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Preparation method of lithium iron phosphate/lithium vanadium phosphate composite material

A technology of lithium vanadium phosphate and lithium iron phosphate, which is applied in the field of electrochemical power supply material preparation, can solve problems such as difficulty in meeting industrialized large-scale preparation, uneven heating of bulk materials, and ascorbic acid consumption, and is easy to realize industrialized scale production. , regular particle morphology, excellent abnormal temperature and low temperature electrochemical performance effect

Inactive Publication Date: 2013-10-16
XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the whole process of WO02 / 083555A2 method including precursor preparation requires inert protection, oxidative ferric iron and nitric acid consume expensive ascorbic acid, which is not conducive to industrialization
Chinese patent CN1431147A uses a closed container to prepare the precursor, which eliminates the protective atmosphere, but the process is still relatively complicated, and it is not easy to expand production
This type of method can obtain pure lithium iron phosphate, but usually uses special test equipment such as a high-pressure reaction vessel, and the microwave method has the disadvantage of uneven heating of bulk materials, so it is difficult to meet the requirements of large-scale industrial production

Method used

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  • Preparation method of lithium iron phosphate/lithium vanadium phosphate composite material
  • Preparation method of lithium iron phosphate/lithium vanadium phosphate composite material
  • Preparation method of lithium iron phosphate/lithium vanadium phosphate composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] a. Molar ratio Fe:V:Li:P:H 2 C 2 o 4 =50:2:53:53:27 Weigh iron phosphate, vanadium pentoxide, lithium carbonate, ammonium dihydrogen phosphate and oxalic acid (raw material purity is 99.9%), fully mix, grind in agate mortar, grind time 3h;

[0032] b. Heat-treat the powder in step a under a protective gas nitrogen atmosphere with an air flow rate of 0.2 L / min, raise the temperature at a heating rate of 5°C / min, bake at a temperature of 300°C for 5 hours, and then heat it at a temperature of 1°C / min. Speed ​​down to room temperature;

[0033] c. Add carbon source glucose with a mass fraction of 5% to the powder obtained in step b (the mass fraction of carbon in the composite material after decomposition is 1.6%-2.4%), and grind for 1 hour;

[0034] d. Press-molding the powder in step c, and heat-treating it under the protective gas nitrogen atmosphere, the molding pressure is 10MPa, the airflow speed is 0.2L / min, the heating rate is 5°C / min, and the temperature is 65...

Embodiment 2

[0037] a. Molar ratio Fe:V:Li:P:H 2 C 2 o 4 =40:2:43:43:22 Weigh iron phosphate, vanadium pentoxide, lithium carbonate, ammonium dihydrogen phosphate and oxalic acid (purity of raw material is 99.9%), mix well, grind in agate mortar, grinding time 5h ;

[0038] b. Heat-treat the powder in step a under the protective gas argon atmosphere, the air flow rate is 0.4L / min, the temperature is raised at a heating rate of 7°C / min, and the temperature is roasted at 330°C for 8 hours, and then the temperature is 3°C / min cooling down to room temperature;

[0039] c. Add carbon source sucrose with a mass fraction of 20% to the powder obtained in step b (the mass fraction of carbon in the composite material after decomposition is 6.7%-10%), and grind for 1-4 hours;

[0040] d. Press-molding the powder in step c, heat treatment under the protective gas argon atmosphere, the molding pressure is 15MPa, the air flow rate is 0.4L / min, the temperature is raised at a heating rate of 7°C / min, ...

Embodiment 3

[0043] a. Molar ratio Fe:V:Li:P:H 2 C 2 o 4 =40:2:43:43:22 Weigh iron phosphate, vanadium pentoxide, lithium hydroxide, ammonium dihydrogen phosphate and oxalic acid (raw material purity is 99.9%), mix well, grind in agate mortar, grind time 5.5 hours;

[0044] b. Heat-treat the powder in step a under the protective gas argon atmosphere, the air flow rate is 0.5L / min, the temperature is raised at a heating rate of 8°C / min, and the temperature is roasted at 350°C for 10 hours, and then the temperature is 5°C / min cooling down to room temperature;

[0045] c. Add 15% carbon source glucose (the mass fraction of carbon in the composite material after decomposition is 4.8%-7.2%) to the powder obtained in step b, and grind for 1-4 hours;

[0046] d. Press-molding the powder in step c, heat-treating it under the protective gas argon atmosphere, the molding pressure is 20MPa, the airflow velocity is 0.5L / min, the temperature is raised at a heating rate of 8°C / min, and then roasted ...

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Abstract

The invention relates to a preparation method of a lithium iron phosphate / lithium vanadium phosphate composite material. The method comprises the following steps: mixing iron phosphate and vanadium pentoxide which are utilized as raw materials with a lithium salt compound; adding a chelating agent; grinding and mixing; performing heat treatment in an inert atmosphere, and then adding a carbon source material; and heating, roasting and cooling to room temperature to obtain the carbon-coated lithium iron phosphate / lithium vanadium phosphate composite material. The lithium iron phosphate / lithiumvanadium phosphate composite material can be assembled into a testing battery of which the discharge specific capacity can reach 144mAh / g with the current of 150mA / g at room temperature and can reach105mAh / g with the current of 30mA / g at the temperature of minus 20 DEG C, the crystal form is complete, the particle appearance is regular, and excellent normal-temperature and low-temperature electrochemical performances are shown. All the raw materials in the method are bulk industrial chemicals, the cost is low, the process route is simple, the industrial scale production is easy to realize and the application prospect is very broad.

Description

technical field [0001] The invention belongs to the technical field of preparation of electrochemical power source materials. In particular, it relates to a method for preparing lithium ion cathode composite materials lithium iron phosphate / lithium vanadium phosphate by oxalic acid chelation-assisted carbothermal reduction method. It has broad application prospects in the field of commonly used secondary lithium ion batteries and power energy battery cathode materials. Background technique [0002] Energy and the environment are two severe issues that must be faced in the 21st century, and the development of clean and renewable new energy is one of the most decisive technical fields in the future world economy. As a kind of electrochemical energy source, lithium-ion battery has the advantages of high working voltage, light weight, large specific energy, small self-discharge, long cycle life, no memory effect, and less environmental pollution. [0003] On the one hand, the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/58
CPCY02E60/12Y02E60/10
Inventor 康雪雅刘志强华宁吐尔迪·吾买尔李程峰
Owner XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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