Method for preparing graphene film through reduction of ferrous iodide acid solution

A technology of graphene film and acidic solution, which is applied in the preparation of low-temperature catalytic reduction of graphene nanomaterials and the reduction of ferrous iodide acidic solution to prepare graphene film, which can solve the problems of incomplete reduction, environmental pollution, and harsh conditions. Achieve mild and controllable reduction reaction, broaden the application range, and achieve the effect of mild and controllable reaction

Active Publication Date: 2014-04-30
SICHUAN INST OF MATERIALS & TECH
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AI Technical Summary

Problems solved by technology

Various methods have their advantages and disadvantages: the mechanical exfoliation method is not suitable for large-scale industrial preparation of graphene due to the limitations of the exfoliation method; the chemical vapor deposition method and the epitaxial growth method have complex processes, harsh conditions, low yield, Disadvantages such as high cost limit its large-scale industrial production and application of graphene
While the existing reducing agent NaBH 4 , various alkoxides and N 2 h 4 And its derivatives still have problems such as incomplete reduction of oxidation functional groups and low conductivity of products. The problem of incomplete reduction in the aforementioned methods affects the application of graphene.
In addition, the organic reducing agent hydrazine and its derivatives are highly toxic and may cause environmental pollution
However, NaH and high-concentration HI are used as reducing agents, although the reducing effect is better, but the reactivity is too high, resulting in too severe reduction reaction and difficult to control.

Method used

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  • Method for preparing graphene film through reduction of ferrous iodide acid solution
  • Method for preparing graphene film through reduction of ferrous iodide acid solution
  • Method for preparing graphene film through reduction of ferrous iodide acid solution

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preparation example Construction

[0032] The preparation method of graphene oxide used in the example is as follows: mix 3g graphite powder, 3g sodium nitrate and 138ml concentrated sulfuric acid ice bath; then slowly add 18g potassium permanganate, after magnetic stirring and mixing, heat in 35 ℃ water bath 1h; then add 240ml deionized water and heat at 90°C for 0.5h, add 600ml deionized water and 18ml hydrogen peroxide after heating.

[0033] The graphene oxide obtained after oxidation is ultrasonically dispersed, then diluted according to a certain ratio, and finally the diluted solution is centrifuged, and the upper suspension is taken, and a graphene oxide film with a certain thickness is prepared by suction filtration. Then measure the film thickness of the graphene film with a step meter, and measure its electrical conductivity with a four-probe method.

Embodiment 1

[0035] After centrifugation, 40ml of graphene oxide (GO) supernatant suspension (GO concentration 0.2mg / ml, solvent is ethanol) was suction-filtered to form a film, and dried for later use. Among them, GO refers to the single-layer graphene oxide obtained by Hamel oxidation.

[0036] Grind 5.08g of iodine particles, then add 4g of iron powder, and mix well to obtain a mixture. Put the mixture into a large beaker, drop 0.1ml of deionized water as a catalyst for the reaction; the reaction unfolds rapidly, at the same time, add 90ml of deionized water, stir quickly with magnetic force to make it fully react, and add 9ml of 12mol / L concentrated hydrochloric acid at the same time (pH value is about 0.1), obtains the ferrous iodide acidic solution of concentration about 0.2mol / L (iron powder is excessive, suppresses Lewis acid hydrolysis).

[0037] Then put the dried graphene oxide (GO) film (thickness is about 2 μm) into ferrous iodide acidic solution, heat to 100 °C, and reduce for...

Embodiment 2

[0045] Mix 1.27g of ground iodine particles and 1g of iron powder evenly, put them into a large beaker, drop in 0.1ml of deionized water as a catalyst for the reaction; the reaction develops rapidly, and add 90ml of N,N-dimethylformamide at the same time (DMF), fast magnetic stirring, make it react fully, add the concentrated hydrochloric acid 9ml (pH value is about 0.1) of 12mol / L simultaneously, make ferrous iodide acidic solution (concentration of ferrous iodide is 0.05mol / L, where excess iron). Then the dried graphene oxide (GO) film was put into ferrous iodide acidic solution and reduced at 140 °C for 1 h under magnetic stirring.

[0046] The test result is: the conductivity of the graphene film is 18351S / m.

[0047] With above-mentioned ferrous iodide acidic solution as reductant, change reductant solvent type, reduction temperature and pH value and the kind of inorganic acid respectively, under the premise that other conditions are constant, the electrical conductivity...

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Abstract

The invention discloses a method for preparing a graphene film through reduction of a ferrous iodide acid solution, belonging to the technical field of chemical synthesis of graphene. A graphene oxide prepared through chemical oxidation is taken as a raw material, and the method comprises a reduction reaction step of reducing the graphene oxide into graphene, wherein the ferrous iodide solution is taken as a reducing agent in the reduction reaction step, rapid reduction of the graphene oxide is realized by controlling the solution concentration, reduction time, reduction temperature, types and pH values of solvents and types of inorganic acids used for pH regulation, oxygen-containing functional groups such as epoxy group, hydroxyl, carboxyl and carbonyl on the graphene oxide are removed, the conductivity of the graphene is completely restored, and the graphene film is prepared. The method is a method for preparing graphene through a low-temperature chemical method suitable for large-scale industrial production. The method has the advantages of low reduction temperature, mild and controllable reactions, complete reduction, environment friendliness and suitableness for industrial production.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis of graphene, and in particular relates to a method for preparing a graphene film by reduction of ferrous iodide acidic solution, specifically a method for preparing a graphene nanomaterial with a single carbon atom thickness by low-temperature catalytic reduction. The graphene film prepared by this method can be widely used in the fields of microelectronic devices, sensors and new energy materials. Background technique [0002] Graphene is a flake graphite material with a thickness of one carbon atom discovered by British scientists in 2004. Due to the long-range π-conjugated bonds of graphene, it has excellent properties in electricity, mechanics, and heat. It will be a new material with a wide range of uses, and it is a current research hotspot. [0003] At present, the preparation methods of graphene mainly include mechanical exfoliation method, chemical vapor deposition method, epi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/184
Inventor 赵晓冲杨盼
Owner SICHUAN INST OF MATERIALS & TECH
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