Preparation of oxidized inserting layer of laminated lithium manganate as lithium ion battery anode

A positive electrode material layer, lithium-ion battery technology, applied in the direction of electrode manufacturing, lithium batteries, battery electrodes, etc., can solve the problems of reaction vessel volume limitation, high price, harsh reaction conditions, etc., achieve uniform particle size controllable, low production cost The effect of low cost and easy availability of raw materials

Inactive Publication Date: 2004-12-08
BEIJING UNIV OF CHEM TECH
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  • Abstract
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Problems solved by technology

The product prepared by the hydrothermal synthesis reaction method has excellent electrochemical properties, but this method requires expensive special equipment—high pressure reactor, and it is not easy to realize large-scale industrial production due to the limitation of the volume of the reaction vessel.
[0007] Ion exchange reaction method: in literature (4) Nature, 1996,381:499, people such as Robert Armstrong A will Na 2 CO 3 and Mn 2 o 3 Mix according to stoichiometric ratio, and react in solid state at 700-730°C for 18-72 hours under argon atmosphere to obtain α-NaMnO 2 , and then a certain amount of α-NaMnO 2 Add it to n-hexanol containing excess LiCl or LiBr, heat it under reflux at 145-150°C for 6-8 hours, cool to room temperature, filter, rinse with n-hexanol and ethanol, and dry to obtain monoclinic LiMnO 2 , in the voltage range of 3.4 ~ 4.3V (vs. Li), the current density of 10μA cm -2 Under the test conditions, the initial charging capacity is 270mAh·g -1 , when the current density is 0.5mA

Method used

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  • Preparation of oxidized inserting layer of laminated lithium manganate as lithium ion battery anode
  • Preparation of oxidized inserting layer of laminated lithium manganate as lithium ion battery anode

Examples

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Embodiment 1

[0029] Weigh MnSO 4 ·H 2 O 16.90g (0.10mol), NaOH 8.00g (0.20mol), in N 2 Dissolve them in 90 mL of boiled deionized water under protection; drop the NaOH solution into the MnSO 4 In solution, the obtained Mn(OH) 2 The precipitate was aged in a water bath at 60°C for 10 hours; weigh LiOH·H 2 O solid powder 20.98g (0.5mol), added to the above Mn (OH) 2 in the suspension and stir to dissolve; weigh the oxidizing agent (NH 4 ) 2 S 2 o 8 17.10g (0.075mol), dissolved in 70mL of boiled deionized water, added dropwise to the reaction system at a uniform rate within 2h, and continued to react in a water bath at 80°C for 10h; filter the product with a glass sand funnel, and then Wash and filter with 180mL deionized water for 3 times, and then vacuum dry at 120°C for 8 hours to obtain the product of the present invention. ICP and XRD analysis showed that the product composition was Li 0.83 MnO 2 , is an orthorhombic layered lithium manganate structure ( figure 1 ), the elec...

Embodiment 2

[0031] Weigh MnSO 4 ·H 2 O 16.90g (0.10mol), KOH 12.34g (0.22mol), in N 2 Dissolve in 90mL boiled deionized water under protection; drop KOH solution into MnSO4 under rapid stirring 4 In solution, the obtained Mn(OH) 2 The precipitate was aged in a water bath at 80°C for 10 hours; weigh LiOH·H 2 O solid powder 41.96g (1.0mol), added to the above Mn(OH) 2 in the suspension and stir to dissolve; weigh K 2 S 2 o 8 Dissolve 16.20g (0.06mol) of oxidizing agent in 70mL of boiled deionized water, drop it into the reaction system at a uniform rate within 2h, and continue the reaction in a water bath at 80°C for 10h; filter the product with a glass sand funnel and then Wash and filter with 180mL deionized water for 3 times, and then vacuum dry at 120°C for 12h to obtain the product of the present invention. ICP and XRD analysis showed that the product composition was Li 0.91 MnO 2 , which belongs to the orthorhombic layered lithium manganese oxide structure, and the electroch...

Embodiment 3

[0033] Weigh MnSO 4 ·H 2 O 16.90g (0.10mol), NaOH 8.80g (0.22mol), in N 2 Dissolve them in 90 mL of boiled deionized water under protection; drop the NaOH solution into the MnSO 4 In solution, the obtained Mn(OH) 2 The precipitate was aged in a water bath at 80°C for 10 hours; weigh LiOH·H 2 O solid powder 41.96g (1.0mol), added to the above Mn(OH) 2 in the suspension and stir to dissolve; weigh (NH 4 ) 2 S 2 o 8 17.10 g (0.075 mol) of oxidant, dissolved in 70 mL of boiled deionized water, was added dropwise to the reaction system at a uniform rate within 2 hours, and the reaction was continued for 15 hours in a water bath at 80°C; the product was filtered with a glass sand funnel and then Wash and filter with 180mL deionized water for 3 times, and then vacuum dry at 120°C for 8 hours to obtain the product of the present invention. ICP and XRD analysis showed that the product composition was Li 0.99 MnO 2 , which is an orthorhombic layered lithium manganese oxide st...

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Abstract

In the method, under protection of nitrogen gas, manganese salt and strong alkali are dissolved in boiled deionisation respectively to prepare forebody material of manganous hydroxide in laminate structure. According to certain proportion, adding intercalation object of lithium compound to suspending liquid of laminate forebody and carrying out intercalation prepares laminate lithium manganate under synergetic effect of oxidant. Chemical constitution formula of lithium manganate is LixMnO2 (0.8 is less than or equal to x is less than or equal to 1.0). Characters of produced lithium manganate are orthorhombic crystal system, Pmnm spatial symmetry, high purity, no impurity phases, and controllable even grain size. Laminate lithium manganate as material of positive pole provides high specific capacity and good cycle performance. Features of the invention are simple technique, cheap material and easy to realize commercial manufacture.

Description

technical field [0001] The invention relates to an oxidation-intercalation preparation method of layered lithium manganese oxide, which is a cathode material of lithium ion batteries, and belongs to the technical field of preparation of lithium ion battery materials. Background technique [0002] In lithium-ion batteries, electrode materials are an important part of them, especially the positive electrode materials are used in a large amount and are expensive, which is a key factor affecting the performance and production cost of lithium-ion batteries. [0003] At present, commercial lithium-ion batteries mostly use layered lithium cobalt oxide LiCoO 2 as anode material. Lithium cobalt oxide has excellent electrochemical performance. However, cobalt is expensive and pollutes the environment, which greatly restricts the popularization of lithium-ion batteries using lithium cobaltate as the positive electrode material, especially in the development of large-capacity electric...

Claims

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Application Information

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IPC IPC(8): C01D15/00C01G45/00H01M4/02H01M4/04H01M4/48H01M4/50H01M4/58H01M10/36
CPCH01M4/505Y02E60/122H01M4/131H01M10/052Y02E60/10
Inventor 段雪杨文胜李晓丹
Owner BEIJING UNIV OF CHEM TECH
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