Method for preparing outer wall-fluorinated multi-walled carbon nanotube containing iron fluoride intercalated substance

A multi-walled carbon nanotube and fluorination technology, applied in electrical components, battery electrodes, non-aqueous electrolyte batteries, etc., can solve the problems of volume expansion and low electronic conductivity, and achieve the effect of increasing output voltage and theoretical specific capacity

Active Publication Date: 2018-01-26
LIAONING LANJING TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Iron fluoride is intercalated in the conductive graphite wall of the inner layer of multi-walled carbon nanotubes to solve the problem of low electronic conductivity and volume expansion caused by polarization during charge and discharge

Method used

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  • Method for preparing outer wall-fluorinated multi-walled carbon nanotube containing iron fluoride intercalated substance
  • Method for preparing outer wall-fluorinated multi-walled carbon nanotube containing iron fluoride intercalated substance

Examples

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Embodiment 1

[0034] In this embodiment, the preparation method of the outer wall fluorinated multi-walled carbon nanotubes containing iron fluoride intercalation comprises the following steps:

[0035] 1. Mix the dry multi-walled carbon nanotubes with KOH evenly, and react in a tube furnace at 700°C for 4 hours under a nitrogen atmosphere, then cool to room temperature, wash with water, and then dry. After drying, it is mixed with concentrated nitric acid (concentration: 68wt%) of 40 times the mass ratio, refluxed at 80° C. for 2 hours, and then washed with water until neutrally dried.

[0036] 2. Place the high-purity multi-walled carbon nanotubes with the end caps opened in a dry, vacuumable heating reactor, and feed ferric chloride vapor with a mass ratio of 2:1 to the multi-walled carbon nanotubes at 330°C React for 6 hours, so that ferric chloride intercalates into the multi-walled carbon nanotubes. After the reaction, the temperature is lowered to 310° C., and the process pressure is...

Embodiment 2

[0042] In this embodiment, the preparation method of the outer wall fluorinated multi-walled carbon nanotubes containing iron fluoride intercalation comprises the following steps:

[0043] 1. Mix the dried multi-walled carbon nanotubes with NaOH evenly, react in a tube furnace at 750°C for 4 hours under a nitrogen atmosphere, then cool to room temperature, wash with water and then dry. After drying, mix with 30 times mass ratio fuming concentrated nitric acid (concentration 85wt%), reflux at 90°C for 2 hours, then wash with water until neutral drying.

[0044] 2. Place the high-purity multi-walled carbon nanotubes with the end caps opened in a dry, vacuumable heating reactor, and feed ferric chloride vapor with a mass ratio of 2:1 to the multi-walled carbon nanotubes at 320°C React for 6 hours, so that ferric chloride intercalates into the multi-walled carbon nanotubes. After the reaction, the temperature is lowered to 310° C., and the process pressure is maintained at 0.3 MPa...

Embodiment 3

[0049] In this embodiment, the preparation method of the outer wall fluorinated multi-walled carbon nanotubes containing iron fluoride intercalation comprises the following steps:

[0050] 1. Mix the dry multi-walled carbon nanotubes with KOH evenly, react in a tube furnace at 730°C for 5 hours under a nitrogen atmosphere, then cool to room temperature, wash with water and then dry. After drying, it is mixed with concentrated hydrochloric acid (concentration 35wt%) of 80 times the mass ratio, refluxed at 80° C. for 3 hours, and then washed with water until neutrally dried.

[0051] 2. Place the high-purity multi-walled carbon nanotubes with the end caps opened in a dry, vacuumable heating reactor, and feed ferric chloride vapor with a mass ratio of 2:1 to the multi-walled carbon nanotubes at 315°C React for 6 hours, so that ferric chloride intercalates into the multi-walled carbon nanotubes. After the reaction, the temperature is lowered to 310° C., and the process pressure is...

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Abstract

The invention belongs to the field of preparation of functional materials, and especially relates to a method for preparing an outer wall-fluorinated multi-walled carbon nanotube containing an iron fluoride intercalated substance. The problems of too low electric conductivity and volume expansion of multi-walled carbon nanotubes with the polarization in the charge and discharge process are solved.The end caps of a multi-walled carbon nanotube are opened, the multi-walled carbon nanotube is purified, iron fluoride is used to carry out intercalation in a heating reactor which can be vacuumized,hydrogen fluoride is sued to convert the iron chloride into iron fluoride, and fluorine gas is used to properly fluorinate the multi-walled carbon nanotube in order to finally form a compounded multi-walled carbon nanotube with the outer wall being fluorinated to a certain degree, the interlayer being iron fluoride and the inner layer having a certain electric conductivity. The method enables theabove material to provide a high output voltage and a theoretical specific capacity through the outer wall fluorination and the iron fluoride interlayer, and keeps the electric conductive of the inner wall of the material as possible, so the material is suitable for being used as a novel lithium battery positive electrode material.

Description

technical field [0001] The invention belongs to the field of preparation of functional materials, and in particular relates to a method for preparing outer-wall fluorinated multi-wall carbon nanotubes containing iron fluoride intercalation substances. Background technique [0002] Reaction of carbon materials with fluorine gas source substances at high temperature will produce a new compound - fluorinated carbon materials. This is a carbon material interlayer compound formed by the combination of carbon and fluorine. The interlayer compound is a fluorine atom, which is divided into a covalent bond type interlayer compound and a semi-ionic type interlayer compound. Fluorinated carbon materials have properties such as extremely low surface energy, high electrical activity, and relatively low sectional area for absorbing thermal neutrons, so fluorinated carbons can be widely used in lubrication, degreasing, antifouling, batteries, nuclear reactions, etc. [0003] When used as ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/583H01M10/052
CPCY02E60/10
Inventor 张柏华
Owner LIAONING LANJING TECH CO LTD
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