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Oxide solid electrolytes based on lithium halide-doping and low-temperature sintering method thereof

A solid electrolyte, low-temperature sintering technology, applied in electrolytes, circuits, electrical components, etc., can solve the problems of increasing the solid-solid interface resistance, deteriorating battery performance, and deviating from the balance ratio of compound components, reducing grain boundary resistance and reducing raw materials. Easy to obtain, avoid the effect of lithium volatilization

Inactive Publication Date: 2018-02-23
YANSHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, at present, this type of electrolyte needs to be sintered at high temperature (usually more than 900°C) for a long time (usually more than 12 hours) to reduce the grain boundary resistance, which not only causes the volatilization of lithium in the material to make the compound composition deviate from the equilibrium ratio, but also causes the electrolyte to be sintered at high temperature. Diffusion reaction with the electrode material increases the solid-solid interfacial impedance and sharply deteriorates the performance of the battery

Method used

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  • Oxide solid electrolytes based on lithium halide-doping and low-temperature sintering method thereof
  • Oxide solid electrolytes based on lithium halide-doping and low-temperature sintering method thereof
  • Oxide solid electrolytes based on lithium halide-doping and low-temperature sintering method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1.2223g Li 2 CO 3 (>99%), 2.3412g La 2 o 3 (>99%), 1.0306g ZrO 2 (>99%), 0.4288g TaCl 5 (>99%) and 0.0603g Al 2 o 3 (>99%) mixed in the glove box, under the protection of high-purity argon (99.999%), with a ball mill at 200 rpm, ball milled for 8h, and then the powder after ball milling was put into an alumina crucible and placed in a muffle In the furnace, heat up to 900°C at a heating rate of 2.5°C / min, keep the temperature for 5 hours, and finally cool to room temperature in the furnace. The cooled block was taken out of the crucible, put into a glove box and manually ground into a powder with a particle size of 20 μm in a mortar to obtain a cubic phase Li 6.15 al 0.2 La 3 Zr 1.75 Ta 0.25 o 12 Solid electrolyte powder. Then 0.79g LiCl (>99%) was dissolved in 1ml deionized water to prepare LiCl solution, which was mixed with the prepared cubic phase Li 6.15 al0.2 La 3 Zr 1.75 Ta 0.25 o 12 Sufficient and uniform wetting, cold pressing into sheets and ...

Embodiment 2

[0027] The purchased commercial cubic phase Li 6.75 La 3 Zr 1.75 Ta 0.25 o 12 Put the solid powder electrolyte into a glove box, and carry out ball milling under the protection of high-purity argon (99.999%). The ball milling adopts a low speed of 100 rpm, and the ball milling time is 1 hour, and is ground into a powder with a particle size of 18 μm. Then 0.26g LiBr was dissolved in 1ml ethanol to prepare LiBr solution, which was mixed with 5g cubic phase Li after ball milling 6.75 La 3 Zr 1.75 Ta 0.25 o 12 The solid powder electrolyte is fully and uniformly wetted, cold-pressed into a sheet, and hot-pressed and sintered at 250 ° C and 20 MPa for 0.5 hours to prepare a lithium bromide-doped oxide solid electrolyte.

[0028] Adopt the impedance test method test described in embodiment 1, such as image 3 As shown, the room temperature conductivity of the ionic conductor can be calculated from the intercept of the oblique line in the curve on the horizontal axis to be a...

Embodiment 3

[0030] 1.3762gLi 2 CO 3 (>99%), 2.3641g La 2 o 3 (>99%), 1.1983g ZrO 2 (>99%) and 0.0591g Al 2 o 3 (>99%) mixed in the glove box, under the protection of high-purity argon (99.999%), use a ball mill at 100 rpm, ball mill for 12h, then put the ball-milled powder into a corundum crucible and place it in a muffle furnace , heated to 850°C at a heating rate of 2°C / min, held for 6 hours, and finally cooled to room temperature with water. The cooled block was taken out from the crucible, put into a glove box and manually ground into powder with a mortar to obtain cubic phase Li 7.7 La 3 Zr 2 al 0.24 o 12 Solid electrolyte powder. 0.52g LiI is dissolved in the tetrahydrofuran solution of the 2M lithium borohydride of 1ml and is formulated into LiI solution, and it is mixed with the cubic phase Li that makes 7.7 La 3 Zr 2 al 0.24 o 12 Sufficient and uniform wetting, cold pressing into sheets and hot pressing and sintering at 100 ° C and 60 MPa for 5 hours to prepare a ...

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Abstract

Provided is an oxide solid electrolyte based on lithium halide-doping. The oxide solid electrolyte is a lithium solid electrolyte, wherein electrolytes in a perovskite type, an NASICON type and a garnet type are taken as substrates, and a lithium halide solution and the oxide solid electrolytes are compounded and sintered at a low temperature. A preparing method comprises the steps that LATP, LLTOand LLZO solid electrolytes are subjected to ball-milling, or self-produced cubic-phase lithium-lanthanum-zirconium-oxygen solid electrolyte powder is subjected to ball-milling and sintered to prepare cubic-phase LLZO solid electrolyte powder, an LIX solution is added to the solid electrolyte powder, and the mixture is pressed into a slice or painted into a membrane, then placed in a muffle furnace at a low temperature of 100-250 DEG C and sintered for 1-10 hours. The oxide solid electrolyte is simple in technology and low in cost, and the prepared lithium solid electrolyte has high ionic conductivity and high repeatability; the oxide solid electrolyte can be on a par with electrolytes prepared through a traditional high-temperature technology, and meanwhile low-temperature sintering canavoid high-temperature diffusion reaction with cathode materials.

Description

technical field [0001] The invention belongs to the field of new energy materials, in particular to a solid electrolyte and a preparation method thereof. Background technique [0002] Among various commercial rechargeable and dischargeable chemical energy storage devices, lithium-ion batteries have the characteristics of high energy density and long service life. . However, the volatile, flammable and explosive organic electrolyte is the main factor causing the safety problem of lithium ions. The use of solid electrolyte instead of electrolyte to develop all-solid-state batteries is the fundamental way to solve the battery safety problem. Solid electrolyte has high thermal stability, wide operating temperature, and wide electrochemical stability window; its high density, high strength and hardness make it able to effectively delay the growth and puncture of lithium dendrites. However, the existing inorganic lithium solid electrolytes still have problems such as low room te...

Claims

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Application Information

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IPC IPC(8): H01M10/0562
CPCH01M10/0562H01M2300/0071Y02E60/10
Inventor 张隆张赵帅
Owner YANSHAN UNIV
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