Preparation method for positive electrode material of iron, lithium and manganese phosphate battery

A cathode material, lithium iron phosphate technology, applied in the field of electrochemical power supply, can solve the problems that cannot meet the application requirements of cathode materials for power lithium-ion batteries, insufficient mixing of reactants, and poor uniformity of reaction products, etc., to shorten the drying time , saving preparation time, and suppressing the effect of hindering charge transfer

Inactive Publication Date: 2014-08-13
宁波艾能锂电材料科技股份有限公司
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Problems solved by technology

Gong Qiang, Liao Xiaozhen 1 The research of Li(Fe y mn 1-y )PO 4 The material has different degrees of improvement in the discharge platform and conductivity, but its rate performance is still not ideal, and it cannot meet its application requirements as a cathode material for power lithium-ion batteries.
On the other hand, the mixing of the reactants in the traditional solid-phase synthesis method is not sufficient, and the poor uniformity of the reaction product is also one of the reasons for the reduction of the effective capacity of the material.
The preparation of sol can make the raw materials mix uniformly to achieve a molecular-level homogeneous multi-component system, but the drying time of sol-gel is long, and the drying energy consumption is large; at the same time, due to the slow dispersion of solvent water, the gel continues to collapse and the volume shrinks greatly

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  • Preparation method for positive electrode material of iron, lithium and manganese phosphate battery

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Embodiment 1

[0016] Example 1 Select lithium hydroxide, ferrous oxalate, manganese oxalate, phosphoric acid, magnesium nitrate and glucose as lithium source, iron source, manganese source, phosphorus source, metal salt and carbon source respectively, according to the elemental molar ratio Li: Fe: Mn :P:Mg=1.07:0.75:0.25:1:0.02 Weigh and set aside. Lithium hydroxide was added to ethanol, heated and stirred at 40°C for 2h. Sol A was formed by adding ferrous oxalate, manganese oxalate and magnesium nitrate. The complexing agent citric acid was added to the phosphoric acid-containing ethanol aqueous solution to obtain solution B, and glucose was added to solution B (converted into carbon and the mass fraction of the total mass of raw materials was 4%). Sol A and solution B were mixed and heated to 60°C, and the pH was adjusted with ammonia water to form gel C. Gel C was microwave-dried for 10 minutes to obtain a powder precursor. The precursor is ground into fine components, and the obtaine...

Embodiment 2

[0017] Example 2 Lithium hydroxide, iron phosphate, manganese oxalate, phosphoric acid, magnesium nitrate and glucose are selected as lithium source, iron source, manganese source, phosphorus source, metal salt and carbon source respectively, according to the elemental molar ratio Li:Fe:Mn: P: Mg=1.07:0.75:0.25:1:0.02 Weigh and set aside. Lithium hydroxide was added to ethanol, heated and stirred at 50°C for 2h. Sol A was formed by adding iron phosphate, manganese oxalate and magnesium nitrate. The complexing agent citric acid was added to the phosphoric acid-containing ethanol aqueous solution to obtain solution B, and glucose was added to solution B (converted into carbon and accounted for 5% of the total mass of raw materials). Sol A and solution B were mixed and heated to 60°C, and the pH was adjusted with ammonia water to form gel C. Gel C was microwave-dried for 10 minutes to obtain a powder precursor. The precursor is ground into fine components, and the obtained pow...

Embodiment 3

[0018] Embodiment 3 selects lithium hydroxide, ferromanganese phosphate, phosphoric acid, magnesium nitrate and glucose as lithium source, iron source, manganese source, phosphorus source, metal salt and carbon source respectively, wherein ferromanganese phosphate is simultaneously used as iron source and manganese source, It can also be used as a phosphorus source, weighed according to the elemental molar ratio Li:Fe:Mn:P:Mg=1.05:0.5:0.5:1:0.02 and then used. Lithium hydroxide was added to ethanol, heated and stirred at 40°C for 2h. Sol A was formed by adding ferromanganese phosphate and magnesium nitrate. The complexing agent citric acid was added to the phosphoric acid-containing ethanol aqueous solution to obtain solution B, and glucose was added to solution B (converted into carbon and the mass fraction of the total mass of raw materials was 2%). Sol A and solution B were mixed and heated to 60°C, and the pH was adjusted with ammonia water to form gel C. Gel C was micr...

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Abstract

The invention provides a method for synthesizing a positive electrode material of a nano-level iron, lithium and manganese phosphate battery (Li(FeyMn1-y)XzPO4/C) which is high in energy density, is provided with a high-discharge-voltage platform and is excellent in conductivity by combining a sol-gel method with a microwave drying method. The method comprises the following steps of a, adding a lithium source, an iron source, a manganese source and metal X salt into ethyl alcohol to prepare sol A; b, adding citric acid into a phosphorus source-containing ethyl alcohol aqueous solution, and adding a carbon source into the phosphorus source-containing ethyl alcohol aqueous solution to obtain a solution B, wherein the carbon source added into the solution B contains 1-5 percent of carbon elements by mass; c, mixing and heating the sol A and the solution B, and adjusting the pH to form gel C; d, performing microwave drying on the gel C to obtain a precursor; e, preparing powder from the precursor, and pre-burning, sintering and screening the powder under protection gas to obtain the positive electrode material of the iron, lithium and manganese phosphate battery.

Description

technical field [0001] The invention belongs to the field of electrochemical power sources, and in particular relates to a sol-gel preparation method of a lithium iron phosphate lithium manganese battery cathode material. Background technique [0002] The development and application of high-performance positive and negative electrode materials still largely influence the development of lithium-ion batteries. At present, commercial lithium-ion batteries mostly use graphite-like carbon materials as negative electrodes, and transition metal oxides (such as LiCoO 2 ) is the cathode material. Olivine-type lithium iron phosphate (Li iron phosphate) can reversibly remove all lithium ions to form structurally stable iron phosphate (iron phosphate), and release a reversible capacity of up to 170mAh / g. Advantages as a cathode material for lithium-ion batteries: Safety issues ; Wide source of raw materials, low price; no pollution; very long cycle life, which can meet the needs of fr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58H01M4/62C01B25/45
CPCC01B25/45H01M4/366H01M4/5825H01M4/625H01M10/0525Y02E60/10
Inventor 肖锋牟菲罗林君苗意外
Owner 宁波艾能锂电材料科技股份有限公司
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