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Heteroatom doped surface hollow spherical graphene material with holes and its preparation method and application

A technology of heteroatoms and graphene, which is applied in large-capacity, heteroatom-doped surface hollow spherical graphene materials and its preparation, high-rate lithium-ion batteries, and can solve the application of heteroatom-doped graphene Restrictions, difficult to use the surface of the sheet, hindering the rapid transfer of ions, etc., to achieve the effect of more reversible active sites for lithium storage, low cost, and easy operation

Active Publication Date: 2017-04-19
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] (1) Due to the existence of van der Waals force between sheets, graphene nanosheets (GNS) will gradually gather into a graphene paper-like structure during the preparation and cycle charge-discharge process, making it difficult to use a large number of sheet surfaces. Its specific surface is much lower than the theoretical specific surface;
[0008] (2) The aggregation of the sheets leads to the continuous reduction of the active surface of the material, and at the same time produces many discontinuous channels, which hinder the rapid transfer of ions in it;
[0009] (3) The graphene sheet with a complete surface, due to its dense surface, the ion transport through the graphene sheet is easily hindered; because although the conductivity of ions in the direction parallel to the graphene surface is very high, its conductivity in the direction perpendicular to the graphene Conductivity efficiency in sheet plane direction is low
[0010] Due to the above-mentioned defects in the heteroatom-doped graphene prepared by the prior art, the application of heteroatom-doped graphene is greatly limited.

Method used

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  • Heteroatom doped surface hollow spherical graphene material with holes and its preparation method and application
  • Heteroatom doped surface hollow spherical graphene material with holes and its preparation method and application
  • Heteroatom doped surface hollow spherical graphene material with holes and its preparation method and application

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Embodiment 1

[0058] A method for preparing a heteroatom-doped surface hollow spherical graphene material with holes, specifically comprising the following steps:

[0059] (1) Synthesis of graphene oxide

[0060] (1-1) Assemble the reaction flask in an ice-water bath, add a solid mixture of 1g of expanded graphite powder and 2.5g of sodium nitrate to the reaction flask under stirring (the stirring speed is 500r / min), and then add 150mL of mass percentage 95% concentrated sulfuric acid, reacted in an ice-water bath for 30 minutes; then, added 15 g of potassium permanganate 60 times (1 min each time), controlled the reaction temperature at 0 ° C, and continued to react for 12 h; then added 150 mL of deionized water to dilute After stirring and reacting for 30 minutes (the rotating speed of stirring is 500r / min), the temperature was raised to 98° C. at a heating rate of 10° C. / min, and the heat preservation reaction was carried out for 48 hours. The color of the solution changed from black to br...

Embodiment 2

[0079] A method for preparing a heteroatom-doped surface hollow spherical graphene material with holes, specifically comprising the following steps:

[0080] (1) synthesis of graphene oxide: same as step (1) in embodiment 1;

[0081] (2) synthesis of graphene oxide with holes on the surface: same as step (2) in Example 1;

[0082] (3) Preparation of positively charged silica sphere template: same as step (3) in Example 1;

[0083](4) Porous graphene oxide@silica sphere composite with core-shell structure: same as step (4) in Example 1;

[0084] (5) Place 300 mg of graphene oxide@silica sphere composite with pores on the surface at the center of the plasma high-temperature tubular reactor, use a mechanical pump to vacuumize to remove impurities and water vapor, and reduce the pressure to 5Pa, and then use it further The molecular pump vacuumizes to 1×10 -3 Pa, then pass protective gas N at one end 2 and gaseous heteroatom doping source diborane to a pressure of 10Pa (N 2 T...

Embodiment 3

[0087] A method for preparing a heteroatom-doped surface hollow spherical graphene material with holes, specifically comprising the following steps:

[0088] (1) synthesis of graphene oxide: same as step (1) in embodiment 1;

[0089] (2) synthesis of graphene oxide with holes on the surface: same as step (2) in Example 1;

[0090] (3) Preparation of positively charged silica sphere template: same as step (3) in Example 1;

[0091] (4) Graphene oxide@silica sphere composite with holes on the surface having a core-shell structure: same as step (4) in Example 1;

[0092] (5) Place 300 mg of the surface-porous graphene oxide@silica sphere composite prepared above at the center of the plasma high-temperature tubular reactor, use a mechanical pump to vacuumize to remove impurities and water vapor, and reduce the pressure to 5Pa, Then further use the molecular pump to evacuate to 1×10 -3 Pa, then pass protective gas N at one end 2 and gaseous heteroatom doping source phosphorus t...

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Abstract

Belonging to the field of carbon materials and electrochemistry, the invention discloses a heteroatom doped surface perforated hollow sphere graphene material, a preparation method and application thereof. The method includes: firstly carrying out ultrasonic reaction on concentrated nitric acid and graphene oxide, and performing standing to obtain surface perforated graphene oxide; then adding hexadecyl trimethyl ammonium bromide into a mixed solution of deionized water, ethylene glycol and ammonia water, carrying out dissolving, heating and stirring, then adding tetraethoxysilane and 3-aminopropyltriethoxysilane in order, carrying out stirring reaction, standing and hydrothermal reaction, thus obtaining positively charged silica spheres; carrying out stirring reaction on a surface perforated graphene oxide aqueous dispersion and a pH adjusted silica sphere aqueous dispersion, and performing freeze drying to obtain a composite material; and finally placing the composite material in a plasma high temperature tubular reactor to carry out reaction, thus obtaining the heteroatom doped surface perforated hollow sphere graphene material. The prepared material has a unique hollow structure, and can improve the electrical conductivity and thermal stability of electrode materials.

Description

technical field [0001] The invention belongs to the field of carbon materials and electrochemistry, and in particular relates to a heteroatom-doped surface hollow spherical graphene material with holes, a preparation method thereof, and an application in a large-capacity, high-rate lithium-ion battery. Background technique [0002] Lithium-ion battery, due to its high open circuit voltage, high energy density, long service life, no memory effect, no pollution and small self-discharge, is the focus of the development of secondary batteries at present, and is used as an important power supply in mobile communications, notebooks, etc. Computers and other electrical appliances occupy a relatively large share, and are expected to be used in electric vehicles and large storage devices in the national grid. At present, if lithium-ion batteries are to be applied to large-scale energy storage devices and high-power devices, it is necessary to maintain good capacity characteristics an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/184C01B33/12H01M4/36H01M4/587H01M10/0525B82Y30/00
CPCY02E60/10
Inventor 蒋仲杰
Owner SOUTH CHINA UNIV OF TECH
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