Garnet structure solid electrolyte material and preparation method thereof

A solid electrolyte and garnet technology, applied in the manufacture of electrolyte batteries, electrolytes, non-aqueous electrolyte batteries, etc., can solve the problems of reducing ceramic density and ionic conductivity, affecting the electrochemical performance of solid electrolytes, and reducing lithium ion content too much , to achieve good chemical stability, chemical stability, simple preparation method

Inactive Publication Date: 2018-04-06
TONGJI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, lithium ions are the medium for charge transfer in the electrolyte. When tantalum is added, since the valence of tantalum (+5) is higher than that of zirconium (+4), in order to achieve charge balance, the concentration of lithium ions in the electrolyte material will be too low. content, which negatively affects ionic conductivity
[0006] Moreover, the current preparation of garnet-structured lithium-ion conductor Li 7 La 3 Zr 2 o 12 The main method is the high-temperature solid-phase method, which usually involves multiple steps of ball milling, high-temperature calcination and sintering, with many steps and large energy consumption.
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Method used

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  • Garnet structure solid electrolyte material and preparation method thereof
  • Garnet structure solid electrolyte material and preparation method thereof
  • Garnet structure solid electrolyte material and preparation method thereof

Examples

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Effect test

Embodiment 1

[0032] The preparation chemical composition is Li 6.05 Ca 0.05 La 2.95 Ta 1.0 Zr 1.0 o 12 Lithium carbonate as a lithium source, lanthanum oxide as a lanthanum source, zirconium acetate as a zirconium source, calcium carbonate as a calcium source, tantalum pentoxide as a source, and acetic acid as a mixed medium. According to the chemical composition Li 6.05 Ca 0.05 La 2.95 Ta 1.0 Zr 1.0 o 12 Proportionally weigh lithium carbonate, lanthanum oxide, zirconium acetate, calcium carbonate, and tantalum pentoxide and add them to acetic acid. The excess of lithium carbonate is 30% to compensate for the volatilization loss of lithium during the preparation process. Stir magnetically at 50°C until The solvent is all volatilized to obtain the precursor mixed powder. The precursor powder was heated to 400°C at a heating rate of 10°C / min and then kept for 2 hours, then heated to 750°C at a heating rate of 10°C / min and then calcined for 8 hours, then cooled to room temperature ...

Embodiment 2

[0034] The preparation chemical composition is Li 6.45 Ca 0.05 La 2.95 Ta 0.6 Zr 1.4 o 12 Lithium carbonate as a lithium source, lanthanum oxide as a lanthanum source, zirconium acetate as a zirconium source, calcium carbonate as a calcium source, tantalum pentoxide as a source, and acetic acid as a mixed medium. According to the chemical composition Li 6.45 Ca 0.05 La 2.95 Ta 0.6 Zr 1.4 o 12 Proportionally weigh lithium carbonate, lanthanum oxide, zirconium acetate, calcium carbonate, and tantalum pentoxide and add them to acetic acid. The excess of lithium carbonate is 30% to compensate for the volatilization loss of lithium during the preparation process. Stir magnetically at 50°C until The solvent is all volatilized to obtain the precursor mixed powder. The precursor powder was heated to 400°C at a heating rate of 10°C / min and then kept for 2 hours, then heated to 750°C at a heating rate of 10°C / min and then calcined for 8 hours, then cooled to room temperature ...

Embodiment 3

[0047] The preparation chemical composition is Li 6.05 Ca 0.05 La 2.95 Ta 0.05 Zr 1.95 o 12 The solid electrolyte material, and using the same raw material as in Example 1, was magnetically stirred at 100° C. until the solvent was completely volatilized, and the precursor mixed powder was obtained. The precursor powder was heated to 300°C at a heating rate of 1°C / min and then kept for 8 hours, then heated to 600°C at a heating rate of 1°C / min and then calcined for 24 hours, then cooled to room temperature at a cooling rate of 1°C / min. get Li 6.05 Ca 0.05 La 2.95 Ta 0.05 Zr 1.95 o 12 Electrolyte powder, the Li 6.05 Ca 0.05 La 2.95 Ta 0.05 Zr 1.95 o 12 The powder was kept under 10MPa pressure for 2h, pressed into a disc with a diameter of 14mm and a thickness of 1mm, and the disc was placed in Li 6.05 Ca 0.05 La 2.95 Ta 0.05 Zr 1.95 o 12 Covered with electrolyte powder, the temperature was raised to 1000°C at a heating rate of 1°C / min and sintered for 24 ho...

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Abstract

The invention relates to a garnet structure solid electrolyte material and a preparation method thereof. The preparation method comprises the following specific steps: mixing a compound containing five elements such as lithium, lanthanum, calcium, zirconium and tantalum in an acid solution, and drying to obtain precursor powder; and sequentially calcining, tabletting and sintering the precursor powder, thereby obtaining the garnet structure solid electrolyte material. The solid electrolyte material has a chemical composition of Li(7+x-y)CaxLa3-xTayZr2-yO12, wherein x is more than 0 and less than or equal to 1, and y is more than 0 and less than or equal to 2. The method has the advantages of simplicity and convenience in operation, low cost, low energy consumption and the like. The methodfurther contributes to obtaining materials with an accurate stoichiometric ratio and uniform particle size and reducing the content of impurities. X-ray diffraction determines that a crystal structureof the obtained solid electrolyte material is a cubic garnet structure, and an AC impedance method determines that the ionic conductivity of lithium ions in the material can reach 4.03*10<-4>S cm<-1>. The garnet structure solid electrolyte material prepared by the method disclosed by the invention is high in ionic conductivity, excellent in chemical stability and applicable to lithium secondary batteries.

Description

technical field [0001] The invention relates to the technical field of battery materials, in particular to a garnet-structured solid electrolyte material and a preparation method thereof. Background technique [0002] With the low-carbon economy in the ascendant, lithium secondary batteries are actively developing in the direction of vehicle power and grid energy storage. [0003] The power lithium secondary battery with traditional structure has the characteristics of high working voltage, high energy density, and good cycle performance. It has been widely used in portable digital products such as mobile phones, cameras, and notebook computers. At the same time, it has gradually been used in the field of electric vehicles. Large-scale application, but because it uses flammable and explosive organic electrolyte as electrolyte, it is prone to electrolyte leakage and battery explosion, resulting in frequent safety accidents such as fires. [0004] At present, an effective way...

Claims

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Application Information

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IPC IPC(8): H01M10/0562H01M10/058
CPCH01M10/0562H01M10/058H01M2300/0071Y02E60/10Y02P70/50
Inventor 薛明喆陈骁澜张存满李冰曹天翔
Owner TONGJI UNIV
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