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Preparation method of lithium iron phosphate cathode material simultaneously blended with silver and iodine

A technology of lithium iron phosphate and positive electrode materials, which is applied in the direction of electrode manufacturing, battery electrodes, capacitor electrodes, etc., can solve the problems of difficult control and instability of the stoichiometric ratio, achieve low raw material costs, increase the discharge voltage platform, and manufacture The effect of simple process

Inactive Publication Date: 2010-03-17
FUJIAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When using the solid-phase sintering method in which oxygen-site dopants are mixed with pre-sintered materials of other parent-site dopants, since the sintering temperature of this patent is in the temperature range of 550°C to 850°C, the doping used for oxygen-site doping Most of the dopants are unstable at high temperature, and the stoichiometric ratio of the dopant used for oxygen doping in the preparation of the product is difficult to control

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] According to the molar ratio of lithium ion: ferrous ion: phosphate ion: silver ion: iodide ion is 0.95: 0.90: 0.90: 0.0010: 0.0010 weighing reaction compound lithium carbonate (Li 2 CO 3 ) 35 grams, ferrous oxalate (FeC 2 o 4 2H 2 O) 161 grams, phosphoric acid (H 3 PO 4 ) 88.2 grams, silver chloride (AgCl) 0.14 grams, lithium iodide (LiI 3H 2 (0) 0.19 g. Weigh out 1.4 grams of polyvinyl alcohol. Measure 28.5mL of methanol and divide it into two portions of 4.75mL and 23.75mL.

[0034] Mix the weighed lithium carbonate, ferrous oxalate, phosphoric acid, and silver chloride, add 1.4 grams of polyvinyl alcohol and 4.75 mL of methanol, and mix them by ball milling at a speed of 100 rpm for 1 hour. Vacuum dry. The dried powder sample was placed in a nitrogen atmosphere, heated from room temperature to 300°C at a heating rate of 1°C / min, kept at the temperature for sintering for 3 hours, then heated from 300°C to 650°C at a heating rate of 1°C / min, and kept at the t...

Embodiment 2

[0037] Weigh the reaction compound lithium hydroxide (LiOH H 2 O) 46 grams, ferrous oxide (FeO) 75.4 grams, ammonium dihydrogen phosphate (NH 4 h 2 PO 4 )132g, Ag 2 O 17.4 grams, potassium iodide (KI) 24.9 grams. Weigh 43 grams of rice bran powder. Measure 8662mL of formic acid and divide it into two parts of 787mL and 7875mL.

[0038] The weighed lithium hydroxide, ferrous oxide, ammonium dihydrogen phosphate, Ag 2 O mixing, adding 43 grams of rice bran powder and 787 mL of formic acid, ball milling and mixing for 1 hour at a speed of 100 rpm, and vacuum drying at 70° C. under a pressure of 10 Pa. The dried powder sample was placed in a mixture of nitrogen and argon with a volume ratio of 10:1, heated from room temperature to 600°C at a rate of 1°C / min, kept at the temperature for sintering for 18 hours, and then sintered at a rate of 1°C / min Heating from 600°C to 650°C, maintaining the temperature for sintering for 3 hours, and cooling to room temperature to prepare a...

Embodiment 3

[0041] Weigh the reaction compound lithium acetate (LiCOOCH 3 2H 2 O) 96 grams, ferrous chloride (FeCl 2 ) 133 grams, ammonium monohydrogen phosphate ((NH 4 ) 2 HPO 4 ) 119 grams, basic silver carbonate (Ag 3 (OH)CO 3 ) 0.14 g, germanium iodide (GeI 4 ) 21.7 grams. Weigh out 1.7 grams of flour. Measure 3451mL of propanol and divide it into two portions of 575mL and 2876L.

[0042] Mix the weighed lithium acetate, ferrous chloride, ammonium monohydrogen phosphate, and basic silver carbonate, add flour and 575mL propanol, and ball mill for 5 hours at a speed of 300 rpm. Vacuum dry. Place the dry powder sample in a mixture of nitrogen and hydrogen with a volume ratio of 10:1, heat it from room temperature to 300°C at a heating rate of 30°C / min, keep the temperature for sintering for 3 hours, and then sinter at a heating rate of 10°C / min Heating from 300°C to 900°C, keeping the temperature for sintering for 15 hours. Cool to room temperature to prepare silver-doped pre...

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Abstract

The invention relates to a preparation method of a lithium iron phosphate cathode material which can be used for lithium ion batteries, lithium batteries, polymer lithium ion batteries and super capacitors. The adopted technical scheme is as follows: mixing lithium source compounds, ferrous source compounds, phosphate source compounds and silver blending agent, adding wet-milling medium and carbon-containing compounds or carbon powder, ball milling and mixing for 1-15 hours, vacuum drying at any temperature between 70 DEG C and 135 DEG C, then preparing a silver-doped precursor out of the dried powder samples by a two-section sintering method; and then mixing the silver-doped precursor, nickel blending agent and wet-milling medium, ball milling and mixing for 1-15 hours, vacuum drying at any temperature between 70 DEG C and 120 DEG C, then preparing the lithium iron phosphate simultaneously blended with silver and iodine from the dried powder samples by a low-temperature sintering method. The method has lower raw material cost, wide raw material source and simple preparation process, simultaneously, the discharge platform of the sample rises in voltage, is prolonged and has excellent cycle performance under the situation of large-current discharge.

Description

technical field [0001] The invention belongs to the technical field of lithium ion battery electrode materials, and relates to a preparation method of a lithium iron phosphate cathode material that can be used for lithium ion batteries, lithium batteries, polymer lithium ion batteries and supercapacitors. technical background [0002] As a new generation of energy systems, lithium-ion batteries are widely used in electric vehicles, satellites, aerospace and military fields. Numerous studies have shown that LiFePO 4 May become one of the most promising cathode materials for lithium-ion batteries. However, since LiFePO 4 Due to the limitations of its own structure, the material has low electronic conductivity and poor ion conductivity, resulting in poor performance of high-rate charge and discharge, and cannot meet the requirements of practical applications without modification. In order to overcome the deficiency of lithium iron phosphate, extensive research has been carri...

Claims

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Application Information

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IPC IPC(8): H01M4/04H01M4/58H01G9/04
CPCY02E60/12Y02E60/13Y02E60/10
Inventor 童庆松
Owner FUJIAN NORMAL UNIV