Ceramic solid electrolyte and preparation method thereof

A solid-state electrolyte and solid-state electrolysis technology, which is applied in electrolytes, circuits, electrical components, etc., can solve the problems of large-scale preparation difficulties, low electrolyte conductivity, and low sintering temperature, and achieve rapid drying process, high conductivity, and high sintering temperature. low effect

Inactive Publication Date: 2016-03-16
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The purpose of the present invention is to solve the problems of low electrolyte conductivity, high sintering temperature, and difficulty in mass production, and provides a ceramic solid electrolyte

Method used

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  • Ceramic solid electrolyte and preparation method thereof
  • Ceramic solid electrolyte and preparation method thereof
  • Ceramic solid electrolyte and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] First take 600ml of deionized water, add 5.53g of citric acid to dissolve, then press Li 7 La 3 Zr 2 o 12 The stoichiometric ratio weighs 4.45g of lithium nitrate, 4.68g of lanthanum nitrate, and 1.12g of zirconium oxynitrate into the above-mentioned citric acid solution, wherein the excess of lithium salt is 10%, stirs the mixed solution for 12h, and then sprays and dries it. The spray feed rate was set at 2r / min, the outlet temperature of the nozzle was 180°C, and the blast pressure was 0.2MPa. The obtained spray material is heated up to 800°C at 1°C / min for sintering, and the sintering time is 6h.

[0032] Morphological characterization of the obtained solid electrolyte and its precursor, such as figure 1 , 2 As shown, it can be seen that the precursor material is spherical, and the morphology changes significantly after sintering, which is due to the increase in crystallinity of the electrolyte at high temperature.

[0033] Carry out XRD test to gained electro...

Embodiment 2

[0036] First take 600ml of deionized water, add 5.53g of citric acid to dissolve, then press Li 7 La 3 Zr 2 o 12 The stoichiometric ratio weighs 4.45g of lithium nitrate, 4.68g of lanthanum nitrate, and 1.12g of zirconium oxynitrate into the above-mentioned citric acid solution, wherein the excess of lithium salt is 10%, stirs the mixed solution for 12h, and then sprays and dries it. The spray feed rate was set at 2r / min, the outlet temperature of the nozzle was 180°C, and the blast pressure was 0.2MPa. The obtained sprayed material is heated up to 800°C at 5°C / min for sintering, and the sintering time is 6h.

Embodiment 3

[0038] First take 600ml of deionized water, add 1.38g of citric acid to dissolve, then press Li 7 La 3 Zr 2 o 12 The stoichiometric ratio weighs 4.45g of lithium nitrate, 4.68g of lanthanum nitrate, and 1.12g of zirconium oxynitrate into the above-mentioned citric acid solution, wherein the excess of lithium salt is 10%, stirs the mixed solution for 12h, and then sprays and dries it. The spray feed rate was set at 2r / min, the outlet temperature of the nozzle was 180°C, and the blast pressure was 0.2MPa. The obtained spray material is heated up to 800°C at 1°C / min for sintering, and the sintering time is 6h.

[0039] Morphological characterization of the obtained solid electrolyte precursor, such as Figure 5As shown, it can be seen that there is a certain difference in the morphology of the precursor material of Example 2 and the precursor of Example 1.

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Abstract

The invention discloses a ceramic solid electrolyte and a preparation method thereof. The ceramic solid electrolyte comprises at least one of NASICON structure type (LiM<2>(PO<4>)<3>, M=Zr, Ge, Mg, Al), oxide (Li<3x>La<2/3-x>TiO<3>) of perovskite structure and oxide (Li<5>La<3>M<2>O<12>) of garnet structure. The preparation method of the ceramic solid electrolyte comprises the following steps of: a) weighing raw materials according to molar ratio of elements in chemical formula of the ceramic solid electrolyte, dissolving the raw materials in solvent, and obtaining mixed solution; b) preparing ceramic solid electrolyte precursor powder from the mixed solution through a spray drying process; c) sintering the precursor powder obtained by spray drying in the air, and finally obtaining the ceramic solid electrolyte with relatively high ionic conductivity and relatively low electronic conductivity. In the method provided by the invention, the spray drying process is used for preparing the ceramic solid electrolyte, spray drying has the advantages that the drying procedure is fast, the mixed solution is directly dried into powder and particle size distribution of the powder is uniform, and thus, large-scale preparation of the ceramic solid electrolyte is expected to be realized, and the method has practical value.

Description

technical field [0001] The invention belongs to the technical field of battery material preparation, and relates to a ceramic solid electrolyte and a preparation method thereof. Background technique [0002] At present, lithium-ion liquid electrolyte batteries have high operating voltage, energy density, mass density, and long cycle life, so they are considered to be the best choice for power batteries in future new energy vehicles. However, most commercial lithium-ion batteries currently have safety hazards such as combustion, explosion, and leakage due to the use of liquid electrolytes, which severely limits the application of lithium-ion batteries in the field of electric vehicles and energy storage power stations. [0003] The all-solid-state lithium battery that uses an inorganic solid electrolyte instead of a liquid electrolyte can fundamentally solve the safety hazards of lithium-ion batteries, and at the same time improve the service temperature range and storage lif...

Claims

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Application Information

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IPC IPC(8): H01M10/0562H01M10/0525
CPCH01M10/0525H01M10/0562H01M2300/002Y02E60/10
Inventor 高云智李琴曹毅付传凯尹鸽平左朋建
Owner HARBIN INST OF TECH
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