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Preparation method of functional nano-graphene

A functional nano-graphene technology, applied in the field of functional carbon materials and nano-functional composite materials, can solve problems such as uneven thickness, loss of graphene properties, and difficult size control, achieving good nano-functionality, reliable preparation principles, The effect of structural performance stability

Inactive Publication Date: 2010-02-24
QINGDAO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0003] At present, the preparation methods of functional nanographene sheets are subject to great limitations. One is to use the preparation method of carbon nanotubes and carbon 60 for chemical deposition; the other is to consider natural graphite as raw material for mechanical refinement, resulting in graphene No major breakthrough in the preparation of
The first type of method is mainly: (1) chemical vapor deposition (CVD) method: using microwave enhanced chemical vapor deposition method, SEM shows that the average thickness of nano-graphite sheets grown by this method is only 1nm, and vertical graphite flakes are observed under HRTEM. (2) Orientation epitaxy method: use the atomic structure of the growth substrate to "plant" graphene, but the graphene flakes produced by this method are often uneven in thickness, and graphene and The bonding between the substrates will affect the characteristics of the carbon layer; (3) The method of heating SiC: Graphene is prepared by removing Si by pyrolysis on the Si-terminated (00001) surface of single crystal 6H-SiC, but from this The quantum Hall effect shown by the two-dimensional graphite exfoliated by HOPG was not observed in the two-dimensional graphene prepared by this method, indicating that the structure of the graphene obtained by this method is not ideal.
Therefore, the disadvantages of the chemical method are its structural inaccuracy, small amount, high cost, etc.
The typical method of the second type of method is microphysics or mechanical separation method: the graphene sheet is peeled off from the surface of fresh graphite crystal by mechanical force, such as peeling and observing single-layer graphene from highly oriented pyrolytic graphite (HOPG), this The method is to use the flakes obtained by rubbing the graphite surface to screen out single-layer graphene flakes, whose size is not easy to control, and it is impossible to reliably manufacture graphite flake samples of sufficient length
The ubiquitous shortcoming of these existing methods is: (1) the addition of alkali makes the oxygen atom and group ionization thereof in graphite oxide generate-O - Na + (2) Use long-chain organic (poly) polymers, which have poor permeability; (3) Obtain complexes based on one-time intercalation, and cannot obtain pure graphene, so the availability is poor; ( 4) The generated graphene sheets contain high oxygen content or the recovery degree of graphene hexagonal grid structure is low, which seriously damages the performance of graphene

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] In this embodiment, expandable graphite is used as the starting material, which is pre-oxidized first; concentrated sulfuric acid (concentration 60-98%wt), potassium persulfate, and phosphorus pentoxide are added to a round-bottomed flask, and after heating and dissolving Add natural graphite to react for 4-5 hours; after the reaction is completed, cool to room temperature, dilute with deionized water, and leave overnight; the next day, filter the mixed solution, wash with deionized water, and dry in air to obtain pre-oxidized graphite.

[0015] Preparation of graphite oxide: Put the pre-oxidized natural graphite into concentrated sulfuric acid, then slowly add potassium permanganate to it, stir while adding, keep the system temperature below 10°C (using an ice bath), and then raise the temperature to 35°C for reaction After 2 hours, dilute with deionized water; the addition of water causes the temperature to rise sharply to 98°C, so add it slowly while stirring; then ad...

Embodiment 2

[0024] In this embodiment, graphite oxide is used as the raw material, and the O / C is 0.20 as measured by elemental analysis. The raw material graphite oxide is ultrasonically oscillated in a 10%wt water suspension for 2 hours, washed with water, filtered, then shaken in the water suspension, and washed twice. Second, remove non-carbon impurities; then, take 200mg of the above-mentioned graphite oxide, add it to 250mL water, and add penetrant H at the same time 2 N-NH 2 HCl, strong mechanical stirring for 5 hours to form a dark brown suspension; make 10%wt aqueous solution of 136mg of penetrant and add graphite oxide water suspension; then, raise the temperature to 100°C, reflux for 22 hours and then fully wash with water , the dried graphene contains oxygen O / C≤0.01, and TEM analysis shows that the obtained graphene has a diameter of 1-3 μm and a thickness of 3-5 nm.

[0025] The dosage of penetrant in this embodiment adopts the following calculation method:

[0026] The ma...

Embodiment 3

[0039] With reference to embodiment 1, adopt glucose and H 2 N-NH 2 The aqueous solution is the penetrating agent, the molar ratio of the two: M 葡萄糖 / M H2N-NH2 =0.25, that is, glucose replaces 25% mol of H 2 N-NH 2 ; Adopt the same steps and conditions as in Example 1 to obtain swollen graphite oxide, then raise the temperature to 100 ° C, reflux for 24 hours and fully wash with water and dry; Elemental analysis shows that the oxygen content of the gained graphene is O / C≤0.01 , TEM analysis showed that the obtained graphene had a diameter of 1-2 μm and a thickness of 2-5 nm.

[0040] Unless otherwise specified, the concentrations involved in the present invention and the examples are all percentages by weight.

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Abstract

The invention relates to a preparation method of functional nano-graphene, belonging to the technical field of nano-graphene functional material. The method comprises the following steps: adding graphite oxide in water while adding one or more kinds of penetrants, stirring with ultrasonic wave or a rapid machine to form brown or black uniform suspension, heating to 70-100 DEG C, refluxing, washingwith water and drying to obtain the nano-graphene containing monolayer or multilayer graphene, wherein in the mixing process, graphite oxide absorbs penetrants and performs interlaminar swelling andthe swelled graphite oxide becomes loose and performs dissociation under the ultrasonic oscillation or the mechanical agitation of the rapid machine. The analysis of TEM finds that the nano-graphene has fold property and high radius-thickness ratio, simple technological process, reliable production principle, accessible raw material, low cost, good nanometer functionality, stable structural performance and good application effect.

Description

Technical field: [0001] The invention belongs to the technical field of functional carbon materials and nano-functional composite materials for preparing nano-graphene by utilizing graphite raw materials, and relates to a method for preparing functional nano-graphene by a chemical infiltration method. Background technique: [0002] Graphite is an inorganic substance whose chemical composition is mainly C. It is usually in the form of scales, iron black to copper gray, smooth, easy to bend, inelastic, and can be completely dissociated. It has extensive reserves and production in my country. Natural graphite generally exists in three forms: amorphous, flaky crystals, and highly crystalline. Graphite has a typical layered structure. The crystal belongs to the mixed bond type crystal. It is formed by overlapping layers of hexagonal network structure of carbon atoms, stacked in a direction parallel to the base plane. The bonding force with the carbon atoms between the layers is ...

Claims

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Application Information

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IPC IPC(8): C01B31/04
Inventor 唐建国丛菲刘继宪王瑶黄林军张磊
Owner QINGDAO UNIV
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