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Method for preparing electrolyte ceramic membrane of lithium ion battery
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A lithium ion battery and electrolyte technology, which is applied to the preparation of lithium ion battery electrolyte ceramic membrane and the field of lithium ion battery electrolyte ceramic membrane preparation by casting method, can solve the problems of complex equipment, high production cost, long production cycle and the like
Inactive Publication Date: 2013-03-13
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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Problems solved by technology
Methods such as physical vapor deposition can precisely control the thickness, and the obtained film is very dense, but the equipment is complicated, the production cost is high, and the production cycle is long, which cannot meet the requirements of large-scale production applications.
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Embodiment 1
[0017] Method is the same as Comparative Example 1, according to Li 1.4 Al 0.4 Ge 0.8 Ti 0.8 (PO 4 ) 3 (LAG-TP) stoichiometric Li 2 CO 3 ,TiO 2 , Al(OH) 3 , GeO 2 with NH 4 h 2 PO 4 Mix evenly by ball milling, then heat treatment at 700°C for 2 hours for decomposition and synthesis, and grind after cooling to obtain powder.
[0018] Add the above-mentioned powder into an ethanol solvent, then add 2wt.% triethanolamine, 6wt.% PVB and 10wt.% plasticizer by weight of the powder, and continue ball milling for 4 hours to obtain a slurry for casting; flow The film obtained after delay has better strength and toughness. The dense electrolyte ceramics were obtained after sintering at 900℃ for 12h.
Embodiment 2
[0020] Method is the same as Comparative Example 1, according to Li 1.4 Al 0.4 Ti 1.6 (PO 4 ) 3 (LAG-TP) stoichiometric Li 2 CO 3 ,TiO 2 , Al(OH) 3 , GeO 2 with NH 4 h 2 PO 4 Mix evenly by ball milling, then heat treatment at 700°C for 2 hours for decomposition and synthesis, and grind after cooling to obtain powder.
[0021] Add the above powder into the azeotropic solution of propanol and trichlorethylene, then add 1wt% triethanolamine, 9wt% PVB and 10.5wt% plasticizer by weight of the powder, and continue ball milling for 4 hours to obtain cast The slurry used; the film obtained after casting has good strength and toughness. The dense electrolyte ceramics were obtained after sintering at 1000℃ for 12h.
Embodiment 3
[0023] Analytical pure Li 2 CO 3 ,, Al(OH) 3 ,, TiO 2 with NH 4 h 2 PO 4 as raw material, according to Li 1.4 Al 0.4 Ge 0.96 Ti 0.64 (PO 4 ) 3 Stoichiometric ratio, fully divided and mixed, heat treated at 700°C for 4 hours to fully decompose easily decomposed products, then cooled and ground for later use. In the glove box of argon atmosphere, a certain quality of precursor material is placed in a stainless steel tank, and a ball milling medium stainless steel ball is added. The selected ball material ratio is 15:1, and the ball milling speed is 500rpm. Ball milling at room temperature obtains an amorphous Powder. Powder TEM such as figure 2 shown.
[0024] Add the above-mentioned amorphous powder to the azeotropic solution of butanone and ethanol, then add 0.5wt.% phosphate ester, 4wt.% PVB and 8wt.% plasticizer by weight of the powder, and continue ball milling for 4 hours. A slurry for casting is obtained; the film obtained after casting has good strength a...
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Abstract
The invention relates to a method for preparing an electrolyte ceramic membrane of a lithium ion battery, in particular to a tape casting method for preparing the electrolyte ceramic membrane of the lithium ion battery, and belongs to the field of ion conductive ceramic materials. The invention adopts the tape casting method; ceramic powder with a chemical formula of Li1.4Al0.4(Gel-xTix)1.6(PO4)3 (wherein x is equal to 0-1.0) is selected as raw material powder; triethanolamine or phosphate are selected as a dispersing agent; ethanol, propyl alcohol, butanone, triclene, or azeotropic solution prepared from any two of the ethanol, propyl alcohol, butanone and triclene is selected as a solvent; polyvinyl butyral (PVB) is selected as an adhesive; polyethylene glycol or dibutyl phthalate is selected as a plasticizer; the range of solid content of slurry is controlled between 18 and 30vol percent; the uniform slurry is prepared through ball milling, and then is prepared into a green belt by the tape casting method, and the green belt is subjected to heat treatment to form the electrolyte ceramic membrane; and the electrolyte ceramic membrane has good strength and toughness, and can be applied to actual production.
Description
technical field [0001] The invention relates to a preparation method of a lithium-ion battery electrolyte ceramic membrane, in particular to the preparation of a lithium-ion battery electrolyte ceramic membrane by a casting method, and belongs to the field of ion-conducting ceramic materials. Background technique [0002] For inorganic solid electrolytes, the NASICON-structured Li-ion conductor has the most suitable tunnel size and skeleton for Li-ion migration. The NASICON-structured lithium-ion solid electrolyte is the most promising material system for all-solid-state lithium batteries. Therefore, the most studied crystalline and glass-ceramic lithium-ion electrolytes are NASICON-structured lithium-ion conductors. [0003] The impedance of the electrolyte is proportional to the thickness of the ceramic, so the impedance of the electrolyte ceramic can be reduced by reducing the thickness of the electrolyte ceramic, which is equivalent to improving the conductivity of the e...
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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/447C04B35/622
Inventor 温兆银许晓雄刘宇王秀艳李宁张群喜黄颖宋树丰
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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