Method adopting a liquid phase stripping method to prepare grapheme and grapheme

A technology of liquid phase exfoliation and graphene, which is applied in the field of multi-layer graphene preparation, can solve the problems of complicated preparation process, decreased electrical conductivity of graphene, time-consuming, etc., and achieve the effect of good electrical conductivity and small structural defects

Inactive Publication Date: 2015-12-02
朱振业
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the yield of graphene prepared by this method is high (50%), the use of a large amount of strong acid and oxidant makes the preparation process complicated and time-consuming, and the presence of residual oxygen functional groups reduces the conductivity of graphene.

Method used

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  • Method adopting a liquid phase stripping method to prepare grapheme and grapheme

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preparation example Construction

[0020] Such as figure 1 as shown, figure 1 A schematic process flow diagram of multilayer graphene prepared according to the preparation method of the present invention is shown. Specifically, the preparation method of the multilayer graphene includes: Step 1, preparing a certain concentration of sodium dodecylbenzenesulfonate ethanol solution; Step 2, sieving expanded graphite; Step 3, stirring the sieved The expanded graphite is dissolved in the solution prepared in step one; step four, the expanded graphite prepared in step three is treated with microwave for 5 minutes (min); step five, the solution after microwave treatment is ultrasonically stripped under ice bath conditions; step six 1. Resting the ultrasonically treated solution for 24 hours (h), and obtaining a graphene sample after centrifugation and dialysis.

[0021] In step five, a large amount of heat is released during the ultrasonic process, so that the temperature of the expanded graphite is higher, and the e...

Embodiment 1

[0025] Such as figure 2 Shown, surfactant uses sodium dodecylbenzene sulfonate (SDBS), and ultrasonic solvent selects ethanol and adopts magnetic stirring to completely dissolve the surfactant of certain quality in the solvent of certain volume (surfactant concentration is 0mg / mL, 4mg / mL, 6mg / mL), add expanded graphite passing through a 0.5mm pore size sieve, continue magnetic stirring and mixing, after fully mixing, microwave the mixed solution dispersed with expanded graphite for 5min, and then ultrasonicate the mixed solution for a period of time , to obtain a graphene dispersion. In order to separate the unexfoliated graphite and graphene, the obtained solution is centrifuged after standing still for a period of time, and the agglomerated graphene can be separated from the unaggregated graphene at the same time after centrifugation, and then the supernatant of the dispersion liquid is taken into a dialysis bag soaked in an aqueous solution for dialysis for a period of t...

Embodiment 2

[0027] Embodiment 2 first compared the influence of the ultrasonic stripping time on the preparation of graphene under the same surfactant concentration condition respectively, and obtained a better graphene preparation condition as when the surfactant concentration was 0mg / ml, and the ultrasonic stripping time was 15h, When the surfactant concentration is 4mg / ml, the ultrasonic stripping time is 10h, when the surfactant concentration is 6mg / ml, the ultrasonic stripping time is 10h, and then it is characterized by SEM, Raman and FTIR to compare the graphene prepared under three better conditions , and finally concluded that the best condition for preparing graphene is that the concentration of surfactant is 6mg / ml, and the ultrasonic stripping time is 10h.

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Abstract

The invention provides a method adopting a liquid phase stripping method to prepare grapheme, which comprises steps: 1 sodium dodecyl benzene sulfonic acid ethanol solution in a certain concentration is prepared; 2 expanded graphite is screened; 3 the expanded graphite after being screened are dissolved into the sodium dodecyl benzene sulfonic acid ethanol solution which is prepared in the step 1 by being stirred through magnetic force; 4 the expanded graphite which is prepared in the step 3 is treated for 5mins through microwaves; 5 the sodium dodecyl benzene sulfonic acid ethanol solution which is treated through the microwaves is peeled through ultrasound in ice bath conditions; and 6 the sodium dodecyl benzene sulfonic acid ethanol solution which is treated through the ultrasound is statically placed for 24h, thereby obtaining graphene samples after centrifugal and dialysis treatment. The grapheme is extremely thin in layers through pattern analysis and structural analysis, smaller than 10 in layer number, small in structural defect and excellent in conductivity.

Description

technical field [0001] The invention relates to a preparation method of multilayer graphene, in particular to a preparation method of graphene applied to lithium-ion battery negative electrode materials. Background technique [0002] Graphene is a plane composed of two-dimensional carbon atoms with an approximate hexagonal lattice structure, a zero-band gap semiconductor with a small overlap between the valence band and the conduction band, and has a high charge carrier mobility at room temperature (10000cm 2 V -1 the s -1 ), super good thermal stability and thermal conductivity (3000-5000Wm -1 K -1 ), super high Young's modulus (1TPa), super large theoretical specific surface area (2630m 2 g -1 ). After stacking, graphene can form our common three-dimensional structure of graphite, and after bending, it can form carbon nanotubes with one-dimensional structure, and can also be wrapped into zero-dimensional fullerene. In graphene sheets (GNSS), the phase The connection...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 朱振业
Owner 朱振业
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