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A manufacturing method of in-situ spray pyrolysis lithium iron phosphate all-solid-state thin-film battery

A technology of lithium iron phosphate and spray pyrolysis, which is applied in the manufacture of electrolyte batteries, non-aqueous electrolyte batteries, and final product manufacturing, to achieve the effects of increasing interlayer matching, improving electronic conductivity, and reducing stress and grain boundaries

Inactive Publication Date: 2014-10-08
NINGBO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The technical problem to be solved by this invention is to propose the method that adopts spray pyrolysis in view of existing background technology by adding slightly excessive non-volatile high-boiling point organic (polymer) matter in the positive electrode precursor solution, make it and positive electrode in spraying process The active materials are evenly mixed, and the air is isolated from the pyrolysis during the subsequent heat treatment process. The carbon obtained by the pyrolysis reduces ferric iron in situ to form a lithium iron phosphate all-solid-state thin-film lithium battery, and the trace carbon after reduction can also serve as an electronic link in the positive electrode material. , to increase its electronic conductivity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1: Place the copper sheet substrate on the surface of a stainless steel heating plate at a constant temperature of 250°C, and connect the spray gun A to the precursor solution I: ferrous acetate Fe(CH 3 COO) 2 (0.1mol / L), CH acetate 3 COOH(0.1mol / L), lithium acetate Li(CH 3 COO) (0.1mol / L), ammonium dihydrogen phosphate NH 4 h 2 PO 4 (0.1mol / L), ethylene glycol methyl ether (0.8wt%) and sucrose (0.2wt%) aqueous solution. Spray gun B is connected to precursor solution II: lanthanum nitrate La(NO 3 )3 (0.2mol / L), n-butyl titanate Ti(OC 4 h 9 ) 4 (0.4mol / L), CH acetate 3 COOH(0.2mol / L), lithium acetate Li(CH 3 COO) (0.18mol / L), and an aqueous solution of n-amyl alcohol (0.5wt%). Spray gun A is 10 cm vertically away from the working surface, and the angle of intersection with the working surface is 65°. The carrier gas atomizes and sprays precursor solution I with a flow rate of 5 mL / min at a pressure of 100 KPa for 30 minutes to the substrate. Then r...

Embodiment 2

[0020] Embodiment 2: Place the silicon wafer substrate on the surface of a stainless steel heating plate at a constant temperature of 300°C, and connect the spray gun A to the precursor solution I: ferrous acetate Fe(CH 3 COO) 2 (0.3mol / L), CH acetate 3 COOH(0.1mol / L), lithium acetate Li(CH 3 COO) (0.3mol / L), ammonium dihydrogen phosphate NH 4 h 2 PO 4 (0.3mol / L), an aqueous solution of ethylene glycol methyl ether (1.0wt%) and sucrose (0.6wt%). Spray gun B is connected to precursor solution II: lanthanum nitrate La(NO 3 ) 3 (0.4mol / L), n-butyl titanate Ti(OC 4 h 9 ) 4 (0.8mol / L), CH acetate 3 COOH(0.2mol / L), lithium acetate Li(CH 3 COO) (0.39mol / L), and an aqueous solution of n-pentanol (0.8wt%). Spray gun A is 12 cm vertically away from the working surface, and the angle of intersection with the working surface is 70°. The carrier gas atomizes and sprays the precursor solution I with a flow rate of 6 mL / min at a pressure of 80 KPa for 40 minutes to the substrate....

Embodiment 3

[0021] Embodiment 3: the nickel sheet substrate is placed on the surface of a stainless steel heating plate with a constant temperature of 450 ° C, and the spray gun A is connected to the precursor solution I: ferrous acetate Fe(CH 3 COO) 2 (0.15mol / L), CH acetate 3 COOH(0.08mol / L), lithium acetate Li(CH 3 COO) (0.15mol / L), ammonium dihydrogen phosphate NH 4 h 2 PO 4 (0.15mol / L), an aqueous solution of polyvinyl alcohol PVA (0.7wt%) and glucose (0.3wt%). Spray gun B is connected to precursor solution II: lanthanum nitrate La(NO 3 ) 3 (0.4mol / L), n-butyl titanate Ti(OC 4 h 9 ) 4 (0.8mol / L), CH acetate 3 COOH(0.5mol / L), lithium acetate Li(CH 3 COO) (0.35mol / L), and an aqueous solution of ethylene glycol methyl ether (1.3wt%). Spray gun A is 15 cm vertically away from the working surface, and the angle of intersection with the working surface is 80°. The carrier gas atomizes and sprays precursor solution I with a flow rate of 10 mL / min at a pressure of 150 KPa for 60 ...

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Abstract

A spray pyrolysis method is used to add a slight excess of non-volatile high-boiling point organic (polymer) matter to the positive electrode precursor solution, so that it can be uniformly mixed with the positive electrode active material during the spraying process, and the air cracking is isolated during the subsequent heat treatment process, The carbon obtained from the cracking reduces ferric iron in situ to form a lithium iron phosphate all-solid-state thin-film lithium battery, and the trace carbon after reduction can also act as an electronic link in the positive electrode material to improve its electronic conductivity. At the same time, double spray guns are used to form two buffer layers at the junction of the positive electrode-solid electrolyte-negative electrode layer and the layer during the spraying process, and the phase composition in adjacent layers changes continuously in the buffer layer. It makes the adjacent layers tightly bonded and greatly increases the matching degree between layers, reduces stress and grain boundaries, improves the conductance of the interface, greatly reduces the influence of the conductance of the interface on the overall performance of the battery, and improves the stability of the battery.

Description

technical field [0001] The invention relates to the field of manufacturing all-solid-state lithium-ion batteries. 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 electrolyte; stable performance, wide operating temperature range ( -50~180℃), c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M10/058
CPCY02E60/10Y02P70/50
Inventor 水淼舒杰任元龙徐丹郑卫东任政娟王青春黄峰涛
Owner NINGBO UNIV