on oxygen doping and preparation method of sulfide solid electrolyt
  • Sulfide solid electrolyte based on oxygen doping and preparation method of sulfide solid electrolyt
  • Sulfide solid electrolyte based on oxygen doping and preparation method of sulfide solid electrolyt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 0.4359gLi 2 S (99.999%), 0.3710gP 2 S 5 (99.999%) and 0.0323gP 2 o 5 (99.999%) and 0.1608gLiCl (99.999%) are put into a mortar and mixed fully in an inert gas-protected glove box, and the mixed powder is pressed into tablets using a tablet press, and the pressed tablets are put into a closed-ended In the quartz tube, evacuate to 0.1 Pa, and seal the quartz tube; then put the sealed quartz tube into the muffle furnace, heat it to 400 ° C at a heating rate of 0.3 ° C / min, keep it for 12 hours, and finally in the Cool in the furnace. The cooled block was taken out from the quartz tube, put into a glove box and manually ground into powder with a mortar to obtain cubic phase Li 6 P.S. 4.4 o 0.6 Cl sulfide solid electrolyte.

[0020] After the above-mentioned sulfide solid electrolyte is sealed with a polyimide film, X-ray diffraction (XRD) test is carried out, and the test adopts SmartLab (40kV, 40mA, Cu Ka, ), the test range is 10°~80°, and the rate is 4° / min. ...

Embodiment 2

[0025] 0.4727gLi 2 S (99.999%), 0.2365gP 2 S 5(99.999%) and 0.1404gAs 2 o 3 (99.999%) and 0.1504gLiCl (99.999%) are put into the mortar and thoroughly mixed in the glove box protected by inert gas, and the mixed powder is pressed into tablets using a tablet press, and the pressed tablets are put into a closed-end In the quartz tube, evacuate to 0.1 Pa, and seal the quartz tube; then put the sealed quartz tube into the muffle furnace, heat it to 450 °C at a heating rate of 0.3 °C / min, keep it for 12 hours, and finally furnace Internally cool to room temperature; the cooled block is taken out from the quartz tube, put into a ball mill jar, the ball mill adopts a low speed of 100 rpm, and the ball milling time is 2 hours, and ball milled under the protection of high-purity argon (99.999%), Cubic Li 6.8 As 0.4 P 0.6 S 4.4 o 0.6 Cl sulfide solid electrolyte.

[0026] The above-mentioned sulfide solid electrolyte was tested by the impedance test method described in Example...

Embodiment 3

[0028] 0.4432gLi 2 S (99.999%), 0.2218gP 2 S 5 (99.999%) and 0.1939gSb 2 o 3 (99.999%) and 0.1411LiCl (99.999%) were put into a mortar and mixed thoroughly in an inert gas-protected glove box, and the mixed powder was pressed into tablets using a tablet press, and the pressed tablets were put into a closed-ended In the quartz tube, evacuate to 0.1 Pa, and seal the quartz tube; then put the sealed quartz tube into the muffle furnace, heat it to 500 °C at a heating rate of 0.3 °C / min, keep it for 12 hours, and finally furnace Internal cooling to room temperature; the cooled block is taken out from the quartz tube, put into a ball mill jar, the ball mill adopts a low speed of 200 rpm, and the ball milling time is 2 hours, and ball milled under the protection of high-purity argon (99.999%), Cubic Li 6.8 Sb 0.4 P 0.6 S 4.4 o 0.6 Cl sulfide solid electrolyte.

[0029] The above-mentioned sulfide solid electrolyte was tested by the impedance test method described in Example...

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Abstract

The invention provides a sulfide solid electrolyte based on oxygen doping. The sulfide solid electrolyte is prepared from the chemical ingredients, in percentage by mass: 36-60% of lithium sulfide orlithium selenide, 18-48% of phosphorus pentasulfide or phosphorus selenide, 1-23% of metal oxide or specific nonmetallic oxide and 8-37% of lithium chloride, lithium bromide or lithium iodide. The preparation method of the sulfide solid electrolyte mainly comprises the steps that the raw materials are sufficiently blended and subjected to tabletting, then placed in a quartz tube to be burned and sealed, the product is placed in a muffle furnace and heated to be 400-600 DEG C at a slow heating rate, the optimal heating rate is 0.3 DEG C / minute, heat preservation is conducted for 12-48 hours, and then the product is cooled to reach the room temperature; and the product is ground to be powder, and the sulfide solid electrolyte based on oxygen doping is prepared. The sulfide solid electrolyteis easy to prepare and high in repeatability, the prepared solid electrolyte has the high ionic conductivity and good stability to the air and positive and negative electrodes.

Description

technical field [0001] The invention belongs to the field of new materials, in particular to a solid electrolyte and a preparation method thereof. Background technique [0002] In recent years, lithium-ion batteries have been widely used as a secondary battery in the fields of mobile phones, electric vehicles, notebook computers and cameras. However, traditional liquid lithium-ion batteries widely use flammable and explosive organic electrolytes, and safety has become a key issue restricting the development of traditional lithium-ion batteries. In recent years, all-solid-state lithium-ion batteries have attracted widespread attention. Since inorganic solid electrolytes not only have the advantages of non-flammability and high temperature resistance, but also have high electrochemical stability, inorganic solid electrolytes are used instead of liquid organic electrolytes. , the development of lithium all-solid-state batteries can well solve the above safety problems. At the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/0562H01M10/052
CPCH01M10/052H01M10/0562H01M2300/0068Y02E60/10
Inventor 张隆张志霞
Owner YANSHAN UNIV
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