Mg<2+>, Al<3+>, Zr<4+> and S<2-> ion co-doped garnet type solid electrolyte

A solid electrolyte, garnet-type technology, applied in the direction of circuits, electrical components, secondary batteries, etc., can solve the problems that researchers of garnet-type solid electrolyte lithium ion migration mechanism have figured out, and achieve the promotion of lithium ion migration and force Weak, activation energy-reducing effect

Inactive Publication Date: 2015-07-15
NINGBO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The lithium ion migration mechanism of this garnet-type solid electrolyte has not yet been fully understood by researchers.

Method used

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  • Mg&lt;2+&gt;, Al&lt;3+&gt;, Zr&lt;4+&gt; and S&lt;2-&gt; ion co-doped garnet type solid electrolyte

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Embodiment 1: Li 2 CO 3 : La 2 o 3 :MgO:Al 2 o 3 : ZrO 2 ; Nb 2 o 5 : thiourea is 2.81: 1.375: 0.25: 0.06: 0.13: 0.875: 0.15 (molar ratio) ratio is evenly mixed, adds 3.2% 95% ethanol, ball mills 10 hours with the rotating speed of 250 rev / mins in ball mill, ball mill finishes Afterwards, dry in a 60°C vacuum oven (vacuum degree 20Pa) for 10 hours, take it out and grind it again in an agate mortar for 30 minutes, and the ground powder is heated to 220°C at a rate of 5°C / min for 3 hours, and then Raise the temperature at a rate of 5°C / min to 720°C for 10 hours, then raise the temperature at a rate of 3°C / min to 900°C for 11 hours to prepare a solid electrolyte powder. The powder is mixed with 2wt% binder PVC and kept under a pressure of 300MPa under a press for 5 minutes to form a thin sheet. The thin sheet is heated to 1000°C at a rate of 11°C / min and kept for 10 hours in an air atmosphere to make a lithium ion solid Electrolyte sheets.

Embodiment 2

[0012] Embodiment 2: Li 2 CO 3 : La 2 o 3 :MgO:Al 2 o 3 : ZrO 2 : Nb 2 o 5 : thiourea is 2.94: 1.3: 0.4: 0.07: 0.2: 0.83: 0.16 (molar ratio) ratio is uniformly mixed, adds 5.5% 95% ethanol, ball mills 15 hours with the rotating speed of 380 rev / mins in ball mill, ball mill finishes Afterwards, dry in a vacuum oven (vacuum degree 95Pa) at 80°C for 30 hours, take it out and re-grind in an agate mortar for 30 minutes, and the ground powder is heated to 250°C at a rate of 6°C / min and kept for 5 hours, and then Raise the temperature at a rate of 8°C / min to 780°C for 10 hours, then raise the temperature at a rate of 7°C / min to 1000°C for 15 hours to prepare a solid electrolyte powder. The powder is mixed with 5wt% binder PVC and kept under a pressure of 450MPa under a press for 2 minutes to form a thin sheet. The thin sheet is heated to 1050°C at a rate of 15°C / min and kept for 10 hours in an air atmosphere to make a lithium-ion solid electrolyte. Flakes.

Embodiment 3

[0013] Embodiment 3: with Li 2 CO 3 : La 2 o 3 :MgO:Al 2 o 3 : ZrO 2 : Nb 2 o 5 : thiourea is 2.7: 1.45: 0.1: 0.05: 0.1: 0.9: 0.12 (molar ratio) ratio is evenly mixed, adds 3% 95% ethanol, ball mills 20 hours with the rotating speed of 300 rev / mins in ball mill, ball mill finishes Afterwards, dry in a 70°C vacuum oven (vacuum degree 50Pa) for 20 hours, take it out and re-grind in an agate mortar for 10 minutes, and the ground powder is heated to 270°C at a rate of 9°C / min and kept for 5 hours, and then Raise the temperature at a rate of 10°C / min to 800°C for 7 hours, then raise the temperature at a rate of 2°C / min to 1050°C for 12 hours to prepare a solid electrolyte powder. The powder is mixed with 1wt% binder PVA and kept under a pressure of 300MPa under a press for 6 minutes to form a thin sheet, which is heated to 1100°C at a rate of 15°C / min and kept for 18 hours in an air atmosphere to make a lithium ion solid Electrolyte sheets.

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Abstract

The invention discloses an Mg<2+>, Al<3+>, Zr<4+> and S<2-> ion co-doped garnet type solid electrolyte Li5La3Nb2O12 which is characterized by comprising the stoichiometric equation: Li[5+x+2y+z]La[3-x]MgxAlyZrzNb[2-y-z]O[12-m]Sm, wherein x is equal to 0.1-0.5, y is equal to 0.1-0.2, z is equal to 0.1-0.2, and m is equal to 0.1-0.3; and the solid electrolyte is formed by uniformly mixing Li2CO3, La2O3, MgO, Al2O3, ZrO2, Nb2O5 and thiourea in the molar ratio of (2.7-3.05):(1.25-1.45):(0.1-0.5):(0.05-0.1):(0.1-0.2):(0.8-0.9):(0.1-0.3), and ball milling, pressing and sintering. According to the invention, the lithium-ion conductivity greater than 10<-4>S / cm can be obtained at room temperature.

Description

technical field [0001] The invention relates to the field of manufacturing a solid lithium ion electrolyte. Background technique [0002] Lithium-ion batteries have absolute advantages such as high volume, high weight-to-energy ratio, high voltage, low self-discharge rate, no memory effect, long cycle life, and high power density. They have an annual share of more than 30 billion US dollars in the global mobile power market and far exceed other The market share of batteries is the most promising chemical power source [Wu Yuping, Wan Chunrong, Jiang Changyin, Lithium-ion Secondary Batteries, Beijing: Chemical Industry Press, 2002.]. At present, most of the lithium-ion secondary batteries at home and abroad use liquid electrolytes. Liquid lithium-ion batteries have some disadvantages, such as: liquid organic electrolytes may leak, and may explode at too high a temperature, causing safety accidents, and cannot be used in some applications. Occasions with high safety requiremen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M10/0562
CPCY02E60/10
Inventor 水淼杨天赐舒杰程亮亮冯琳任元龙郑卫东高珊
Owner NINGBO UNIV
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