CN105174248B - A kind of preparation method of different piece number of plies graphene oxide sheet/liquid crystal/films - Google Patents
A kind of preparation method of different piece number of plies graphene oxide sheet/liquid crystal/films Download PDFInfo
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- CN105174248B CN105174248B CN201510369445.1A CN201510369445A CN105174248B CN 105174248 B CN105174248 B CN 105174248B CN 201510369445 A CN201510369445 A CN 201510369445A CN 105174248 B CN105174248 B CN 105174248B
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Abstract
The invention belongs to technical field of preparation of graphene oxide, specifically discloses a kind of preparation method of different piece number of plies graphene oxide sheet/liquid crystal/films.Graphite oxide is scattered in solvent, is ultrasonically treated, is then centrifuged, extracting a centrifuge tube subnatant at interval of 0.5 3h is labeled as one group of sample, and untill upper liquid water white transparency, the solvent removed in sample produces graphene oxide sheet；By the further centrifugal concentrating of graphene oxide sheet, take subnatant to remove solvent therein and produce graphene oxide liquid crystal；Graphene oxide liquid crystal drop is coated in substrate, 15 35 DEG C of dryings, produces graphene oxide film.The present invention solves the problems, such as can not to be accurately obtained multilayer simultaneously at present, the graphene oxide sheet and liquid crystalline phase of two layers and one layer prepare it is complicated.Graphene oxide liquid crystal of the present invention is prepared simply, and raw material zero is lost, and film assembling cycle is short, and gained film has optical anti-counterfeiting ability, it is had good development prospect in anti-counterfeit field.
Description
Technical field
The invention belongs to technical field of preparation of graphene oxide, and in particular to and a kind of different piece number of plies graphene oxide sheets/
The preparation method of liquid crystal/film.
Background technology
Graphene oxide with liquid crystal behavior can carry out effectively self assembly, and the self-assembled material formed has excellent
Different mechanical strength and good toughness, thus as structure module material, great application prospect.Graphite oxide based on individual layer
Liquid crystal behavior possessed by alkene piece is reported by people, however the liquid crystal behavior of multilayer and two layers of graphene oxide sheet and
Its self assembling process is there is not yet report.Therefore the development and utilization of the graphene oxide liquid crystal behavior of two layers and multilayer, profit are carried out
In effective utilization of resource, great economy and social effect.
The content of the invention
It is an object of the invention to provide a kind of preparation method of different piece number of plies graphene oxide sheet/liquid crystal/films.
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of preparation method of different piece number of plies graphene oxide sheet/liquid crystal/films, step are as follows：
（1）, by graphite oxide（It can be the graphite oxide particulate of arbitrary dimension）It is scattered in solvent, is made into mass concentration
0.05-0.5% suspension, 20-60min is ultrasonically treated, then it is centrifuged under 8000-20000 r/min,
A centrifuge tube subnatant is extracted at interval of 0.5-3h and is labeled as one group of sample, untill upper liquid water white transparency, removes sample
Solvent in product produces graphene oxide sheet, and obtained graphene oxide sheet is gradual with the increase of extraction time, the piece number of plies
Reduce；
（2）, by step（1）The obtained further centrifugal concentrating of graphene oxide sheet, the centrifugation rate and step of this centrifugation
Suddenly（1）Centrifugation rate it is identical, centrifugation time and step（1）Interval time it is identical, take subnatant to remove solvent therein i.e.
Obtain graphene oxide liquid crystal；
（3）, by step（2）Obtained graphene oxide liquid crystal drop is coated in substrate, 15-35 DEG C of drying, produces oxidation stone
Black alkene film.
The solvent is water, N,N-dimethylformamide, 1-METHYLPYRROLIDONE, ethanol, isopropanol, n-butanol and second two
One or more combinations in alcohol.
The present invention has the advantage that relative to prior art：
The present invention solves and can not be accurately obtained multilayer, the graphene oxide sheet and liquid crystal of two layers and one layer simultaneously at present
Mutually prepare the problem of complicated.Graphene oxide liquid crystal of the present invention is prepared simply, and raw material zero is lost, and film assembling cycle is short, gained
Film has the phenomenon of optical birefringence, and this has a good application prospect in optical anti-counterfeiting field, and simply easy with method
, film dimensions are controllable, the technical advantage of green non-pollution.
Brief description of the drawings
Fig. 1：30min is spaced in embodiment 1（Left figure）、3h（Middle figure）、6h（Right figure）Extract the graphene oxide sheet prepared
Atomic force microscopy.
Fig. 2：30min is spaced in embodiment 1（Left figure）、3h（Middle figure）、6h（Right figure）Extract the graphene oxide liquid prepared
Brilliant polarisation photo.
Fig. 3：The photo in kind during graphene oxide film is prepared in embodiment 1.
Fig. 4：30min is spaced in embodiment 1（Left figure）、3h（Middle figure）、6h（Right figure）It is thin to extract the graphene oxide prepared
The polarisation photo of film.
Embodiment
Technical scheme is illustrated with specific embodiment below, but protection scope of the present invention is not limited to
This：
Embodiment 1
（1）, 2g graphite oxides are dispersed in 1600ml deionized waters, form the suspension that mass concentration is 0.125%,
Ultrasonic 0.5h, makes graphite oxide be uniformly dispersed in deionized water under 240W power；By dispersion liquid 10000 r/min it is constant from
Centrifuged under heart speed, extracting a centrifuge tube subnatant at interval of 30min is designated as one group of sample, extracts 12 times altogether,
The atomic force microscopy of the sample extracted when 30min, 3h, 6h is shown in Fig. 1, it is known that：It is spaced what is extracted when 30min, 3h, 6h
Sample is respectively the graphene oxide sheet of multilayer, bilayer and individual layer, i.e., with the increase of extraction time, thickness of sample（The piece number of plies）
It is gradually reduced；
（2）And then the sample extracted when again by above-mentioned interval 30min, 3h, 6h centrifuged respectively under 10000 r/min it is dense
Contracting 30min, subnatant are graphene oxide liquid crystal, and corresponding petrographic microscope is shown in Fig. 2, it is observed that obvious liquid crystal row
For；
（3）And then interval 30min, 3h, 6h graphene oxide liquid crystal drop correspondingly obtained are applied on a glass（It is in kind
See Fig. 3）, 25 DEG C of natural dryings of room temperature, graphene oxide film is obtained, corresponding petrographic microscope is shown in Fig. 4, it is observed that tool
There is obvious birefringent phenomenon.
Embodiment 2
By step（1）In interval time extend to 2h, extract 4 times, correspondingly, step（2）In centrifugation time also prolong
Length is other with embodiment 1 to 2h.
Embodiment 3
（1）, 1g graphite oxides are dispersed in 1500ml deionized waters, form the suspension that mass concentration is 0.067%,
Ultrasonic 20min, makes graphite oxide be uniformly dispersed in deionized water under 240W power；Dispersion liquid is constant in 10000 r/min
Centrifuged under centrifugation rate, extracting a centrifuge tube subnatant at interval of 1h is designated as one group of sample, extracts 6 times, produces altogether
The graphene oxide sheet that the number of plies gradually reduces；
（2）And then by above-mentioned sample, the centrifugal concentrating 1h under 10000 r/min, subnatant are graphite oxide respectively again
Alkene liquid crystal；
（3）And then apply obtained graphene oxide liquid crystal drop on a glass, 25 DEG C of natural dryings of room temperature, had
There is the graphene oxide film of birefringent phenomenon.
Claims (4)
1. a kind of preparation method of graphene oxide liquid crystal, it is characterised in that step is as follows：
（1）, graphite oxide is scattered in solvent, be made into mass concentration 0.05-0.5% suspension, be ultrasonically treated 20-
60min, then it is centrifuged under 8000-20000 r/min, a subnatant mark is extracted at interval of 0.5-3h
For one group of sample, untill upper liquid water white transparency, the solvent removed in sample produces graphene oxide sheet, and obtain
With the increase of extraction time, the piece number of plies is gradually reduced graphene oxide sheet；
（2）, by step（1）The obtained further centrifugal concentrating of graphene oxide sheet, the centrifugation rate and step of this centrifugation（1）
Centrifugation rate it is identical, centrifugation time and step（1）Interval time it is identical, take subnatant to remove solvent therein and produce oxidation
Graphene liquid crystal.
2. the preparation method of graphene oxide liquid crystal as claimed in claim 1, it is characterised in that：The solvent is water, N, N-
One or more combinations in dimethylformamide, 1-METHYLPYRROLIDONE, ethanol, isopropanol, n-butanol and ethylene glycol.
3. a kind of preparation method of graphene oxide film, it is characterised in that step is as follows：
（1）, graphite oxide is scattered in solvent, be made into mass concentration 0.05-0.5% suspension, be ultrasonically treated 20-
60min, then it is centrifuged under 8000-20000 r/min, a subnatant mark is extracted at interval of 0.5-3h
For one group of sample, untill upper liquid water white transparency, the solvent removed in sample produces graphene oxide sheet, and obtain
With the increase of extraction time, the piece number of plies is gradually reduced graphene oxide sheet；
（2）, by step（1）The obtained further centrifugal concentrating of graphene oxide sheet, the centrifugation rate and step of this centrifugation（1）
Centrifugation rate it is identical, centrifugation time and step（1）Interval time it is identical, take subnatant to remove solvent therein and produce oxidation
Graphene liquid crystal；
（3）, by step（2）Obtained graphene oxide liquid crystal drop is coated in substrate, 15-35 DEG C of drying, produces graphene oxide
Film.
4. the preparation method of graphene oxide film as claimed in claim 3, it is characterised in that：The solvent is water, N, N-
One or more combinations in dimethylformamide, 1-METHYLPYRROLIDONE, ethanol, isopropanol, n-butanol and ethylene glycol.
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| CN108441232A (en) * | 2018-03-26 | 2018-08-24 | 京东方科技集团股份有限公司 | Liquid-crystal composition and preparation method, display panel, display device |
| CN114717688A (en) * | 2022-03-09 | 2022-07-08 | 北京创新爱尚家科技股份有限公司 | Graphene aerogel fiber, graphene aerogel thermal insulation flocculus and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102750998A (en) * | 2012-07-09 | 2012-10-24 | 深圳市贝特瑞纳米科技有限公司 | Transparent graphene conductive thin film and preparation method thereof |
| CN102815697A (en) * | 2012-08-28 | 2012-12-12 | 中国科学院过程工程研究所 | Preparation method of graphene oxide microspheres |
| CN104386676A (en) * | 2014-11-05 | 2015-03-04 | 北京化工大学 | Preparation method of graphene |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102750998A (en) * | 2012-07-09 | 2012-10-24 | 深圳市贝特瑞纳米科技有限公司 | Transparent graphene conductive thin film and preparation method thereof |
| CN102815697A (en) * | 2012-08-28 | 2012-12-12 | 中国科学院过程工程研究所 | Preparation method of graphene oxide microspheres |
| CN104386676A (en) * | 2014-11-05 | 2015-03-04 | 北京化工大学 | Preparation method of graphene |
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