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Mist pyrolysis preparation method of all-solid-state film lithium battery

A spray pyrolysis and lithium battery technology, applied in the manufacture of electrolyte batteries, non-aqueous electrolyte batteries, and final product manufacturing, etc., can solve the problem of difficulty in overcoming the difficulty of conducting the interface between the electrode sheet and the electrolyte sheet, the degree of particle matching is not high, affecting the battery. Overall performance and other issues, to achieve the effect of reducing stress, reducing grain boundaries, and increasing matching

Inactive Publication Date: 2012-12-19
NINGBO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In spray pyrolysis, the substrate temperature is usually not high and the kinetic energy brought by the carrier gas to the particles is limited (much less than magnetron sputtering or pulsed laser), resulting in a low degree of tightness and matching of the interface between layers, so the grain boundary resistance of the interface Higher, will seriously affect the overall performance of the battery
[0008]2. There are few solid electrolyte materials suitable for spray pyrolysis preparation. At present, the solid electrolyte LiPON (nitrogen-doped lithium phosphate) with good performance can only be produced by magnetron sputtering preparation
[0009]3. There are many process parameters that can be adjusted, such as carrier gas flow rate, material flow rate, substrate temperature, distance between nozzle and substrate, etc., optimization of process conditions more difficult
[0010] At present, research and development personnel have made some explorations on the preparation of all-solid-state thin-film batteries by spray pyrolysis, such as the Chinese invention patent with application number 200910044488.7, such as the literature [P. FRAGNAND, R NAGARAJAN., D. VUJIC, J. Power Sources, 1995, 54: 362.], basically the positive or negative electrode or electrolyte sheet of the whole film battery prepared by the traditional spray pyrolysis method, and it is difficult to overcome the electrode The interface conduction between the sheet and the electrolyte sheet is difficult, which affects the overall performance of the battery

Method used

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  • Mist pyrolysis preparation method of all-solid-state film lithium battery

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1: Place a copper substrate on the surface of a heated work board at a constant temperature of 250°C, and spray gun A for spraying precursor solution I: ammonium metavanadate NH with a concentration of 0.3 mol / L 4 VO 3 , Ammonia NH with a concentration of 0.08 mol / L 3 ·H 2 O, the concentration of 0.1mol / L lithium acetate Li(CH 3 COO), and an aqueous solution of ethylene glycol methyl ether with a concentration of 0.2% by weight. Spray gun B is used to spray precursor solution II: lanthanum nitrate with a concentration of 0.2mol / L La(NO 3 ) 3 , The concentration of 0.4mol / L n-butyl titanate Ti(OC 4 H 9 ) 4 , Acetic acid CH with a concentration of 0.2mol / L 3 COOH, the concentration of 0.18mol / L lithium acetate Li(CH 3 COO) and an aqueous solution of n-pentanol with a concentration of 0.1wt% by mass. The vertical distance between spray gun A and the surface of the heating work plate is 10cm, and the intersection angle between spray gun A and the surface of the heatin...

Embodiment 2

[0027] Example 2: Place the silicon wafer substrate on the surface of the heating work plate at a constant temperature of 350°C, and spray gun A is used to spray precursor solution I: ammonium metavanadate NH with a concentration of 1.0 mol / L 4 VO 3 , Ammonia NH with a concentration of 0.15mol / L 3 ·H 2 O, the concentration of 0.3mol / L lithium acetate Li(CH 3 COO), and an aqueous solution of ethylene glycol methyl ether with a concentration of 2wt% by mass percentage. Spray gun B sprays precursor solution II: lanthanum nitrate with a concentration of 0.5mol / L La(NO 3 ) 3 , The concentration is 1.0mol / L n-butyl titanate Ti(OC 4 H 9 ) 4 , Acetic acid CH with a concentration of 0.5mol / L 3 COOH, the concentration of 0.52mol / L lithium acetate Li(CH 3 COO) and 2.2wt% polyvinyl alcohol PVA (average molecular weight o , The carrier gas with a pressure of 150Kpa is applied to spray gun A, spray gun A atomizes and sprays the precursor solution I onto the substrate, and the spray is continue...

Embodiment 3

[0031] Example 3: Place a nickel substrate on the surface of a heated work plate at a constant temperature of 500°C, and spray gun A is used for spray flooding solution I: ammonium metavanadate NH with a concentration of 2.0 mol / L 4 VO 3 , The concentration of 0.28mol / L ammonia water NH 3 ·H 2 O, lithium acetate Li(CH 3 COO), and an aqueous solution of n-pentanol with a mass percentage concentration of 4.5 wt%. Spray gun B sprays precursor solution II: lanthanum nitrate with a concentration of 1.0mol / L La(NO 3 ) 3 , The concentration of 2.0mol / L n-butyl titanate Ti(OC 4 H 9 ) 4 , Acetic acid CH with a concentration of 0.9mol / L 3 COOH, the concentration of 0.95mol / L lithium acetate Li(CH 3 COO), and an aqueous solution of ethylene glycol methyl ether with a concentration of 4.7% by weight. The vertical distance between spray gun A and the surface of the heating work plate is 19cm, and the intersection angle between spray gun A and the surface of the heating work plate is 80 o , ...

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Abstract

The invention discloses a mist pyrolysis preparation method of an all-solid-state film lithium battery. According to the invention, double spray guns are adopted to spray precursor solution of two layers at boundaries of electrode film layers simultaneously. A flow rate of the precursor solution at a lower layer is gradually reduced, and the flow rate of the precursor solution at an upper layer is gradually increased, and a buffering layer is formed between two settled layers. The contents of the components of the two layers in the buffering layer are morphing. The content of the components of the lower layer is gradually reduced, and the content of the components of the upper layer is gradually increased. The method is advantaged in that: with the method, the upper layer and the lower layer are compactly combined, the coupling between the two layers is increased, stress force and grain boundary are reduced, conductivities of the interfaces are increased, the influence of interface conductivities on the integral performance of the battery is reduced as far as possible, and the performance of the battery is improved.

Description

technical field [0001] The invention relates to a preparation method of a lithium battery, in particular to a spray pyrolysis preparation method of an all-solid thin film lithium battery. Background technique [0002] The all-solid-state lithium-ion battery composed of inorganic solid electrolyte has the following advantages: it has higher specific energy than traditional nickel-cadmium and nickel-hydrogen batteries; the shape design of the battery is also more convenient and flexible, and can be prepared into almost any shape and size , can be directly integrated in the circuit; it has excellent charge-discharge cycle performance, low self-discharge rate, and can overcome the problem of gradual failure of the liquid electrolyte lithium-ion battery due to the dissolution of the electrode active material in the electrolyte after a period of use [Z. R. Zhang, Z. L. Gong, and Y. Yang, J. Phys. Chem. B, 108, 2004, 17546.]; high safety, no gas generated during work, no leakage of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M10/058
CPCY02E60/12Y02E60/10Y02P70/50
Inventor 郑卫东水淼舒杰任元龙王青春黄峰涛徐丹
Owner NINGBO UNIV
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