CN109052376A - A kind of preparation method of high fold grapheme material - Google Patents
A kind of preparation method of high fold grapheme material Download PDFInfo
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- CN109052376A CN109052376A CN201811194670.6A CN201811194670A CN109052376A CN 109052376 A CN109052376 A CN 109052376A CN 201811194670 A CN201811194670 A CN 201811194670A CN 109052376 A CN109052376 A CN 109052376A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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Abstract
The present invention provides a kind of preparation method of high fold grapheme material.Graphene oxide and high alumina particles filter into laminated film after mixing, and naturally dry after impregnating in enough dilute hydrochloric acid solutions heats to remove residual solvent, restored to obtain the graphene film of independent self-supporting with hydroiodic acid.Alumina particles, which are present in graphene oxide interlayer, in the method for the invention causes lamella to be more likely formed fold, alumina particles, which react the hydrogen generated with hydrochloric acid and spontaneously dry, can also manufacture a large amount of folds with the ethyl alcohol to volatilize in heating process, high fold graphene film can efficiently be prepared, it consumes energy low, easy to control, synthesis step is simple, and the requirement to equipment is lower, suitable for industry or laboratory operation, an approach is provided for high fold graphene film material scale of mass production.
Description
Technical field
The present invention relates to graphene film preparation field more particularly to a kind of utilization high fold graphenes of high alumina particle preparation
The method of film.
Background technique
Graphene has excellent optics, electricity, mechanical characteristic, and specific surface area is high, and high temperature resistant is corrosion-resistant, materialogy,
Sea water desalination, micro-nano technology, the energy, biomedicine and drug delivery etc. are with important application prospects, it is considered to be one
The following revolutionary material of kind.One main application form of graphene is by microcosmic graphene oxide or graphene film
It is assembled into the graphene film of macroscopic view, for diversified necks such as electrically conducting transparent touch screen, filter membrane, coating, electrode materials
Domain.
High fold graphene has unique pleated structure, has excellent tensile property, can provide higher specific surface
It is long-pending and mesoporous, in conjunction with graphene own advantages, the material is made to be expected to become flexible device, filter membrane, high-performance super capacitor
With the electrode material of lithium ion battery, all had in FPD, anticorrosion, thermo electric material, energy storage field, Industrial Catalysis field
Preferable application prospect.But the preparation method of existing high fold graphene mainly passes through chemical vapor deposition or dry
Wet process transfer, complex process, energy consumption are high, and equipment requirement is high, and fold graphene technical report is seldom, needs to develop one kind
Effective high fold graphene large-scale preparation method.
Summary of the invention
Propose a kind of preparation method of high fold grapheme material.Nano aluminum due to activity it is too high, be not easy to save with
Using the present invention chooses the biggish high alumina particles of partial size, and high alumina grain diameter is in apparent tri-modal distribution, and coarse granule peak value is 80
μm or so, for fine grained peak value at 0.7 μm or so, middle crest is located at 10 μm or so.Peak value is the high alumina of 0.7 μm with 10 μm of partial sizes
Grain can be used to be combined into independent self-supporting film with graphene oxide, and alumina particles cause fold in graphene oxide interlayer and hinder
The only overlapping of graphene oxide film interlayer, and more folds are further formed with the generated reactive gas of hydrochloric acid, when drying, are more
Remaining hydrochloric acid volatilization can also form pleated structure.It is thin that graphene oxide film forms high fold graphene after hydroiodic acid restores
Film.
The present invention adopts the following technical scheme:
A kind of preparation method of high fold grapheme material, includes the following steps:
(1) that graphene oxide and high alumina particles are added to ultrasonic mixing in ethanol solution is uniform, filters into laminated film,
Laminated film is added in enough dilute hydrochloric acid solutions and is impregnated, after reaction by film naturally dry；
(2) heated oxide graphene film obtains independent self-supporting using hydroiodic acid solution reduction to remove residual solvent
Graphene film.
The partial size of high alumina particles in step (1) is 0.7 μm or 10 μm.
Graphene oxide and high alumina granular mass ratio in step (1) are 0.1~10, preferably 2.
Ultrasonic time in step (1) is 0.5~6 hour, preferably 1h.
Dilute hydrochloric acid solution mass fraction in step (1) is 10%, hydrochloric acid total amount should be more than for high alumina particle reaction
Amount used.
Heating temperature in step (2) is 60~100 DEG C, and the time is 2~10h.
The present invention has the advantage that
(1) alumina particles are present in graphene oxide interlayer lamella are caused to be more likely formed fold, aluminium in the method for the invention
Particle, which reacts the hydrogen generated with hydrochloric acid and spontaneously dries, can also manufacture a large amount of folds with the ethyl alcohol to volatilize in heating process,
High fold graphene film can efficiently be prepared.
(2) aluminium element used used in the method for the invention is the most abundant metallic element of content in the earth's crust.
(3) the method for the invention energy consumption is low, and easy to control, synthesis step is simple, and the requirement to equipment is lower, is suitable for industry
Or laboratory operation, an approach is provided for high fold graphene film material scale of mass production.
Detailed description of the invention
Fig. 1 is the SEM figure on graphene film surface prepared by the method for the present invention comparative example 1.
Fig. 2 is the SEM figure on high fold graphene film surface prepared by embodiment of the present invention method 1.
Specific embodiment
Of the invention for ease of understanding, it is as follows that the present invention enumerates embodiment.Those skilled in the art are it will be clearly understood that the implementation
Example is used only for helping to understand the present invention, should not be regarded as a specific limitation of the invention.
Embodiment 1
(1) the high alumina particles that 2g graphene oxide and 1g partial size peak value are 0.7 μm are added to ultrasound 1h in ethanol solution.
(2) solution is filtered with vacuum filtration method prepare laminated film.
(3) laminated film is added in the dilute hydrochloric acid solution that enough mass fractions are 10% and impregnates 2h, reaction terminates
Afterwards by film naturally dry.
(4) independent self-supporting film is heated at a temperature of 70 DEG C, continues 4h.
(5) independent self-supporting film is put into reduction in hydroiodic acid solution and obtains the graphene film of independent self-supporting.
Fig. 2 is the SEM figure that the present embodiment prepares high fold graphene film surface.
Embodiment 2
(1) the high alumina particles that 1g graphene oxide and 1g partial size peak value are 0.7 μm are added to ultrasound 1h in ethanol solution.
(2) solution is filtered with vacuum filtration method prepare laminated film.
(3) laminated film is added in the dilute hydrochloric acid solution that enough mass fractions are 10% and impregnates 2h, reaction terminates
Afterwards by film naturally dry.
(4) independent self-supporting film is heated at a temperature of 70 DEG C, continues 4h.
(5) independent self-supporting film is put into reduction in hydroiodic acid solution and obtains the graphene film of independent self-supporting.
Embodiment 3
(1) the high alumina particles that 2g graphene oxide and 1g partial size peak value are 10 μm are added to ultrasound 1h in ethanol solution.
(2) solution is filtered with vacuum filtration method prepare laminated film.
(3) laminated film is added in the dilute hydrochloric acid solution that enough mass fractions are 10% and impregnates 2h, reaction terminates
Afterwards by film naturally dry.
(4) independent self-supporting film is heated at a temperature of 70 DEG C, continues 4h.
(5) independent self-supporting film is put into reduction in hydroiodic acid solution and obtains the graphene film of independent self-supporting.
Embodiment 4
(1) the high alumina particles that 2g graphene oxide and 1g partial size peak value are 0.7 μm are added to ultrasound 1h in ethanol solution.
(2) solution is filtered with vacuum filtration method prepare laminated film.
(3) laminated film is added in the dilute hydrochloric acid solution that enough mass fractions are 10% and impregnates 2h, reaction terminates
Afterwards by film naturally dry.
(4) independent self-supporting film is heated at a temperature of 100 DEG C, continues 2h.
(5) independent self-supporting film is put into reduction in hydroiodic acid solution and obtains the graphene film of independent self-supporting.
Comparative example 1
(1) 2g graphene oxide is added to ultrasound 1h in ethanol solution.
(2) solution is filtered with vacuum filtration method prepare film.
(3) film is put into reduction in hydroiodic acid solution and obtains the graphene film of independent self-supporting.
Fig. 1 is the SEM figure that the present embodiment prepares graphene film surface.
The Applicant declares that the present invention is explained by the above embodiments detailed process equipment and process flow of the invention,
But the present invention is not limited to the above detailed process equipment and process flow, that is, it is above-mentioned detailed not mean that the present invention must rely on
Process equipment and process flow could be implemented.It should be clear to those skilled in the art, any improvement in the present invention,
Addition, selection of concrete mode of equivalence replacement and auxiliary element to each raw material of product of the present invention etc., all fall within of the invention
Within protection scope and the open scope.
Claims (6)
1. a kind of preparation method of high fold grapheme material, includes the following steps:
(1) that graphene oxide and high alumina particles are added to ultrasonic mixing in ethanol solution is uniform, filters into laminated film, will answer
It closes film and is added in enough dilute hydrochloric acid solutions and impregnate, after reaction by film naturally dry；
(2) heated oxide graphene film obtains the stone of independent self-supporting using hydroiodic acid solution reduction to remove residual solvent
Black alkene film.
2. preparation method according to claim 1, which is characterized in that the partial size of the high alumina particles in step (1) is 0.7
μm or 10 μm.
3. preparation method according to claim 1, which is characterized in that graphene oxide and high alumina particles in step (1)
Mass ratio is 0.1~10.
4. preparation method according to claim 1, which is characterized in that ultrasonic time is 0.5~6 hour in step (1).
5. preparation method according to claim 1, which is characterized in that dilute hydrochloric acid solution mass fraction is in step (1)
10%, hydrochloric acid total amount should be more than for high alumina particle reaction amount used.
6. preparation method according to claim 1, which is characterized in that heating temperature is 60~100 DEG C in step (2), when
Between be 2~10h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201811194670.6A CN109052376A (en) | 2018-09-29 | 2018-09-29 | A kind of preparation method of high fold grapheme material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811194670.6A CN109052376A (en) | 2018-09-29 | 2018-09-29 | A kind of preparation method of high fold grapheme material |
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| Publication Number | Publication Date |
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| CN109052376A true CN109052376A (en) | 2018-12-21 |
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| CN201811194670.6A Withdrawn CN109052376A (en) | 2018-09-29 | 2018-09-29 | A kind of preparation method of high fold grapheme material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113522059A (en) * | 2021-07-02 | 2021-10-22 | 五邑大学 | Folded graphene oxide film and preparation method thereof |
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2018
- 2018-09-29 CN CN201811194670.6A patent/CN109052376A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113522059A (en) * | 2021-07-02 | 2021-10-22 | 五邑大学 | Folded graphene oxide film and preparation method thereof |
| CN113522059B (en) * | 2021-07-02 | 2023-02-17 | 五邑大学 | Folded graphene oxide film and preparation method thereof |
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Application publication date: 20181221 |
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