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Preparation method of borate ion crosslinked conductive graphene paper

An ion-crosslinking, conductive graphite technology, applied in the field of graphene paper, can solve the problems of toxic chemical reagents, such as electrical conductivity, electrical conductivity not meeting requirements, damage to film structure integrity, etc., achieving easy control, close electrical conductivity, Easy-to-use effects

Active Publication Date: 2015-01-07
SOUTHEAST UNIV
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Problems solved by technology

At present, the preparation methods of macroscopic two-dimensional graphene-based materials mainly include the following types: 1. Chemical vapor deposition method, which is generally prepared by depositing carbon on a copper substrate or dialysis carbon on a nickel substrate under high temperature conditions. One-layer or multi-layer graphene, the product has good crystallization performance and good electrical conductivity, but it requires special equipment, the cost is high, and the practical application is greatly limited
2. Graphene oxide layer-by-layer assembly, this type of method usually uses micro-nano-scale graphene oxide sheets prepared by the improved Hummers method as raw materials, and prepares membranes by evaporation self-assembly, filtration self-assembly, pulling, spin coating, etc. structure, it is generally necessary to use chemical reducing agents (such as hydrazine hydrate, citric acid, vitamins, sodium borohydride, etc.) to reduce graphene oxide to restore the electrical conductivity of graphene materials, the use of toxic chemical reagents or the electrical conductivity can not meet the requirements limit further application
In addition, high-temperature hydrogenation reduction under the protection of inert gas, or direct heating and reduction can restore the electrical conductivity, but high-temperature heating may damage the integrity of the film-like structure
3. Graphene or graphene oxide is assembled after doping and modification. Generally, high temperature and special equipment are required. The conductive properties can be controlled and adjusted, but it is not easy to scale production, so the practical application is also restricted
4. Ionic or molecular cross-linked graphene oxide assembly, by adding a certain amount of metal ions, such as Ca 2+ , Mg 2+ , Fe 3+ , or cross-linked molecules (such as dopamine, ethylenediamine, polyimide, polyvinylpyrrolidone), etc., and then filter and assemble to form a two-dimensional graphene-based material. The mechanical properties of this material have been significantly enhanced, but the electrical conductivity Performance still falls short

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  • Preparation method of borate ion crosslinked conductive graphene paper
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preparation example Construction

[0027] A kind of preparation method of the conductive graphene paper of borate ion crosslinking, comprises the steps:

[0028] Step 1. Using graphite powder less than or equal to 50 μm as the carbon source, the modified Hummers method is used to prepare graphite oxide, and the graphene oxide hydrosol with a concentration of 2-5 mg / mL is obtained by ultrasonic exfoliation in deionized water.

[0029] Step 2. Add sodium hydroxide solution to the graphene oxide hydrosol prepared in step 1 to adjust the pH to 10-12, and then add boric acid according to the mass ratio of boric acid and graphene oxide at 0.1-2:50, and under electromagnetic stirring conditions Heat to 80-90°C, keep warm for 3-5 hours, then cool naturally, filter or centrifuge, wash with deionized water for several times, ultrasonically disperse in deionized water to obtain pure and evenly dispersed borate with a concentration of 1-5 mg / mL Ionically crosslinked reduced graphene oxide hydrosols. Sodium hydroxide can n...

Embodiment 1

[0033] 1. Using graphite powder with a particle size of 30 μm as a carbon source, prepare graphite oxide by the above-mentioned improved Hummers method, and ultrasonically peel off in deionized water to form a uniformly dispersed 3 mg / mL graphene oxide hydrosol, such as figure 1 As shown, the obtained graphene oxide sheet has a high purity, basically a few layers overlapped together, and has an obvious wrinkled structure.

[0034]2. Take 50mL of the 3mg / mL graphene oxide hydrosol prepared above, add an appropriate amount of sodium hydroxide solution to adjust the pH to 11, then add 5mg of boric acid, heat to 90°C under the condition of electromagnetic stirring in a fume hood, and keep it warm for 5h. After natural cooling, centrifugation, deionized water washing 3 times, ultrasonic redispersion in deionized water, to obtain pure and uniformly dispersed 2mg / mL borate ion cross-linked reduced graphene oxide hydrosol, such as figure 2 As shown, it can be seen that the reduced gr...

Embodiment 2

[0039] 1. Using graphite powder with a particle size of 50 μm as a carbon source, prepare graphite oxide by the above-mentioned improved Hummers method, and ultrasonically exfoliate it in deionized water to form a uniformly dispersed 5 mg / mL graphene oxide hydrosol.

[0040] 2. Take 50mL of the 5mg / mL graphene oxide hydrosol prepared above, add an appropriate amount of sodium hydroxide solution to adjust the pH to 12, then add 10mg of boric acid, heat to 90°C under the condition of electromagnetic stirring in a fume hood, and keep it warm for 5h. After natural cooling, centrifugation, deionized water washing 3 times, ultrasonic redispersion in deionized water, to obtain pure and uniformly dispersed 5 mg / mL borate ion cross-linked reduced graphene oxide hydrosol.

[0041] 3. Take 50 mL of the borate ion-crosslinked reduced graphene oxide hydrosol prepared above, and filter layer-by-layer self-assembly through a mixed cellulose ester microporous filter membrane with a diameter of...

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Abstract

The invention discloses a preparation method of borate ion crosslinked conductive graphene paper. The preparation method comprises the following steps: preparing graphite oxide by adopting an improved Hummers method and ultrasonically stripping in deionized water to obtain graphite oxide hydrosol; then, adding a sodium hydroxide solution into the graphite oxide hydrosol to adjust the pH to 10-12; then adding boric acid; heating to 80-90 DEG C under a stirring condition; insulating heat for 3-5 hours; then naturally cooling; separating; washing; ultrasonically dispersing in deionized water; and finally filtering by a millipore filter and self-assembling layer by layer to obtain the borate ion crosslinked conductive graphene paper. The preparation method disclosed by the invention is simple, convenient to operate and low in cost, does not need special equipment and is easy for batch production. The obtained graphene paper has an excellent conductive performance and possibly can be used as an ideal conductive material for optoelectronic devices.

Description

technical field [0001] The invention relates to the technical field of graphene paper, in particular to a method for preparing conductive graphene paper cross-linked by borate ions. Background technique [0002] Graphene oxide is a derivative of graphene with a thickness of one atomic layer. It is usually used as a precursor for the preparation of graphene. Recently, it has become one of the research hotspots due to its unique properties. Graphene oxide has the characteristics of low production cost, easy large-scale production, easily soluble in polar solvents such as water, and excellent processing performance; it also has good mechanical and chemical properties. There are a large number of covalently bonded oxygen-containing functional groups in the plane and on the boundary of graphene oxide, with sp 2 and sp 3 The structure of hybridized carbon atoms can be controlled by controlling its size, shape and sp 2 The relative proportion of the hybrid region further modulat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 徐春祥田正山理记涛朱刚毅吴靖石增良
Owner SOUTHEAST UNIV
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