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Double-coated composite solid lithium manganate material and preparation method thereof

A technology of lithium manganate and double coating is applied in the field of preparation of double-coated composite solid lithium manganate materials, and can solve the problems of difficulty in building a conductive network, poor conductivity of graphene oxide, and inability to achieve effective coating, etc. To achieve the effect of suppressing the Jahn-Teller effect, strong peeling ability, and easy to purchase

Inactive Publication Date: 2020-03-13
SUZHOU PHYLION BATTERY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The Chinese invention patent with the publication number CN107331853A discloses a graphene composite multilayer porous spherical lithium manganate electrode material and a lithium ion battery prepared therefrom. First, the multilayer porous spherical lithium manganate is prepared by a precipitation method, and Stir and mix with graphene in a wet method, and obtain a graphene-composite lithium manganate material after drying. The problem with this method is that graphene agglomerates seriously, and simple stirring is difficult to disperse evenly, and the effect is poor.
In order to effectively disperse, graphene oxide can be used instead of graphene. The Chinese invention patent with the publication number CN108878856A discloses a preparation method of a graphene-lithium manganate battery positive electrode material. First, lithium manganate powder is prepared by precipitation method, and combined with Graphene oxide solution is mixed, dried and ball milled to obtain graphene-lithium manganate battery positive electrode material. The problem with this method is that graphene oxide has poor conductivity and it is difficult to achieve the expected role of building a conductive network.
Further, the Chinese invention patent with the publication number CN 105206799A discloses a method for preparing a porous metal-doped lithium manganate / graphene lithium battery positive electrode material, using a sol-gel method to prepare porous doped lithium manganate and graphene oxide The solution is mixed, dried and then calcined to obtain the positive electrode material of porous metal-doped lithium manganate / graphene lithium battery. The problem of this method is that the simple method of magnetic stirring and ultrasonic dispersion cannot achieve the effect of effective coating. At the same time, a large number of Solvent energy consumption is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Weigh 2.91g of lithium carbonate, 8.22g of titanium dioxide, 0.93g of alumina, 20.89g of ammonium dihydrogen phosphate and 32.95g of ethanol, put them into a 100ml ball mill jar, the ball-to-material ratio is 2: 1, ball mill for 4 hours, mix well, and dry Then place it in a muffle furnace at 750°C for 12 hours to generate Li 1.3 Al 0.3 Ti 1.7 (PO 4 ) 3 . Add 200g of single crystal lithium manganate, 2.4g of LATP, and 80g of graphene oxide aqueous solution into a sand mill with a ball-to-material ratio of 10:1, grind for 20 minutes, dry and place in a tube furnace, and feed in hydrogen with a content of 5% The argon gas mixture was kept at 900°C for 12 hours to prepare a solid electrolyte and graphene double-coated lithium manganate cathode material.

[0028]The obtained lithium manganate cathode material was mixed with sp, CNTs and PVDF at a mass ratio of 95: 1: 2: 2, NMP was added to stir the mixture into a cathode slurry, and evenly coated on aluminum foil, dried...

Embodiment 2

[0030] Weigh 3.78g of lithium carbonate, 15.51g of titanic acid, 5.06g of aluminum nitrate, 15.59g of diammonium hydrogen phosphate and 39.94g of ethanol, put them into a 100ml ball mill jar, the ball-to-material ratio is 2: 1, and ball mill for 12 hours to mix well, bake After drying, place it in a muffle furnace at 650°C for 12 hours to generate LATP. Add 200g single crystal lithium manganese oxide, 6.0g LATP, and 80g graphene oxide aqueous solution into a sand mill with a ball-to-material ratio of 10:1, grind for 40 minutes, dry and place in a tube furnace, and feed 1% hydrogen The argon gas mixture was kept at 700°C for 4 hours to prepare a solid electrolyte and graphene double-coated lithium manganate cathode material.

[0031] The obtained lithium manganate cathode material was mixed with sp, CNTs and PVDF at a mass ratio of 95: 1: 2: 2, NMP was added to stir the mixture into a cathode slurry, and evenly coated on aluminum foil, dried at 80°C for 6 hours, 120 ℃ vacuum d...

Embodiment 3

[0033] Take by weighing 1.89g lithium hydroxide, 8.22g titanium dioxide, 2.43g aluminum nitrate, 20.89g ammonium dihydrogen phosphate and 33.43g ethanol, put into 100ml ball mill jar, ball material ratio is 2: 1, ball mill 4 hours fully mix, bake After drying, place it in a muffle furnace at 800°C for 4 hours to generate LATP. Add 200g single crystal lithium manganese oxide, 3.0g LATP, and 80g graphene oxide aqueous solution into a sand mill with a ball-to-material ratio of 10:1, grind for 8 minutes, dry and place it in a tube furnace, and feed it with 5% hydrogen The argon gas mixture was kept at 900°C for 12 hours to prepare a solid electrolyte and graphene double-coated lithium manganate cathode material.

[0034] The obtained lithium manganate cathode material was mixed with sp, CNTs and PVDF at a mass ratio of 95: 1: 2: 2, NMP was added to stir the mixture into a cathode slurry, and evenly coated on aluminum foil, dried at 80°C for 6 hours, 120 ℃ vacuum drying for 12 hou...

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Abstract

The invention discloses a double-coated composite solid-state lithium manganate material and a preparation method thereof. The preparation method comprises the following steps of mixing and sinteringa lithium salt, a titanium salt, an aluminum salt and a phosphate raw material to obtain a solid-state electrolyte lithium titanium aluminum phosphate (Li <1+x> Al <x> Ti <2-x> (PO4) 3 (LATP); addingLATP, single crystal lithium manganate, a graphene oxide aqueous solution and zirconium oxide balls into a sand mill to be fully ground, nanocrystallizing the LATP and attaching the LATP to the surface of the lithium manganate, and meanwhile, coating the lithium manganate with graphene oxide; and after drying, reducing the graphene oxide into graphene at a high temperature in a hydrogen atmosphereto obtain the solid electrolyte and the graphene double-coated lithium manganate positive electrode material. According to the method, the consistency and repeatability of the material are ensured, the manufacturing cost is low, the solid electrolyte can inhibit the dissolution of manganese, the graphene blocks the reaction between the electrolyte and the positive electrode material, and the cycle performance and the high-temperature performance are improved.

Description

technical field [0001] The invention relates to the field of lithium ion batteries, in particular to a preparation method of a double-coated composite solid lithium manganate material and a lithium ion battery. Background technique [0002] The specific capacity of positive electrode materials is the most important factor affecting the energy density and cycle life of lithium-ion batteries. Among the four common systems of lithium cobaltate, ternary materials, lithium iron phosphate and lithium manganate, lithium manganate has abundant resources and low cost. It is an ideal cathode material for power batteries due to its advantages of low cost, no heavy metals, high voltage, good safety, and good rate performance. However, its poor cycle performance and high temperature stability greatly limit its industrialization. The main reason is that lithium manganese oxide generates more Mn at the end of discharge. 3+ , prone to the Jahn-Teller effect, the disproportionation of triva...

Claims

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Application Information

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IPC IPC(8): H01M4/505H01M4/62H01M10/0525
CPCH01M4/505H01M4/625H01M4/628H01M10/0525H01M2004/021H01M2004/028Y02E60/10
Inventor 赵成龙王正伟朱华君王永琛张秀奎吴叶超
Owner SUZHOU PHYLION BATTERY
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