Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Lithium iron phosphate and ferrous phosphate, and preparation methods thereof

A technology of ferrous phosphate and lithium iron phosphate, which is applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc. Control the morphology, the crystal is easy to grow larger and other problems, to achieve the effect of suitable for large-scale production, low synthesis cost, and easy control

Inactive Publication Date: 2011-05-25
TSINGHUA UNIV
View PDF3 Cites 12 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently commonly used iron source precursors mainly include: ferric phosphate, ammonium ferrous phosphate, ferrous oxalate, ferrous acetate, ferric oxide and ferric oxide; It must go through a high-temperature reduction reaction, and the high-temperature reduction reaction is difficult to control, so the ferric salt due to incomplete reaction or elemental iron due to excessive reduction is very likely to appear in the product; the precursor of ferrous ammonium phosphate It is difficult to control the morphology during the preparation process, and the crystals are easy to grow larger, which seriously affects the bulk density and high-current electrochemical performance of the final lithium iron phosphate product; if ferrous oxalate or ferrous acetate is used as the iron source precursor , then iron and phosphorus are in different compounds, and iron and phosphate radicals are difficult to diffuse in solid-state reactions, so as long as the raw materials are not mixed uniformly at the atomic level, the reaction may not be complete

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Lithium iron phosphate and ferrous phosphate, and preparation methods thereof
  • Lithium iron phosphate and ferrous phosphate, and preparation methods thereof
  • Lithium iron phosphate and ferrous phosphate, and preparation methods thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 1) prepare the mixed solution of ferrous sulfate and phosphoric acid, wherein the concentration of ferrous sulfate is 1.5mol / L, and the concentration of phosphoric acid is 1mol / L; Configuration concentration is the sodium hydroxide solution of 3mol / L; Under stirring condition, use The mixed solution of ferrous sulfate and phosphoric acid and sodium hydroxide solution are continuously input into the reactor with a volume of 1.5L by the metering pump respectively, and the flow rate of the mixed solution of ferrous sulfate and phosphoric acid is controlled at 6mL / min. The flow rate of 5L / min is fed into nitrogen; the flow rate of sodium hydroxide solution is adjusted so that the pH value of the reaction liquid in the reactor is 6.5±0.05; the temperature of the reaction liquid in the reactor is 50°C; the mixed material in the reactor is reacted The overflow port of the reactor is naturally overflowed and discharged; stop feeding after 20 hours of continuous feeding, and disc...

Embodiment 2

[0025] 1) prepare the mixed solution of ferrous chloride and potassium phosphate, wherein the concentration of ferrous chloride is 3mol / L, and the concentration of potassium phosphate is 2mol / L; Configuration concentration is the potassium hydroxide solution of 6mol / L; Next, the mixed solution of ferrous chloride and potassium phosphate, and potassium hydroxide solution were continuously input into a reactor with a volume of 1.5 L with a metering pump, and the flow rate of the mixed solution of ferrous chloride and potassium phosphate was controlled at 3 mL / min. , while feeding argon into the reactor at a flow rate of 20 L / min; adjusting the flow rate of the potassium hydroxide solution so that the pH value of the reaction solution in the reactor is 6.0 ± 0.05; the temperature of the reaction solution in the reactor is 30 ° C; The mixed material in the reactor is naturally overflowed and discharged through the overflow port of the reactor; stop feeding after 20 hours of continu...

Embodiment 3

[0029] 1) prepare the mixed solution of ferrous sulfate and sodium phosphate, wherein the concentration of ferrous sulfate is 0.15mol / L, the concentration of sodium phosphate is 0.1mol / L; Configuration concentration is the sodium hydroxide solution of 0.1mol / L; Stir Under the conditions, the mixed solution of ferrous sulfate and sodium phosphate, sodium hydroxide solution are continuously input into the reactor with a volume of 1.5L respectively with a metering pump, and the flow of the mixed solution of ferrous sulfate and sodium phosphate is controlled at 10mL / min. At the same time, feed nitrogen into the reactor at a flow rate of 0.1L / min; adjust the flow rate of the sodium hydroxide solution so that the pH value of the reaction solution in the reactor is 7.0 ± 0.05; the temperature of the reaction solution in the reactor is 80 ° C; The mixed material in the reactor is naturally overflowed and discharged through the overflow port of the reactor; stop feeding after 20 hours o...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses lithium iron phosphate and ferrous phosphate, and preparation methods thereof. The preparation method of the ferrous phosphate comprises the following steps of: mixing bivalent iron salt aqueous solution and phosphate ion aqueous solution under the protection of inert gas; controlling the pH value in the reaction process to be between 6.0 and 7.0; drying after the reaction is finished to obtain a spherical ferrous phosphate hydrate precursor; and performing thermal processing to obtain the ferrous phosphate. The preparation method of the lithium iron phosphate comprises the following steps of: uniformly mixing the obtained ferrous phosphate, a phosphorus source compound, a lithium source compound and a carbon source compound; and performing thermal treatment in an inert gas atmosphere at a high temperature to obtain the lithium iron phosphate. The ferrous phosphate precursor with the particle diameter of between 0.5 and 10 mu m can be prepared by the method; reduction reaction is not required in the process of preparing the lithium iron phosphate from the precursor, so the thermal treatment temperature can be greatly reduced; and the prepared lithium iron phosphate material has higher stacking density and higher electrochemical performance and has a great application prospect in the field of lithium ion batteries.

Description

technical field [0001] The invention belongs to the technical field of energy materials, and relates to lithium ion battery positive electrode materials, in particular to lithium iron phosphate, a lithium ion battery positive electrode material, and its precursor, ferrous phosphate, and their preparation methods. Background technique [0002] LiFePO with orthorhombic olivine structure 4 Cathode materials have become ideal cathode materials for power lithium-ion batteries due to their excellent low cost, long cycle life and high safety performance. Its advantages are outstanding, but there are also some shortcomings. The low bulk density and poor high-current electrochemical performance are the main obstacles affecting the application of this material in the field of high-power and large-capacity lithium-ion batteries. Synthesizing powder particles with a spherical shape can greatly increase the packing density of the material; compounding with conductive carbon materials ca...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C01B25/45C01B25/37H01M4/1397H01M4/58
CPCY02E60/12Y02E60/122Y02E60/10
Inventor 高剑姜长印李建军杨改万春荣陈克勤
Owner TSINGHUA UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products