Preparation method of phosphate potential boron-doped carbon-wrapped phosphoric acid iron-lithium material

A carbon-coated lithium iron phosphate and phosphorus-positioned boron technology, which is applied to electrical components, battery electrodes, circuits, etc., can solve the problems of difficulty in controlling the uniformity of synthesis conditions, uneven distribution of elements, and high energy consumption.

Inactive Publication Date: 2013-07-24
XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, solid-phase methods, hydrothermal methods, rheological phase methods, and sol-gel methods all have certain problems in large-scale production, and the energy consumption in the synthesis process is high, which does not meet the current low-carbon and environmental protection requirements, and is not easy to industrialize Applications, for example: Although the process steps of the solid-phase method are simple, the raw material particles are agglomerated during the mixing process of the raw materials, resulting in uneven mixing of the raw materials, resulting in uneven distribution of elements in the product and incomplete lattice structure, which in turn affects the cycle s

Method used

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  • Preparation method of phosphate potential boron-doped carbon-wrapped phosphoric acid iron-lithium material
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  • Preparation method of phosphate potential boron-doped carbon-wrapped phosphoric acid iron-lithium material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] a. The molar ratio is Li:Fe:B:C 2 h 2 o 4 =1:1:0.05:1.2, the amount of carbon source added is 20 wt%, add deionized water, lithium acetate and oxalic acid into the container, stir to dissolve, then add iron phosphate, boric acid and starch, stir at a temperature of 40°C After 15 hours to evaporate to dryness, the stirring speed was 320 r / min, and the evaporated to dryness product was obtained;

[0020] b. Place the evaporated product of step a in an oven at a temperature of 120° C. to fully dry it and grind it thoroughly to obtain a mixture powder;

[0021] c, the mixture powder of step b in N 2 Carry out rapid high-temperature heat treatment under the protection of the atmosphere. The heat treatment conditions are: the flow rate of the protective gas is 0.5 L / min, the temperature is raised at a heating rate of 6°C / min, and the temperature is 450°C for 4 hours at a constant temperature;

[0022] d. Finally, naturally cool down to room temperature with the furnace to...

Embodiment 2

[0024] a. The molar ratio is Li:Fe:B:C 2 h 2 o 4 = 1:1:0.15:1.3, the amount of carbon source added is 5 wt%, add deionized water, lithium oxalate and oxalic acid into the container, stir to dissolve, then add iron phosphate, boric acid and sucrose, and stir at a temperature of 90 °C After 1 hour until evaporated to dryness, the stirring speed was 200 r / min, and the evaporated product was obtained;

[0025] b. Place the evaporated product of step a in an oven at a temperature of 90° C. to fully dry it and grind it thoroughly to obtain a mixture powder;

[0026] c, the mixture powder of step b in N 2 Carry out rapid high-temperature heat treatment under the protection of the atmosphere. The heat treatment conditions are: the gas flow rate of the protective gas is 0.3 L / min, the temperature is raised at a heating rate of 8°C / min, and the temperature is constant for calcination at 650°C for 3 hours;

[0027] d. Finally, naturally cool down to room temperature with the furnace ...

Embodiment 3

[0029] a. The molar ratio is Li:Fe:B:C 2 h 2 o 4 = 1:1:0.20:3.5, the amount of carbon source added is 15 wt%, add deionized water, lithium oxide and oxalic acid into the container, stir to dissolve, then add iron phosphate, boric acid and glucose, stir at a temperature of 45 °C After 13 hours to evaporate to dryness, the stirring speed was 240 r / min, and the product was evaporated to dryness;

[0030] b. Place the evaporated product of step a in an oven at a temperature of 100° C. for sufficient drying, and then fully grind to obtain a mixture powder;

[0031] c, the mixture powder of step b in N 2 Carry out rapid high-temperature heat treatment under the protection of the atmosphere. The heat treatment conditions are as follows: the flow rate of the protective gas is 0.6 L / min, the temperature is raised at a heating rate of 9°C / min, and the temperature is constant for calcination at a temperature of 750°C for 0.5 hours;

[0032] d. Finally, naturally cool down to room tem...

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Abstract

The invention relates to a preparation method of a phosphate potential boron-doped carbon-wrapped phosphoric acid iron-lithium material. According to the preparation method, phosphoric acid iron, a lithium source, boric acid, oxalic acid and a carbon source which are taken as raw materials are prepared into a carbon-wrapped mixed primary raw material in a liquid phase through water bath stirring, and the carbon-wrapped mixed primary raw material is subjected to rapid high-temperature thermal treatment to generate a carbon-wrapped boron-doped lithium iron phosphate LiFeP1-xBxO4/C (x is greater than or equal to 0.05 and less than or equal to 0.20) anode material. The lithium iron phosphate anode material prepared by using the preparation method has the advantages that crystal grains grow sufficiently, the grain appearance is regular, and excellent electrochemical property is achieved. The preparation method provided by the invention has the advantages of simplicity and easiness in synthesis process, environmental-friendliness, easiness in in-scale production and industrialization.

Description

technical field [0001] The invention belongs to the technical field of preparation of electrochemical power source materials, and has wide application prospects in the fields of commonly used secondary lithium ion batteries and positive electrode materials of power energy batteries. Background technique [0002] With the advent of the era of "low-carbon economy" and the rapid development of communication, transportation and electronic information technology, people have put forward higher requirements for the volume, energy, and cycle life of power supplies. Traditional chemical power supplies such as lead-acid, nickel Cadmium batteries cannot meet the market demand well due to problems such as memory effect, low energy density, and environmental pollution during synthesis and use. Among the currently widely concerned batteries, lithium-ion batteries have become the most popular for adapting to market changes due to their advantages such as small size, light weight, large ca...

Claims

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Application Information

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IPC IPC(8): H01M4/58H01M4/1397
CPCY02E60/10
Inventor 吐尔迪·吾买尔窦俊青张璐陈铭德康雪雅徐金宝韩英徐国庆
Owner XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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