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Novel lithium ion conduction oxide solid electrolyte and method for preparing same

A solid electrolyte, lithium ion technology, applied in the field of new lithium ion conductive oxide solid electrolyte and its preparation, can solve the problems of increased interface resistance and poor electrochemical stability of solid-state batteries, achieve excellent chemical stability, and promote uniform mixing. , the effect of easy sintering

Active Publication Date: 2018-11-13
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] There are still many defects in the oxide solid electrolytes discovered so far. There are metals in the valence state in the perovskite and NASICON structure solid electrolytes, and the electrochemical stability is poor; the garnet structure solid electrolytes will form Li on the surface in humid air. 2 CO 3 , so that the interface resistance of the solid-state battery assembled by it increases sharply

Method used

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  • Novel lithium ion conduction oxide solid electrolyte and method for preparing same
  • Novel lithium ion conduction oxide solid electrolyte and method for preparing same
  • Novel lithium ion conduction oxide solid electrolyte and method for preparing same

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preparation example Construction

[0030] like Figure 4 Shown, the present invention provides a kind of preparation method of novel oxide solid electrolyte, and it comprises the steps:

[0031] S1 wet ball milling mixed raw materials:

[0032] Weigh and analyze the pure chemical raw material lithium source (Li) according to the designed stoichiometric ratio 2 CO 3 , LiOH), Ta 2 o 5 , ZrO 2 , SiO 2 , and placed in a 100ml zirconia ball mill jar (the material of the ball mill is ZrO 2), add 30ml of ball milling liquid (ethanol, isopropanol or water), and use a planetary ball mill to mill for 24h under the condition of 50 rpm to realize the mixing of raw material powder, wherein the solid electrolyte is Li 1+x Ta 1-x Zr x SiO 5 , the content of doping components is 05 Formation;

[0033] S2 Calcination to prepare powder:

[0034] After the mixed slurry is dried, it is calcined at 850°C to 950°C for 12 to 24 hours to realize the decomposition of the lithium source in the raw material and the preliminar...

Embodiment 1

[0040] Li 1.1 Ta 0.9 Zr 0.1 SiO 5 Preparation of solid electrolyte, wherein lithium content is excessive 1%, tantalum is missing 1%, and silicon content is excessive 5%, the specific steps are as follows:

[0041] Weigh the raw material powder according to the designed stoichiometric ratio, that is, according to the chemical formula Li 1.1 Ta 0.9 Zr 0.1 SiO 5 Calculate the amount of each raw material, then adjust the amount of the raw material to make it lower or higher than the calculated value according to the excess or missing requirements, and finally weigh each raw material according to the adjusted value, for example, according to the chemical formula Li 1.1 Ta 0.9 Zr 0.1 SiO 5 Calculate Li 2 CO 3 、 Ta 2 o 5 , ZrO 2 and SiO 2 Respective amount, Li is adjusted according to 0% excess lithium content, 0% tantalum deficiency, and 5% excess silicon content 2 CO 3 、 Ta 2 o 5 and SiO 2 The amount of lithium content in excess of 0%, then Li 2 CO 3 The amoun...

Embodiment 2

[0046] Li 1.05 Ta 0.95 Zr 0.05 SiO 5 The preparation of the solid electrolyte, wherein the excess lithium content is 0%, the tantalum is missing 2%, and the silicon content is excessive 3%, the specific steps are as follows:

[0047] Weigh the raw material powder according to the designed stoichiometric ratio, that is, according to the chemical formula Li 1.05 Ta 0.95 Zr 0.05 SiO 5 Calculate the amount of each raw material, and then adjust the amount of raw materials according to the excess or lack of requirements to make it lower or higher than the calculated value, and finally weigh each raw material according to the adjusted value, that is, weigh Li according to the respective amount 2 CO 3 、 Ta 2 o 5 , ZrO 2 and SiO 2 , and then placed in a 100ml zirconia ball mill jar, added 30ml of ethanol, and ball milled for 24h under the condition of 50 rpm to obtain a mixed slurry of raw materials;

[0048] The slurry mixed with raw materials was dried at 100°C, transferr...

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Abstract

The invention belongs to the field of lithium ion solid electrolyte, and particularly discloses novel lithium ion conduction oxide solid electrolyte and a method for preparing the same. The method particularly includes weighing raw materials according to designed stoichiometric ratios and mixing the raw materials with one another by means of ball-milling by the aid of wet processes; carrying out step-by-step calcination on the mixed raw materials to prepare solid electrolyte powder; maintaining pressures for the solid electrolyte powder under appropriate pressure conditions for 30-60 min, thenburying blanks in powder with identical components, heating the blanks at the speeds of 1-2 DEG C / min until the temperatures of the blanks reach 1100-1200 DEG C and preserving heat for 12-24 h to obtain the required novel lithium ion conduction oxide solid electrolyte. The novel lithium ion conduction oxide solid electrolyte and the method have the advantages that technological processes are simple, and the novel lithium ion conduction oxide solid electrolyte and the method are low in cost; the novel lithium ion conduction oxide solid electrolyte prepared by the aid of the method is high in lithium ion conductivity and excellent in chemical stability and can be used as solid electrolyte for lithium ion batteries.

Description

technical field [0001] The invention belongs to the field of lithium ion solid electrolytes, and more specifically relates to a novel lithium ion conductive oxide solid electrolyte and a preparation method thereof. Background technique [0002] Lithium-ion batteries are currently the most widely used electrochemical energy storage devices, and have a wide range of applications in microelectronic devices, mobile electronic devices, electric vehicles, and smart grids. Traditional lithium-ion batteries use liquid electrolytes, which are easy to leak and burn, so there are obvious safety hazards in traditional lithium-ion batteries. Solid-state lithium-ion batteries use solid electrolytes, which can significantly improve the safety of lithium-ion batteries, and also have advantages in terms of energy density, power density, and service life. [0003] Solid electrolytes are the key factors determining the performance of solid-state lithium-ion batteries, mainly including sulfide...

Claims

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Application Information

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IPC IPC(8): C04B35/16C04B35/64H01M10/0562
CPCC04B35/16C04B35/64C04B2235/3203C04B2235/3251C04B2235/6562H01M10/0562Y02E60/10
Inventor 吴剑芳郭新汪其
Owner HUAZHONG UNIV OF SCI & TECH
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