Method and equipment for exfoliating layered materials and separating two-dimensional nanosheets by size screening

A technology of two-dimensional nano and layered materials, which is applied in nanotechnology, nanocarbon, nanotechnology, etc. for materials and surface science. Improved peeling yield and narrow size range

Active Publication Date: 2020-12-29
SHENZHEN GRADUATE SCHOOL TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method also has the problems mentioned above. The size and thickness distribution of the graphene sheet is very wide, and the size is small (less than 600nm), and the thickness is thicker (average 5-8 layers).
Since the device is used in an open environment, it is difficult to ensure that the exfoliated 2D nanosheets will not be oxidized in the air and introduce new defects during the exfoliation process.
More importantly, after the stripping reaches a certain time, the rapid increase of the stripping products makes it difficult for the shear force to act on the raw material, and the stripping is difficult to continue. Even if the stripping time is prolonged, the stripping yield will not be further improved
Therefore, there are still many problems in the mechanical exfoliation of graphene, which makes it difficult to produce on a large scale and needs to be solved urgently.

Method used

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  • Method and equipment for exfoliating layered materials and separating two-dimensional nanosheets by size screening
  • Method and equipment for exfoliating layered materials and separating two-dimensional nanosheets by size screening
  • Method and equipment for exfoliating layered materials and separating two-dimensional nanosheets by size screening

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] A device for exfoliating layered materials and size-screening to separate two-dimensional nanosheets, such as figure 1 As shown, it includes an emulsification disperser 1, a first-stage separator 2 (horizontal centrifuge is selected) and a cascaded separator 3 for size screening connected in series with the first-stage separator 2, and the cascaded separator 3 Including the second-stage separator 31 (selecting a horizontal centrifuge) and the third-stage separator 32 (selecting a horizontal centrifuge) connected in series; the outlet 12 of the emulsifying disperser 1 passes through the first pipeline 01 and the first The feed port 22 of the stage separator 2 is connected; the solid phase discharge port 21 of the first stage separator is connected with the feed port 11 of the emulsification disperser through the second pipeline 02 or with the storage material arranged at the feed port 11 The tank 4 is connected (the discharge port 12 of the present embodiment is connecte...

Embodiment 2

[0054] Turn on the emulsification disperser 1, the first stage separator 2 and the second stage separator 31.

[0055] Mix 325-mesh graphite powder with 1000L N-methylpyrrolidone (NMP) evenly (graphite concentration is 10g / L), add emulsification disperser 1 under nitrogen atmosphere (rotation speed is 6000rpm, stator-rotor gap is 0.24mm) for peeling , the stripped product enters the first stage separator 2 (rotating speed is 500rpm) and carries out solid-liquid phase separation, obtains the precipitate containing the unstripped graphite and the liquid phase part containing graphene, and the precipitate returns to the storage tank In 4, after mixing with the 1000LNMP pre-added in the storage tank 4, enter the emulsification disperser 1 and circulate continuously for 10 times to obtain a large amount of graphene dispersion. The liquid phase part containing graphene enters the second stage separator 31 (rotating speed is 3000rpm), and the second stage separator 31 obtains the ave...

Embodiment 3

[0058] On the basis of Embodiment 2, first close the first output port of the emulsification disperser 1 and the first valve 8 (flowing to the outlet of the first stage separator 2) and the second valve 16, and open the second output of the first valve 8 Port (flowing to the storage tank 4), the stripped mixed solution first enters the emulsification disperser for continuous circulation and stripping for 1h, then closes the second output port of the first valve 8, opens the first output port of the first valve 8, and strips The final product enters the first stage separator 2 for solid-liquid separation. Compared with Example 2, the product concentration obtained in Example 3 is higher. According to different layered materials to be peeled off, its concentration can be increased by about 10 to 50 times, that is, the peeling yield is improved.

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Abstract

The invention discloses a method and equipment for peeling a layered material and screening and separating two-dimensional nanosheets. The layered material is of a lamellar structure, and is peeled toobtain the two-dimensional nanosheets. The method comprises the following steps: S1, mixing a layered material and a solvent; S2, adding the mixed solution into an emulsifying-dispersing machine forpeeling; S3, introducing the peeled mixed solution into a primary separator for separating to obtain a precipitate containing the non-peeled layered material and a liquid phase part containing two-dimensional nanosheets, carrying out a step S4 on the precipitate, and carrying out a step S5 on the liquid phase part; S4, mixing the precipitate and the solvent again for peeling, carrying out the stepS3 again after peeling, and repeatedly peeling the layered material; S5, conveying the liquid phase part into a secondary for screening and separating. By adopting the method and equipment, the layered material with the lamellar structure is peeled continuously and mechanically, and the two-dimensional nanosheets obtained by peeling are screened and separated, so that two-dimensional nanosheets with a narrow and single size range can be obtained.

Description

technical field [0001] The invention relates to the field of preparation of two-dimensional nanosheets, in particular to a method and equipment for peeling off layered materials and screening and separating two-dimensional nanosheets by size. Background technique [0002] Various two-dimensional nanosheets represented by graphene have attracted extensive attention due to their excellent mechanical, optical, electrical, magnetic, and thermal properties. In addition, these two-dimensional nano-graphite sheets, two-dimensional nano-sulfides, two-dimensional nano-hexagonal boron nitride and other two-dimensional nano-sheets have broad application prospects in the fields of lubrication, nano-filling, batteries, and electrocatalysis. As the application scenarios become more and more extensive, the production yield and size requirements of two-dimensional nanosheets are further improved, so a preparation method is urgently needed to match it. Taking graphene as an example, the com...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/19B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01B2204/32C01B32/19
Inventor 杨诚刘康伟梁斌
Owner SHENZHEN GRADUATE SCHOOL TSINGHUA UNIV
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