Oxide ceramic composite solid electrolyte, its preparation method and application

An oxide ceramic and solid electrolyte technology, applied in the field of electrochemistry, can solve problems such as deterioration, difficulty in compensating for the volume change of lithium deintercalation of electrode materials, safety problems, etc., so as to inhibit the formation of lithium dendrites and improve the interface between electrolyte and electrode. Good contact and thermal stability

Active Publication Date: 2022-04-19
ZHEJIANG NARADA POWER SOURCE CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The existing technology adopts a lithium-ion battery composite solid electrolyte and its preparation method, and prepares a composite film of an inorganic fast ion conductor and a polymer by electrospinning and impregnation, but it is difficult to compensate for the electrode material only by virtue of the elasticity of the polymer. The volume change that occurs during the lithium-deintercalation process, the interface problem still exists and will deteriorate with the charge-discharge cycle
There are also existing technologies that use a small amount of liquid electrolyte to improve the electrode / electrolyte interface contact problem in solid-state batteries, but the presence of electrolyte still poses safety issues

Method used

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  • Oxide ceramic composite solid electrolyte, its preparation method and application
  • Oxide ceramic composite solid electrolyte, its preparation method and application
  • Oxide ceramic composite solid electrolyte, its preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Preparation of garnet-type ceramic electrolyte Li by traditional solid-state sintering method 6.4 La 3 Zr 1.4 Ta 0.6 o 12 . Weigh Li according to the stoichiometric ratio 2 CO 3 , La 2 o 3 , ZrO 2 and Ta 2 o 5 , and 30ml of isopropanol were added into the ball mill jar, and ball milled at a speed of 250rpm for 20h. In order to compensate for the loss of lithium volatilization during high-temperature calcination, set Li 2 CO3 10% excess. After the ball milling, the obtained mixed solution was dried in a blast oven at 80° C. for 12 hours to obtain a precursor powder. The obtained powder was transferred to a porcelain boat and calcined in a tube furnace at 900 °C for 8 h in an air atmosphere. The pre-sintered powder was ground again, and then calcined at 1100 °C in air for 24 h to obtain cubic Li 6.4 La 3 Zr 1.4 Ta 0.6 o 12 .

[0030] Weigh 0.8 g of polyethylene oxide and 0.8 g of polypropylene carbonate and add them into 50 ml of anhydrous acetonitrile...

Embodiment 2

[0035] Preparation of garnet-type ceramic electrolyte Li by traditional solid-state sintering method 6.2 al 0.2 La 3 Zr 1.8 Ta 0.2 o 12 . Weigh LiOH, Al according to stoichiometric ratio 2 o 3 , La 2 o 3 , ZrO 2 and Ta 2 o 5 , and 50ml of isopropanol were added into a ball mill jar, and ball milled at a speed of 300rpm for 24h. In order to compensate for the loss of lithium volatilization during high-temperature calcination, an excess of 15% LiOH is set. After the ball milling, the obtained mixture was dried in a blast oven at 60° C. for 8 hours to obtain a precursor powder. The resulting powder was transferred to a porcelain boat and calcined at 800 °C for 6 h in an air atmosphere in a tube furnace. The pre-sintered powder was ground again, and then calcined at 1050 °C in air for 20 h to obtain cubic Li 6.2 al 0.2 La 3 Zr 1.8 Ta 0.2 o 12 .

[0036] Weigh 1.4 g of polyethylene oxide and 0.2 g of polypropylene carbonate and add them into 50 ml of N-methylpy...

Embodiment 3

[0041] Preparation of garnet-type ceramic electrolyte Li by traditional solid-state sintering method 6.35 La 2.95 Rb 0.05 Zr 1.2 Ta 0.8 o 12 . Weigh LiOH·H according to the stoichiometric ratio 2 O, La 2 o 3 , Rb 2 CO 3 , ZrO 2 and Ta 2 o 5 , and 50ml of isopropanol were added into a ball mill jar, and ball milled at a speed of 200rpm for 16h. In order to compensate for the loss of lithium volatilization during high-temperature calcination, an excess of 10% of the lithium source is set. After the ball milling, the obtained mixture was dried in a blast oven at 60° C. for 24 hours to obtain a precursor powder. The obtained powder was transferred to a porcelain boat and calcined in a tube furnace at 900 °C for 12 h in an air atmosphere. The pre-sintered powder was ground again, and then calcined at 1200 °C in air for 24 h to obtain cubic Li 6.35 La 2.95 Rb 0.05 Zr 1.2 Ta 0.8 o 12 .

[0042] Weigh 1.12 g of polyethylene oxide and 0.48 g of polypropylene carbo...

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Abstract

The invention provides an oxide ceramic composite solid state electrolyte, its preparation method and application. Oxide ceramic composite solid electrolyte, comprising the following components: 20wt.% to 50wt.% tantalum doped garnet type oxide ceramics; 30wt.% to 60wt.% polymer electrolyte; 10wt.% to 30wt.% Lithium salt; and 5wt.%-20wt.% fluorine-containing imidazole ionic liquid. The preparation method of the oxide ceramic composite solid state electrolyte comprises a preparation step, a sintering step and a mixing step. Preparation steps: weigh lithium source, La 2 o 3 , ZrO 2 and Ta 2 o 5 , and isopropanol are added together into a ball mill jar for ball milling; sintering step: the material obtained after ball milling is removed from the isopropanol, pre-sintered, and then secondary sintered after grinding again to obtain oxide ceramics; and mixing step: mixing tantalum Mixed garnet-type oxide ceramics, polymer electrolyte, lithium salt and ionic liquid are added to an organic solvent, dispersed evenly, poured into a mold, and the organic solvent is volatilized to obtain an oxide-ceramic composite electrolyte.

Description

technical field [0001] The invention relates to the technical field of electrochemistry, in particular to an oxide ceramic composite solid state electrolyte, its preparation method and its application. Background technique [0002] Lithium-ion batteries have become the most widely used rechargeable batteries due to their high specific energy, long cycle life, high rated voltage, low self-discharge rate, and environmental protection. However, the current lithium-ion batteries generally use organic electrolytes, which have problems such as easy decomposition at high temperatures, flammability, and narrow electrochemical windows, which are key factors restricting battery safety and energy density. Compared with traditional electrolytes, solid-state electrolytes do not contain flammable and volatile components, have good compatibility with lithium metal, have a wide electrochemical stability window, and have a large room for energy density improvement. In addition, solid-state ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M10/056H01M10/052H01M10/0525H01M12/08
CPCY02E60/10
Inventor 屠芳芳郭锋刘月学蔡若愚李小平
Owner ZHEJIANG NARADA POWER SOURCE CO LTD
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