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A method for preparing nickel-manganese composite oxide hollow spheres
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A composite oxide, hollow sphere technology, applied in electrochemical generators, electrical components, battery electrodes, etc., can solve the problem of reducing the cycle performance of materials, and achieve the effect of maintaining monodispersity and improving electrochemical performance.
Active Publication Date: 2016-05-18
HEFEI GUOXUAN HIGH TECH POWER ENERGY
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Co-precipitation preparation technology has become a very important method for this material, but in the process of preparing spinel from the product obtained by using carbonate as a coprecipitant, it is inevitable that the manganese in the material will completely become tetravalent, and a large amount of trivalent manganese The existence of the material will significantly reduce the cycle performance of the material
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Embodiment 1
[0030] In this embodiment, the nickel salt is nickel sulfate, the manganese salt is manganese sulfate, the carbonate is sodium carbonate, the oxidizing agent is potassium permanganate, and the lithium source is lithium acetate.
[0031] 1. Weigh 13.14g of nickel sulfate and 15.21g of manganese sulfate, and add them into deionized water to form a 400mL metal ion mixed solution, and weigh 19.29g of sodium carbonate to form a 400mL aqueous solution, and use a peristaltic pump to control the feeding rate to 2mL / min, adding the mixed solution of metal ions to the mixed solution of carbonate. After the addition is complete, age for 10-20 h, filter the precipitate and wash with deionized water. Vacuum dry before use.
[0032] 2. Weigh 0.237g of potassium permanganate and dissolve it in 30mL of deionized water, add 0.4075g of the dried precipitate, evenly disperse it, transfer it to a hydrothermal reaction kettle with a teflon liner, heat to 160°C, and keep it warm for 14h . The t...
Embodiment 2
[0038] In this embodiment, the nickel salt is nickel sulfate, the manganese salt is manganese sulfate, the carbonate is sodium carbonate, the oxidizing agent is potassium persulfate, and the lithium source is lithium carbonate.
[0039] 1. Weigh 6.57g of nickel sulfate and 12.675g of manganese sulfate, add them into deionized water to form a 300mL aqueous solution, weigh 12.72g of sodium carbonate to form a 300mL aqueous solution, use a peristaltic pump to control the feeding rate to 2mL / min, and mix the metal ions The mixed solution is added to the mixed solution of carbonate. After adding, age for 10-20h, filter the precipitate and wash with deionized water, dry it in vacuum and set aside
[0040] 2. Weigh 0.5134g of potassium persulfate and dissolve it in 30mL of deionized water, add 0.3480g of the dried precipitate, evenly disperse, transfer to a hydrothermal reaction kettle with a teflon liner, heat to 120°C, and keep warm for 6h. The target product was obtained after ce...
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Abstract
The invention discloses a method for preparing hollow nickle-manganese composite oxide balls. The method comprises the following steps: adding water into nickle salt and manganese salt to prepare a metal-ion mixed solution, preparing carbonate into a carbonate solution, and adding the metal-ion mixed solution into the carbonate mixed solution to form a coprecipitation precursor; uniformly dispersing the prepared coprecipitation precursor and a solution containing an oxidizing agent, and performing hydrothermal reaction to prepare a product; and uniformly mixing the obtained product and a lithium source according to a molar ratio of 1:(1-1.1), and calcining for 8-24 hours at the temperature of 500-900 DEG C. The method disclosed by the invention has the advantages that the in-situ oxidation-reduction reaction is adopted and the coprecipitated carbonate can be oxidized in situ to form a precursor of nickle-manganese spinel material, so that the condition of increase of trivalent manganese caused by the incomplete oxidation of Mn in the conversion process from pure carbonate to nickle-manganese spinel is avoided; due to the Kirkendal effect in the chemical reaction, the hollow structure is formed, so that the electro-chemical performance of the material is enhanced.
Description
technical field [0001] The invention belongs to the field of raw materials and negative electrodes of positive electrode materials of lithium ion batteries, and in particular relates to a method for preparing nickel-manganese composite oxide hollow spheres. Background technique [0002] Transition metal oxides have attracted the attention of scientists, especially lithium battery scientists, for many years. Existing positive electrode materials of mature systems such as: lithium cobalt oxide with layered structure, lithium manganese oxide and lithium nickel manganese oxide with spinel structure, and lithium iron phosphate materials with olivine structure. The central elements correspond to transition elements respectively. cobalt, manganese, nickel, iron, etc. As an important negative electrode material for lithium-ion batteries, transition metal oxides, such as CoO, Co3O4, Fe2O3, and CuO, all use the valence change of transition metal oxides to make them have reversible ca...
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