Carbon-free nanoscale lithium iron phosphate and preparation method thereof

A lithium iron phosphate, carbon nanotechnology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of affecting electrochemical performance, Fe dislocation, low temperature, etc., to achieve enhanced electrochemical performance, fine particle size, simple craftsmanship

Active Publication Date: 2010-01-20
SHENZHEN DYNANONIC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with the high-temperature solid-phase method, the synthesis temperature of the hydrothermal method is lower, about 150°C to 200°C, and the reaction time is only about 1/5 of the solid-state reaction, and lithium iron phosphate can be directly obtained, and the product grain size is smaller , uniform phase, especially

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Lithium carbonate (molecular formula Li 2 CO 3 , 0.475mol) 35.15g, ferric nitrate (molecular formula Fe(NO 3 ) 3 9H 2 O, 1mol) 404g, ammonium dihydrogen phosphate (molecular formula NH 4 h 2 PO 4 , 1mol) 115g, aluminum nitrate (molecular formula Al(NO 3 ) 3 9H 2 (2,0.05mol) and 18.75g were mixed to obtain mixture A. Mixture A was mixed with 57.3 g of malic acid and dissolved in water to obtain a mixed material. Mill the mixed material in a planetary ball mill for 10 hours, place the milled mixed material in a blower dryer at a temperature of 80°C for 20 hours to obtain a powder, and pulverize the obtained powder with a crushing equipment. The pulverized The powder is placed in an air atmosphere furnace and sintered at a temperature of 400° C. for 10 hours to obtain an oxidized carbon-free nano-lithium iron phosphate powder material. The obtained powder was placed in a mixed atmosphere furnace of hydrogen and nitrogen (the volume of hydrogen is 5%, the rest is...

Embodiment 2

[0031] Lithium hydroxide (molecular formula LiOH, 1mol) 24g, ferric hydroxide (molecular formula Fe(OH) 3 , 0.95mol) 101.65g, phosphoric acid (molecular formula H 3 PO 4 , 1mol) 98g, copper nitrate (molecular formula Cu(NO 3 ) 2 ·3H 2 (2,0.05mol) and 12.08g were mixed to obtain mixture A. The mixture A was mixed with 1178.65 g of sucrose and dissolved in ethanol to obtain a mixed material. The mixed material was ball-milled in a planetary ball mill for 20 hours, and the ball-milled mixed material was placed in a blast dryer at a temperature of 100° C. for 18 hours to obtain a powder, which was pulverized by a crushing device. The pulverized powder is placed in an air atmosphere furnace and sintered at a temperature of 450° C. for 8 hours to obtain an oxidized carbon-free nano-lithium iron phosphate powder material. The obtained powder was placed in a mixed atmosphere furnace of hydrogen and nitrogen (the volume of hydrogen is 10%, the rest is nitrogen) and treated at a t...

Embodiment 3

[0035] Lithium nitrate (molecular formula LiNO 3 , 1mol) 69g, ferrous oxalate (molecular formula FeC 2 o 4 2H 2 O, 1mol) 179.9g, diammonium hydrogen phosphate (molecular formula (NH 4 ) 2 HPO 4 , 0.95mol) 125.4g, boron oxide (molecular formula B 2 o 3 , 0.025mol) and 1.74g were mixed to obtain mixture A. The mixture A was mixed with 752 g of glucose and dissolved in propanol to obtain a mixed material. The mixed material was ball-milled in a planetary ball mill for 30 hours, and the ball-milled mixed material was placed in a blast dryer at a temperature of 150° C. for 15 hours to obtain a powder, which was pulverized by a crushing device. The pulverized powder is placed in an oxygen atmosphere furnace and sintered at a temperature of 500° C. for 6 hours to obtain an oxidized carbon-free nano-lithium iron phosphate powder material. The obtained powder was placed in a mixed atmosphere furnace of hydrogen and nitrogen (the volume of hydrogen is 20%, the rest is nitrogen)...

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Abstract

The invention relates to a carbon-free nanoscale lithium iron phosphate and a preparation method thereof. The carbon-free nanoscale lithium iron phosphate is prepared by mixing a lithium compound, an iron compound, a phosphorous compound and a doped element compound according to a molar ratio so as to form a mixture A; and the mixture A and a complexing agent are mixed and dissolved in a solvent to form the lithium iron phosphate with a nanoscale grain size. The preparation method comprises the following steps: mixing the mixture A and the complexing agent to form a mixed material; ball milling and drying the mixed material to obtain a powder material; pulverizing the obtained powder by pulverizing equipment and then sintering the powder in an oxidized atmosphere furnace to obtain an oxidized carbon-free nanoscale lithium iron phosphate powder material; and treating the obtained powder material in a reducing atmosphere furnace to obtain carbon-free nanoscale lithium iron phosphate powder. The carbon-free nanoscale lithium iron phosphate has the grain size of 30-500nm, a specific surface area of 1-50m<2>/g and tap density of 0.7-2.5g/cm<3>, has fine and even grain and high purity and does not contain carbon materials. Because doped elements are added, the electrochemical performance is enhanced. The preparation method has simple process and easy realization of industrialization.

Description

【Technical field】 [0001] The invention relates to nano-lithium iron phosphate and a preparation method thereof, in particular to a carbon-free nano-lithium iron phosphate and a preparation method thereof. 【Background technique】 [0002] Lithium iron phosphate (LiFePO 4 ) is a lithium battery cathode material with an olivine structure developed in recent years, which has the characteristics of reversibly intercalating and deintercalating lithium. Compared with traditional lithium-ion secondary battery cathode materials, its raw materials have wider sources, lower prices, non-toxicity, and no environmental pollution. In particular, its safety performance and cycle life are unmatched by other materials. These It is also the most important technical index of power batteries, which makes countries all over the world compete to realize industrialized production. Lithium iron phosphate has high energy density (its theoretical specific capacity is 170mAh / g, and the actual specific...

Claims

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Application Information

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IPC IPC(8): C01B25/45H01M4/58H01M4/24
CPCY02E60/124Y02E60/10
Inventor 孔令涌吉学文王允实
Owner SHENZHEN DYNANONIC
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