Solid electrolyte for inhibiting lithium dendrites growth in full-solid-state battery, and preparation method thereof

A solid-state electrolyte and all-solid-state battery technology, applied in secondary batteries, electrochemical generators, circuits, etc., can solve the problems of different thermodynamic properties, chemical stability and electrochemical stability between solid-state electrolytes and electrode materials, and improve the interface Effects of ion conductivity, reduction of grain boundary migration resistance, and reduction of porosity

Inactive Publication Date: 2017-06-13
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, computational studies have shown that the thermodynamic properties, chemical stability, and electrochemical stability of solid-state electrolytes and electrode materials are different, and there is still a large gap in the study of their compatibility in solid-state batteries.

Method used

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  • Solid electrolyte for inhibiting lithium dendrites growth in full-solid-state battery, and preparation method thereof
  • Solid electrolyte for inhibiting lithium dendrites growth in full-solid-state battery, and preparation method thereof
  • Solid electrolyte for inhibiting lithium dendrites growth in full-solid-state battery, and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] A method for preparing a solid-state electrolyte for inhibiting the growth of lithium dendrites in an all-solid-state battery, using the following steps:

[0040] Step 1: Weigh lithium carbonate, lanthanum oxide, and zirconium oxide according to the stoichiometric ratio, and grind them evenly by dry grinding method, so that the mixture is fully mixed, and then placed in an alumina crucible with a cover;

[0041] The second step: put the mixture in the first step in an alumina crucible with a cover, sinter in a muffle furnace at 900°C for 3 to 6 hours, the heating and cooling rate is 5°C / min, and cool to room temperature;

[0042] The third step: transfer the reactant in the second step to an agate mortar for grinding, mix well, and record it as mother powder A;

[0043] Step 4: Grind the reactants in the second step in an agate mortar, add 0.1-10 wt% of the second phase with a low melting point, mix well, and record it as mother powder B;

[0044] Step 5: Add 0.3g of t...

Embodiment 2

[0050] The preparation method in this example is the same as in Example 1. In step 4 of this example, a low-temperature second-phase sintering aid is used, the lithium-containing garnet with lithium borate is marked as LLZ+LBO, and the lithium-containing garnet with lithium borate is added. Garnet is marked as LLZ+LPO, and lithium-containing garnet with lithium borate is marked as LLZ+LSO. Depend on figure 2 It can be seen that the XRD of the lithium-containing garnet prepared in Example 2 is completely consistent with the standard cubic phase lithium-containing garnet (c-LLZ), and the doping of the low-temperature second-phase sintering aid lithium-containing garnet does not change its crystal structure, good crystallinity, and no second phase additive detected by XRD.

[0051] Depend on image 3 It can be seen that undoped lithium-containing garnet, lithium-containing garnet with lithium borate (LLZ+LBO), lithium-containing garnet with lithium borate (LLZ+LPO), lithium-co...

Embodiment 3

[0055] The preparation method in this example is the same as in Example 1, the only difference is that the mass ratio of lithium carbonate, lanthanum oxide, and zirconia is 20:50:20, the addition of the second phase in the preparation process is different, and the temperature rise and fall speed of the muffle furnace The control is 1° C. / minute, and the auxiliary agent added in Step 4 of this embodiment is lithium borate.

[0056] The phase of the lithium-containing garnet prepared in Example 3 was characterized by X-ray diffraction and other means. X-ray diffraction shows that the lithium-containing garnet obtained in Example 3 at 900° C. for 16 hours is a cubic phase. The lithium borate second phase effectively reduces the sintering temperature of lithium-containing garnet.

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Abstract

The invention relates to a solid electrolyte for inhibiting lithium dendrites growth in a full-solid-state battery, and a preparation method thereof. The solid electrolyte is prepared from lithium-lanthanum-zirconium oxide ceramic and 0.1 to 10 weight percent of low-melting-point sintering aid. The preparation method comprises the following steps of dry grinding and uniformly mixing stoichiometric lithium carbonate, lanthanum oxide and zirconium oxide, and then presintering in a muffle furnace at the temperature of 900 DEG C to form a phase; adding the low-melting-point sintering aid into presintering powder, and dry grinding and mixing to obtain a manual pressed sheet sample; densifying during a further high-temperature sintering process to form the solid electrolyte with high ionic conductance, stable performance and high repeatability. Compared with the prior art, without influencing a conductive property of a lithium-contained garnet lithium ion, a low-cost second phase is used so that the conductive property of the lithium ion at a crystal boundary part is improved, the solid electrolyte can better realize lithium ion transmission and plays a role in inhibiting the lithium dendrites growth in the full-solid-state battery, and the safety of the lithium battery is improved.

Description

technical field [0001] The invention relates to the field of all-solid-state electrolytes for lithium batteries, in particular to a solid-state electrolyte for inhibiting the growth of lithium dendrites in all-solid-state batteries and a preparation method thereof. Background technique [0002] Lithium batteries, which have the advantages of light weight, high specific energy / specific power, long life, and no memory effect, are more and more widely used in mobile communications, electric vehicles, aerospace and military fields. Lithium metal has a theoretical specific capacity as high as 3860mAh g -1 , light weight and many other advantages, it has become a research hotspot for the next generation of lithium battery anode. [0003] However, with the development of lithium battery technology, the safety requirements for battery materials are getting higher and higher. In the actual application process, metal lithium electrodes will react with flammable and volatile organic l...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/0562C04B35/50C04B35/622C04B35/64
CPCC04B35/50C04B35/622C04B35/64C04B2235/3203C04B2235/3246C04B2235/3409C04B2235/3427C04B2235/447C04B2235/6562C04B2235/6567C04B2235/786H01M10/0562Y02E60/10
Inventor 段华南徐比翼刘河洲郭益平康红梅李华
Owner SHANGHAI JIAO TONG UNIV
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