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Modified NASICON type sodium ion ceramic electrolyte and preparation method and application thereof

A ceramic electrolyte and sodium ion technology, which is applied in the manufacture of electrolyte batteries, composite electrolytes, non-aqueous electrolyte batteries, etc., can solve problems such as insufficient contact, deterioration, and poor interface compatibility, and achieve reduced interface resistance, stable connection interface, and high conductivity. rate-boosting effect

Active Publication Date: 2021-07-13
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the Na of the NASICON structure 1+x Zr 2 Si x P 3-x o 12 (0<x<3) has stable chemical properties, wide electrochemical window and relatively high sodium ion conductivity (at room temperature can reach 10 - 4 S / cm), but still far below the ionic conductivity of traditional electrolytes
Moreover, in an all-solid-state battery, the complex interface between the solid electrode and the solid electrolyte, such as insufficient contact, or mechanical failure caused by phase change or volume change during the working process, and degradation of the ion-conducting interface layer, will cause electrolyte / electrode High interfacial impedance between
[0006] From the above, it can be seen that the existing solid electrolytes still have problems such as low sodium ion conductivity, poor interfacial compatibility between the solid electrolyte and electrodes, and high sintering temperature during preparation.

Method used

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  • Modified NASICON type sodium ion ceramic electrolyte and preparation method and application thereof
  • Modified NASICON type sodium ion ceramic electrolyte and preparation method and application thereof
  • Modified NASICON type sodium ion ceramic electrolyte and preparation method and application thereof

Examples

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preparation example Construction

[0050] In the second aspect, the embodiment of the present invention provides a method for preparing the modified NASICON type sodium ion ceramic electrolyte described in the first aspect, such as figure 1 Shown, this preparation method comprises:

[0051] In step 1 (S1), boron oxides, sodium source compounds, zirconium source compounds, silicon source compounds and phosphorus source compounds are mixed by ball milling, dried and pre-sintered to obtain ceramic powder.

[0052] During specific implementation, the low melting point boron oxide, sodium source compound, zirconium source compound, silicon source compound and phosphorus source compound are ball milled and mixed, dried and pre-sintered to obtain reactant powder, namely ceramic powder.

[0053] In this implementation step, the low melting point boron oxide is H 3 BO 3 , B 2 o 3 、Na 2 B 4 o 7 , Zn 3 B 2 o 6 or SiO 2 -B 2 o 3 One or a combination of several of them; the sodium source is sodium oxalate, sodi...

Embodiment 1

[0067] Embodiment 1 (preparation Na 3 Zr 2 Si 2 PO 12 )

[0068] (1) Na 2 CO 3 , ZrN 2 o 7 , SiO 2 with NH 4 h 2 PO 4 Weigh according to the stoichiometric ratio, add ethanol and ball mill for 12 hours at a speed of 300r / min, after the ball mill is uniform, discharge and dry;

[0069] (2) Place the mixture described in step (1) in a muffle furnace, raise the temperature to 1000°C, keep it warm for 6h, the heating rate is 3°C / min, and cool to room temperature;

[0070] (3) The reactant obtained in step (2) is subjected to secondary ball milling, discharging, and after drying, it is placed in an agate mortar and added with a concentration of 0.5% PVA methanol solution, fully ground and dried;

[0071] (4) Compressing the powder obtained in step (3) into tablets under a pressure of 10MPa, wherein the holding time is 1s;

[0072] (5) Debinding the molded sheet in step (4), then transfer it to a muffle furnace, raise the temperature to 1200°C for sintering for 10 hours...

Embodiment 2

[0075] (1) This implementation step is similar to the preparation steps of Example 1, the difference is that: the raw material powder used in Example 1 and the Na 2 B 4 o 7 Mixing, ball milling and drying to obtain the mixture;

[0076] (2) Place the mixture in step (1) in a muffle furnace, heat up to 600°C, sinter for 6 hours, and cool to room temperature at a heating rate of 3°C / min;

[0077] (3) The reactant obtained in step (2) is subjected to secondary ball milling, discharging, and after drying, it is placed in an agate mortar and added with a concentration of 0.5% PVA methanol solution, fully ground and dried;

[0078] (4) Compressing the powder obtained in step (3) into tablets under a pressure of 10MPa, wherein the holding time is 1s;

[0079] (5) Debinding the molded sheet in step (4), then transfer it to a muffle furnace, heat up to 1000°C for sintering for 10 hours, and heat up at a rate of 3°C / min, then cool to room temperature to obtain a dense ceramic electro...

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Abstract

The invention provides a modified NASICON type sodium ion ceramic electrolyte and a preparation method and application thereof. The modified NASICON type sodium ion ceramic electrolyte is obtained by connecting a low-melting-point boron oxide to a crystal boundary of Na<3>Zr<2>Si<2>PO<12> ceramic. The low-melting-point boron oxide is connected to the grain boundary of the Na<3>Zr<2>Si<2>PO<12> ceramic for wetting, so that the density sintering temperature of the sodium ion ceramic electrolyte is reduced; and meanwhile, the generated modified NASICON type sodium ion ceramic electrolyte has no impure phase, the sodium ion conductivity is obviously improved, and the modified NASICON type sodium ion ceramic electrolyte has relatively low interface resistance and excellent stability for metal sodium.

Description

technical field [0001] The invention relates to the technical field of sodium ion batteries, and mainly relates to a modified NASICON type sodium ion ceramic electrolyte and its preparation method and application. Background technique [0002] The depletion of fossil energy has prompted the continuous development of renewable clean energy such as solar energy, wind energy, and geothermal energy. Therefore, it is urgent to develop a matching energy storage system. Due to the advantages of high efficiency and convenient maintenance, electrochemical energy storage has the greatest potential for application and promotion. Since the commercial application of lithium-ion batteries in 1991, it has not only occupied a dominant position in the field of small consumer electronics such as notebook computers, mobile phones, and digital cameras, but also has shown impressive development prospects in the fields of power batteries and energy storage systems in recent years. . [0003] Du...

Claims

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Application Information

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IPC IPC(8): H01M10/0562H01M10/058H01M10/054
CPCH01M10/0562H01M10/058H01M10/054H01M2300/0088Y02P70/50Y02E60/10
Inventor 赵永杰孙政王成志金海波
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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