NASICON lithium-ion solid electrolyte synergistically doped with F<-> and Y<3+> ions and preparation method thereof

A solid electrolyte and lithium ion technology, applied in the manufacture of electrolyte batteries, non-aqueous electrolyte batteries, circuits, etc., to achieve the effect of weakening the bonding force, improving conductivity, and enhancing migration ability

Inactive Publication Date: 2015-11-18
XI'AN INST OF OPTICS & FINE MECHANICS - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The only solid electrolyte currently used commercially is Li 1.3 Al 0.3 Ti 1.7 (PO 4 ) 3 , but due to the price change problem of Ti, its application is limited, and LiZr, which is also a NASICON (sodium fast ion conductor) system 2 (PO 4 ) 3 There is no problem of price change

Method used

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  • NASICON lithium-ion solid electrolyte synergistically doped with F&lt;-&gt; and Y&lt;3+&gt; ions and preparation method thereof
  • NASICON lithium-ion solid electrolyte synergistically doped with F&lt;-&gt; and Y&lt;3+&gt; ions and preparation method thereof
  • NASICON lithium-ion solid electrolyte synergistically doped with F&lt;-&gt; and Y&lt;3+&gt; ions and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] In this example, according to Y(NO 3 ) 3 ·6H 2 O:LiF:ZrOCl 2 ·8H 2 O:(NH 4 ) 2 HPO 4 :LiNO 3 Mix evenly in a ratio of 0.1:0.1:1.9:3.0:1.0 (molar ratio), put it into a 150ml beaker, add 100ml of deionized water, heat and stir on a magnetic heating stirrer at 60°C for 10h, and dry to obtain the precursor , with AR isopropanol as the ball milling solvent, ball milled in a ball mill for 10 hours at a speed of 100 rpm, after the ball milling was finished, it was dried in a vacuum oven at 60°C (vacuum degree at 60Pa) for 5 hours, and after it was taken out, it was placed in an agate mortar Re-grind for 30 minutes, and the ground powder is heated to 900°C at a rate of 3°C / min and kept for 10 hours to make a solid electrolyte powder, whose chemical formula is Li 1.0 Y 0.1 Zr 1.9 P 3 o 11.9 f 0.1. The powder was mixed under a press to form a sheet under a pressure of 200 MPa for 2 minutes, and the sheet was heated to 1210° C. at a rate of 3° C. / min for 10 hours to ...

Embodiment 2

[0024] In this example, according to Y(NO 3 ) 3 ·6H 2 O:LiF:ZrOCl 2 ·8H 2 O:(NH 4 ) 2 HPO 4 :LiNO 3 Mix evenly in a ratio of 0.1:0.2:1.9:3.0:0.9 (molar ratio), put it into a 150ml beaker, add 100ml of deionized water, heat and stir on a magnetic heating stirrer at 80°C for 20h, and dry to obtain the precursor , with AR isopropanol as the ball milling solvent, ball milled for 20 hours at a speed of 200 rpm in a ball mill, dried in a vacuum oven at 80°C (vacuum degree at 100Pa) for 10 hours after ball milling, and put it in an agate mortar after taking it out Re-grind for 60 minutes, and the ground powder is heated at a rate of 5°C / min to 1000°C for 10 hours to make a solid electrolyte powder, whose chemical formula is Li 0.9 Y 0.2 Zr 1.9 P 3 o 11.8 f 0.2 . The powder was mixed under a press to form a sheet under a pressure of 200 MPa for 6 minutes, and the sheet was heated to 1210° C. at a rate of 5° C. / min for 30 hours to make a lithium ion solid electrolyte shee...

Embodiment 3

[0026] In this example, Y(NO 3 ) 3 ·6H 2 O:LiF:ZrOCl 2 ·8H 2 O:(NH 4 ) 2 HPO 4 :LiNO 3 Mix evenly in a ratio of 0.2:0.1:1.8:3.0:1.1 (molar ratio), put it into a 150ml beaker, add 100ml of deionized water, heat and stir on a magnetic heating stirrer at 70°C for 15h, and dry to obtain the precursor , with AR isopropanol as the ball milling solvent, ball milled in a ball mill for 25 hours at a speed of 300 rpm, dried in a vacuum oven at 70°C (vacuum degree at 90Pa) for 15 hours after ball milling, and put it in an agate mortar after taking it out Re-grind for 50 minutes, and the ground powder is heated to 1150°C at a rate of 5°C / min and kept for 20 hours to make a solid electrolyte powder, whose chemical formula is Li 1.1 Y 0.2 Zr 1.8 P 3 o 11.9 f 0.1 . The powder was mixed under a press to form a sheet under a pressure of 300 MPa for 4 minutes, and the sheet was heated to 1210° C. at a rate of 5° C. / min for 30 hours to make a lithium-ion solid electrolyte sheet. T...

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Abstract

The invention relates to a NASICO lithium-ion solid electrolyte synergistically doped with F<-> and Y<3+> ions and a preparation method thereof. The stoichiometric formula is shown as Li<1+x-y>Y<x>Zr<2-x>P3O<12-y>F<y>, wherein x is equal to 0.1 to 0.5, and y is equal to 0.1 to 0.2. The preparation method comprises the following steps of: uniformly mixing Y(NO3)3.6H2O, LiF, ZrOC12.8H2O, (NH4)2HPO4 and LiNO3 according to a mole ratio of (0.1-0.5):(0.1-0.2):(1.5-1.9):3.0:(0.9-1.4); and carrying out heating, stirring, stoving, ball milling, pressing and sintering. The lithium-ion conductivity of the prepared solid electrolyte thin film at a room temperature is greater than 10<-4>S / cm.

Description

technical field [0001] The invention belongs to the field of manufacturing lithium-ion solid electrolytes, in particular to a F - and Y 3+ Ion cooperatively doped NASICON type lithium ion solid electrolyte and preparation method thereof. Background technique [0002] With the development of society, the demand and dependence of human society on electric energy are getting stronger and stronger. The continuous depletion of traditional fossil energy and the massive emission of carbon dioxide have brought serious threats to people's living environment. People pay more and more attention to the development of renewable energy such as solar energy, wind energy, and water conservancy. With the rapid expansion of my country's new energy power generation scale, wind power, hydropower, photovoltaic power generation, short-term power regulation, peak shaving and valley filling, and pure electric vehicle access will form an industrial energy storage market of more than 200 billion y...

Claims

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Application Information

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IPC IPC(8): H01M10/0562H01M10/058
CPCH01M10/0562H01M10/058Y02E60/10Y02P70/50
Inventor 张洪李文龙王浩静苏洲刘欢杨利青
Owner XI'AN INST OF OPTICS & FINE MECHANICS - CHINESE ACAD OF SCI
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