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Li and Mn codoped manganese phosphate/carbon composite material and preparation method thereof

A carbon composite material, lithium manganese phosphate technology, applied in electrical components, battery electrodes, circuits, etc., can solve the problems of difficult control of particle size and distribution, low discharge specific capacity, unstable cycle, etc., and achieve the suppression of particle agglomeration , speed up the diffusion rate, increase the effect of the reaction contact area

Active Publication Date: 2014-03-26
广东省科学院资源利用与稀土开发研究所
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to solve the problems of existing lithium manganese phosphate positive electrode materials such as poor conductivity, low discharge specific capacity, unstable cycle, etc., and overcome the difficulty in controlling the particle size and distribution of traditional solid-phase reaction products in the existing preparation technology, carbon-coated Cover uneven defects, provide a Li, Mn site co-doped manganese phosphate lithium / carbon composite material and its preparation method

Method used

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  • Li and Mn codoped manganese phosphate/carbon composite material and preparation method thereof
  • Li and Mn codoped manganese phosphate/carbon composite material and preparation method thereof
  • Li and Mn codoped manganese phosphate/carbon composite material and preparation method thereof

Examples

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Effect test

Embodiment 1

[0030] Disperse manganese carbonate and ferrous oxalate in a 30.0wt% oxalic acid solution at a molar ratio Mn:Fe of 0.88:0.12, and stir for 0.5 hours to form a 2.0mol / L emulsion. The emulsion was flash-dried to obtain a dry mixed powder, and the mixed powder was calcined at 600 °C for 2 hours under the protection of argon to synthesize the product Mn 0.88 Fe 0.12 O, obtained nanoscale Mn by ball milling 0.88 Fe 0.12 O. Next, diammonium hydrogen phosphate, lithium hydroxide, magnesium hydroxide and nanoscale Mn 0.88 Fe 0.12 O is dispersed in the ratio of 1.04:0.9:0.12:0.88 by molar ratio P:Li:Mg:Mn in the oxalic acid solution of 30.0wt% and adds sucrose, and the addition amount of sucrose is ammonium dihydrogen phosphate, lithium hydroxide, magnesium hydroxide and Nanoscale Mn 0.88 Fe 0.12 20.0wt% of the total mass of the mixture formed by O was stirred for 3 hours to form a 2.0mol / L emulsion, and the emulsion was dried at 80°C for 8 hours to obtain a paste, which was st...

Embodiment 2

[0032] Disperse manganese oxalate and nickel acetate in a 30.0wt% oxalic acid solution at a molar ratio Mn:Ni of 0.92:0.08, and stir for 4 hours to form a 2.5mol / L emulsion. The emulsion was flash-dried to obtain a dry mixed powder, and the mixed powder was calcined at 550°C for 4 hours under the protection of nitrogen to synthesize

[0033] Product Mn 0.92 Ni 0.08 O, obtained nanoscale Mn by ball milling 0.92 Ni 0.08 O. Next, ammonium dihydrogen phosphate, lithium acetate, magnesium acetate and nanoscale Mn 0.92 Ni 0.08 O is dispersed in the ratio of 1.02:0.94:0.08:0.92 by molar ratio P:Li:Mg:Mn in 30.0wt% oxalic acid solution and adds citric acid, and the addition amount of citric acid is ammonium dihydrogen phosphate, lithium acetate, magnesium acetate, Nanoscale Mn 0.92 Ni 0.08 10.0wt% of the total mass of the mixture formed by O, stirred for 4 hours to form a 2.5mol / L emulsion, the emulsion was dried at 80°C for 6 hours to obtain a paste, and the paste was roasted...

Embodiment 3

[0035] Disperse manganese acetate and nickel hydroxide in a 50vol% ethanol solution at a molar ratio Mn:Ni of 0.85:0.15, and stir for 6 hours to form a 1.0mol / L emulsion. The emulsion was flash-dried to obtain a dry mixed powder, and the mixed powder was calcined at 400°C for 3 hours under the protection of argon to synthesize the product Mn 0.85 Ni 0.15 O, obtained nanoscale Mn by ball milling 0.85 Ni 0.15 O. Next, disodium hydrogen phosphate, lithium oxalate, copper acetate and nanoscale Mn 0.85 Ni 0.15 O is dispersed in a 50.0vol% ethanol solution with a molar ratio of P:Li:Cu:Mn of 1.03:0.87:0.15:0.85 and glucose is added. The amount of glucose added is disodium hydrogen phosphate, lithium oxalate, copper acetate, nano-scale mn 0.85 Ni 0.15 15.0wt% of the total mass of the mixture formed by O was stirred for 0.5 hours to form a 1.0mol / L emulsion, which was dried at 80°C for 2 hours to obtain a paste, which was stored at 750°C under the protection of argon Roast for...

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Abstract

The invention relates to an Li and Mn codoped manganese phosphate / carbon composite material which is characterized in that a general formula of the Li and Mn codoped manganese phosphate / carbon composite material is Li[1-x]AxMn[1-y]ByPO4 / C, wherein x is more than or equal to 0.01 and smaller than or equal to 0.15, y is more than or equal to 0.01 and smaller than or equal to 0.15, x is equal to y, and A and B are divalent metal ions. The preparation method comprises the following steps of firstly preparing nanoscale Mn[1-y]ByO from divalent manganese source and a compound containing metallic element B; preparing paste from a phosphorus source, a lithium source and a compound containing metallic element A and nanoscale Mn[1-y]ByO; and finally roasting the paste under the protection of argon or nitrogen, ball-milling, introducing C1-4 n-alkane gas at 400-600 DEG C to obtain the Li and Mn codoped manganese phosphate Li[1-x]AxMn[1-y]ByPO4 / C. Through the Li and Mn codoping, the electrical conductivity in the material can be improved effectively, and the carbon layer covering the surfaces of particles is uniform and sufficient. The synthetic material has a relatively good discharge performance and cycling stability, the process is simple, the cost is low, and the material can meet the green chemistry development requirement.

Description

technical field [0001] The invention belongs to the technical field of energy material preparation, and specifically relates to a Li and Mn site co-doped lithium manganese phosphate / carbon composite material and a preparation method thereof. Background technique [0002] With the high integration of electronic equipment and the increasingly prominent environmental problems, the development of new chemical power sources with high energy density has become an urgent requirement for the sustainable development of society. With the characteristics of high energy density, long life, safety, reliability, and environmental protection, lithium-ion batteries have been widely used in emerging portable electronic products such as mobile phones, notebook computers, and cameras, and have also played an important role in the field of space technology. However, the electrode material is an important factor restricting the large-scale application of lithium-ion batteries. At present, the m...

Claims

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Application Information

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IPC IPC(8): H01M4/36H01M4/58
CPCH01M4/5825H01M4/62H01M4/626Y02E60/10
Inventor 肖志平王英唐仁衡肖方明李伟孙泰
Owner 广东省科学院资源利用与稀土开发研究所
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