Preparation method of lithium iron phosphate/carbon nanotube composite cathode material

A carbon nanotube composite and positive electrode material technology, which is applied in the direction of positive electrodes, battery electrodes, active material electrodes, etc., can solve problems such as difficult to remove, difficult to prepare composite materials, and poor dispersion of carbon nanotubes

Active Publication Date: 2021-07-16
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, carbon nanotubes have poor dispersion due to their own characteristics, and it is difficult to prepare uniform composite materials.
In the content disclosed in CN102427130A and CN101533904A, although the composite material of carbon nanotubes and lithium iron phosphate is generated in situ by chemical vapor deposition, an additional catalyst is added in the process of preparing the material, and it is difficult to remove

Method used

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  • Preparation method of lithium iron phosphate/carbon nanotube composite cathode material

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Embodiment 1

[0024] like figure 1 Shown, the embodiment of the present invention provides a kind of preparation method of lithium iron phosphate / carbon nanotube composite cathode material, comprises the following steps:

[0025] Step 1: take 50g median particle diameter and be the iron-based catalyst (iron content is 98wt%) of 0.82um, iron-based catalyst is put into the tubular electric resistance furnace, assemble experimental device and check the airtightness of device; Nitrogen is used to remove the air in the device, the nitrogen flow rate is 300 sccm, and the temperature of the tubular resistance furnace is raised to 750° C. at 15° C. / min. When the temperature in the furnace reached the set temperature, the nitrogen gas was turned off, and methane was fed in at the same time, and the gas flow rate was 100 sccm. After feeding ethylene for 25 minutes, stop feeding carbon source gas, start feeding nitrogen gas, keep warm for 30 min, cool down to room temperature naturally, and take out ...

Embodiment 2

[0031]Step 1: Weigh 50g of catalyst with a median particle size of 0.82um (98wt% iron content), put the catalyst into a tubular resistance furnace, assemble the experimental device and check the airtightness of the device. Nitrogen gas was introduced to remove the air in the device, the flow rate of nitrogen gas was 300 sccm, and the temperature of the tubular resistance furnace was raised to 750 °C at 15 °C / min. When the temperature in the furnace reached the set temperature, the nitrogen gas was turned off, and methane was fed in at the same time, and the gas flow rate was 100 sccm. After feeding ethylene for 25 minutes, stop feeding carbon source gas, start feeding nitrogen gas, keep warm for 30 min, cool down to room temperature naturally, take out the iron powder / carbon nanotube composite material; perform inductively coupled plasma spectroscopy (ICP-OES) on the material Test, it is found that the content of iron in the composite material is 88.78wt%;

[0032] Step 2: We...

Embodiment 3

[0037] Step 1: Weigh 50g of a catalyst with a median particle size of 2.54um (the iron content is 95wt%), put the catalyst into a tubular resistance furnace, assemble the experimental device and check the airtightness of the device. Argon gas was introduced to remove the air in the device, the flow rate of argon gas was 500 sccm, and the temperature of the tube resistance furnace was raised to 800 °C at 15 °C / min. When the temperature in the furnace reaches the set temperature, the argon gas is turned off, and acetylene is introduced at the same time, and the gas flow rate is 30 sccm. After feeding ethylene for 15 minutes, stop feeding carbon source gas, start feeding argon gas, keep warm for 20 min, cool down to room temperature naturally, and take out the iron powder / carbon nanotube composite material. The material was tested by inductively coupled plasma spectroscopy (ICP-OES), and the content of iron in the composite material was measured to be 84.37wt%;

[0038] Step 2: ...

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Abstract

The invention provides a preparation method of lithium iron phosphate / carbon nanotube composite positive electrode material, comprising: (1) preparing iron-based catalyst / carbon nanotube composite material by chemical vapor deposition; (2) mixing catalyst / carbon nanotube composite Materials and acidic solution, add a certain amount of phosphorus source, iron source and hydrogen peroxide to obtain a mixed solution, after stirring for a certain period of time, adjust the pH value with an alkaline solution to obtain a precipitate, after repeated filtration, washing, and drying to obtain a precursor / carbon nanotube composite material; (3) mixing the precursor / carbon nanotube composite material and lithium source according to a certain ratio; (4) sintering the mixed material at high temperature to obtain lithium iron phosphate / carbon nanotube composite positive electrode material. The carbon nanotubes in the lithium iron phosphate / carbon nanotube composite cathode material prepared by the invention form a good conductive network, which solves the problem of poor conductivity of the lithium iron phosphate cathode material and improves the electrochemical performance of the material.

Description

technical field [0001] The invention relates to the technical field of lithium ion battery materials, in particular to a preparation method of a lithium iron phosphate / carbon nanotube composite cathode material. Background technique [0002] Since the commercialization of lithium-ion batteries, due to their advantages such as high energy density, high working voltage, long cycle life and environmental friendliness, they have become the most concerned secondary batteries at present. Lithium-ion batteries are widely used in portable electronic products, power batteries and large-scale energy storage and other fields. With the continuous improvement of performance requirements for lithium-ion batteries in various fields, research on lithium-ion batteries has become more and more in-depth. Lithium-ion batteries are mainly composed of positive electrodes, negative electrodes, diaphragms, electrolytes, casings, etc. Among them, the positive electrode materials have the most signif...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/62H01M4/58H01M10/0525
CPCH01M4/5825H01M4/625H01M10/0525H01M2004/028Y02E60/10
Inventor 颜果春王接喜李新海席昭王志兴郭华军胡启阳彭文杰
Owner CENT SOUTH UNIV
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