Tantalum-doped cubic garnet structured Li7La3Zr<2-x>TaxO12 material synthesized via intermediate phase, and synthesis method thereof

A garnet and cubic technology, applied in the field of lithium ion battery electrolyte materials, can solve problems such as cost increase, loss of Li element, energy consumption, etc., and achieve the effects of good crystal form, reduced roasting time, and increased peak intensity

Inactive Publication Date: 2016-02-17
SHANGHAI POWER ENERGY STORAGE BATTERY SYST ENG TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The solid-state reaction method is a commonly used material preparation method in the industry, but in the existing solid-state reaction, it is basically necessary to roast the raw materials for a long time (6-12h), and the roasting temper

Method used

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  • Tantalum-doped cubic garnet structured Li7La3Zr&lt;2-x&gt;TaxO12 material synthesized via intermediate phase, and synthesis method thereof
  • Tantalum-doped cubic garnet structured Li7La3Zr&lt;2-x&gt;TaxO12 material synthesized via intermediate phase, and synthesis method thereof
  • Tantalum-doped cubic garnet structured Li7La3Zr&lt;2-x&gt;TaxO12 material synthesized via intermediate phase, and synthesis method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Weigh lanthanum zirconate, lanthanum oxide, lithium carbonate and lithium tantalate, the molar ratio of lanthanum zirconate to lanthanum oxide is 1:1, the molar ratio of lanthanum zirconate to lithium carbonate is 0.75:3.5, lanthanum zirconate The molar ratio with lithium tantalate is 3:2 to meet Li 7 La 3 Zr 1.5 Ta 0.5 o 12 The molar ratio of each metal element in the molecular formula. Place in a zirconium jar and add isopropanol as a ball milling medium, and mill for 12 hours.

[0031] (2) After ball milling, dry at 80°C for 4 hours, and then grind in an agate mortar for 30 minutes to obtain the raw material precursor.

[0032] (3) The precursor was roasted in a tube furnace at 900°C for 3 hours to obtain Li 7 La 3 Zr 1.5 Ta 0.5 o 12 A roasted product.

[0033] (4) The first-time roasted product was evenly ball-milled and pressed into tablets, and then second-time roasted at 1125°C for 10 hours to obtain the solid electrolyte Li 7 La 3 Zr 1.5 Ta 0....

Embodiment 2

[0035] (1) Weigh lanthanum zirconate, lanthanum hydroxide, lithium carbonate and lithium tantalate, the molar ratio of lanthanum zirconate and lanthanum oxide is 0.7:0.8, the molar ratio of lanthanum zirconate and lithium carbonate is 1:5, zirconate The molar ratio of lanthanum to lithium tantalate is 0.7:0.6 to meet the Li 7 La 3 Zr 1.4 Ta 0.6 o 12 The molar ratio of each metal element in the molecular formula. Place in a zirconium jar and add isopropanol as a ball milling medium, and mill for 12 hours.

[0036] (2) After ball milling, dry at 80°C for 4 hours, and then grind in an agate mortar for 30 minutes to obtain the raw material precursor.

[0037] (3) The precursor was roasted in a tube furnace at 900°C for 3 hours to obtain Li 7 La 3 Zr 1.4 Ta 0.6 o 12 A roasted product.

[0038] (4) The first-time roasted product was evenly ball-milled and pressed into tablets, and then second-time roasted at 1125°C for 10 hours to obtain the solid electrolyte Li 7 La 3 ...

Embodiment 3

[0044] (1) Weigh lanthanum zirconate, lanthanum hydroxide, lithium carbonate and lithium tantalate, the molar ratio of lanthanum zirconate and lanthanum hydroxide is 0.7:1.6, the molar ratio of lanthanum zirconate and lithium carbonate is 1:5, zirconium The molar ratio of lanthanum acid to lithium tantalate is 0.7:0.6 to meet the Li 7 La 3 Zr 1.4 Ta 0.6 o 12 The molar ratio of each metal element in the molecular formula. Place in a zirconium jar and add isopropanol as a ball milling medium, and mill for 12 hours.

[0045] (2) After ball milling, dry at 80°C for 4 hours, and then grind in an agate mortar for 30 minutes to obtain the raw material precursor.

[0046] (3) The precursor was roasted in a tube furnace at 900°C for 5 hours to obtain Li 7 La 3 Zr 1.4 Ta 0.6 o 12 A roasted product.

[0047] (4) The primary roasted product is ball-milled and pressed into tablets, and then secondarily roasted at 1125°C for 12 hours. To obtain the solid electrolyte Li 7 La 3 ...

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Abstract

The invention discloses a tantalum-doped cubic garnet structured Li7La3Zr<2-x>TaxO12 material synthesized via an intermediate phase, and a synthesis method thereof. The synthesis method comprises following steps: step 1, lanthanum zirconate, a lanthanum source, a lithium source, and a tantalum source used for doping are weighed at a metal element molar ratio according with that of Li7La3Zr<2-x>TaxO12, and the above materials are fully mixed; step 2, an obtained mixture is dried at 80 DEG C for 4 to 6h, and is grinded for 30min so as to obtain a raw material precursor; and step 3, the raw material precursor is subjected to roasting at 900 DEG C for 3 to 5h, so as to obtain a one time roasted product of Li7La3Zr<2-x>TaxO12, wherein x ranges from 0.25 to 1. According to the synthesis method, lanthanum zirconate is taken as a raw material; the tantalum-doped cubic garnet structured Li7La3Zr<2-x>TaxO12 material is convenient to prepare; technical route is simple; roasting time can be shortened greatly; energy consumption is reduced; lithium high temperature loss is reduced; and the synthesis method is suitable for large scale production.

Description

technical field [0001] The invention belongs to the field of electrolyte materials for lithium ion batteries, and relates to a preparation method of an inorganic oxide, in particular to a tantalum-doped garnet structure Li 7 La 3 Zr 2-x Ta x o 12 The method of preparation of the material. Background technique [0002] Rechargeable lithium batteries are playing an increasingly important role in the electronic product market and mobile power sources such as electric vehicles. With the development of society, the rapid popularization of mobile Internet and the wide application of Internet of Things technology, wearable devices have increasingly become an indispensable part of people's daily life, smart home, health care and sports and fitness. As a power source for wearable devices, lithium batteries are required to be light in weight, high in safety, and can be made into any shape. However, most of the organic liquid electrolytes currently used have potential safety haza...

Claims

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Application Information

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IPC IPC(8): H01M10/0562H01M10/058
CPCH01M10/0562H01M10/058H01M2300/0085Y02E60/10Y02P70/50
Inventor 王婷解晶莹王可王久林罗英
Owner SHANGHAI POWER ENERGY STORAGE BATTERY SYST ENG TECH
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