CN105174248A - Preparation method of graphene oxide sheet with different layers/liquid crystal/film - Google Patents
Preparation method of graphene oxide sheet with different layers/liquid crystal/film Download PDFInfo
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- CN105174248A CN105174248A CN201510369445.1A CN201510369445A CN105174248A CN 105174248 A CN105174248 A CN 105174248A CN 201510369445 A CN201510369445 A CN 201510369445A CN 105174248 A CN105174248 A CN 105174248A
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Abstract
The present invention belongs to the technical field of graphene oxides, and specifically discloses a preparation method of a graphene oxide sheet with different layers/liquid crystal/film. The preparation method comprises: dispersing graphite oxide in a solvent, carrying out an ultrasound treatment, carrying out centrifugation separation, extracting the lower layer liquid in the centrifugation tube every 0.5-3 h and labeling as a group of the samples until the supernatant is colorless and transparent, and removing the solvent from the sample so as to obtain the graphene oxide sheet; carrying out further centrifugation concentration on the graphene oxide sheet, taking the lower layer liquid, and removing the solvent to obtain a graphene oxide liquid crystal; and coating the graphene oxide liquid crystal onto a substrate in a dropwide manner, and drying at a temperature of 15-35 DEG C so as to obtain the graphene oxide film. According to the present invention, with the preparation method, the problems that the graphene oxide sheets with multiple layers, two layers and one layer can not be concurrently and precisely obtained and the liquid crystal phase preparation is complex in the prior art are solved; and the graphene oxide liquid crystal preparation is simple, the raw materials achieve the zero loss, the film assembly period is short, and the obtained film has the optical anti-counterfeiting capability, such that the obtained film has the good development prospects in the anti-counterfeiting field.
Description
Technical field
The invention belongs to technical field of preparation of graphene oxide, be specifically related to a kind of preparation method of different sheet number of plies graphene oxide sheet/liquid crystal/film.
Background technology
The graphene oxide with liquid crystal behavior can carry out self-assembly effectively, and the self-assembled material formed has excellent physical strength and good toughness, thus as building module material, has application prospect.The liquid crystal behavior had based on the graphene oxide sheet of individual layer report by people, but the liquid crystal behavior of multilayer and two-layer graphene oxide sheet and self assembling process thereof there is not yet report.Therefore carry out development and utilization that is two-layer and the graphene oxide liquid crystal behavior of multilayer, be beneficial to effective utilization of resource, have economy and social effect.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of different sheet number of plies graphene oxide sheet/liquid crystal/film.
For achieving the above object, the technical solution used in the present invention is as follows:
A preparation method for different sheet number of plies graphene oxide sheet/liquid crystal/film, step is as follows:
(1), graphite oxide (can be the graphite oxide particulate of arbitrary dimension) is scattered in solvent, be made into the suspension of mass concentration 0.05-0.5%, supersound process 20-60min, then it is carried out centrifugation under 8000-20000r/min, extract a centrifuge tube subnatant at interval of 0.5-3h and be labeled as one group of sample, till upper liquid water white transparency, namely solvent in removing sample obtains graphene oxide sheet, and the graphene oxide sheet obtained is with the increase of extraction time, the sheet number of plies reduces gradually;
(2) the further centrifugal concentrating of graphene oxide sheet, step (1) obtained, this time centrifugal centrifugation rate is identical with the centrifugation rate of step (1), centrifugation time is identical with the interval time of step (1), gets subnatant removing solvent wherein and namely obtains graphene oxide liquid crystal;
(3), be coated in substrate by the graphene oxide liquid crystal drop that step (2) obtains, 15-35 DEG C of drying, obtains graphene oxide film.
Described solvent is one or more the combination in water, DMF, N-Methyl pyrrolidone, ethanol, Virahol, propyl carbinol and ethylene glycol.
The present invention, relative to prior art, has following advantage:
The invention solves and accurately can not obtain the complicated problem of multilayer, the graphene oxide sheet of two-layer and one deck and mesomorphic phase preparation at present simultaneously.Graphene oxide liquid crystal preparation of the present invention is simple, raw material zero loss, 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 it is simple and easy to get to have method, film dimensions is controlled, the technical superiority of green non-pollution.
Accompanying drawing explanation
, scheme in 3h(Fig. 1: 30min(left figure in interval in embodiment 1)), the right figure of 6h() extract the atomic force microscopy of graphene oxide sheet of preparation.
, scheme in 3h(Fig. 2: 30min(left figure in interval in embodiment 1)), the right figure of 6h() extract the polarisation photo of graphene oxide liquid crystal of preparation.
Fig. 3: prepare the photo in kind during graphene oxide film in embodiment 1.
, scheme in 3h(Fig. 4: 30min(left figure in interval in embodiment 1)), the right figure of 6h() extract the polarisation photo of graphene oxide film of preparation.
Embodiment
With specific embodiment, technical scheme of the present invention is described below, but protection scope of the present invention is not limited thereto:
Embodiment 1
(1), by 2g graphite oxide be dispersed in 1600ml deionized water, forming mass concentration is the suspension of 0.125%, and ultrasonic 0.5h under 240W power, makes graphite oxide be uniformly dispersed in deionized water; By dispersion liquid centrifugation under the constant centrifugation rate of 10000r/min, extract a centrifuge tube subnatant at interval of 30min and be designated as one group of sample, altogether extract 12 times, the atomic force microscopy of the sample extracted when interval 30min, 3h, 6h is shown in Fig. 1, known: the sample extracted when interval 30min, 3h, 6h is respectively the graphene oxide sheet of multilayer, bilayer and individual layer, namely along with the increase of extraction time, thickness of sample (the sheet number of plies) reduces gradually;
And then the sample centrifugal concentrating 30min under 10000r/min respectively will extracted when above-mentioned interval 30min, 3h, 6h (2), subnatant is graphene oxide liquid crystal, and Fig. 2 is shown in by corresponding polarizing microscope, can observe obvious liquid crystal behavior;
(3), then the graphene oxide liquid crystal drop that interval 30min, 3h, 6h correspondence obtains is coated with on a glass (material object is shown in Fig. 3), room temperature 25 DEG C of seasoninies, obtain graphene oxide film, Fig. 4 is shown in by corresponding polarizing microscope, can observe and have obvious birefringent phenomenon.
Embodiment 2
Interval time in step (1) is extended to 2h, extracts 4 times, correspondingly, the centrifugation time in step (2) also extends to 2h, and other is all with embodiment 1.
Embodiment 3
(1), by 1g graphite oxide be dispersed in 1500ml deionized water, forming mass concentration is the suspension of 0.067%, and ultrasonic 20min under 240W power, makes graphite oxide be uniformly dispersed in deionized water; By dispersion liquid centrifugation under the constant centrifugation rate of 10000r/min, extract a centrifuge tube subnatant at interval of 1h and be designated as one group of sample, altogether extract 6 times, obtain the graphene oxide sheet that the number of plies reduces gradually;
(2) and then by above-mentioned sample centrifugal concentrating 1h under 10000r/min respectively, subnatant is graphene oxide liquid crystal;
(3), be then coated with on a glass by the graphene oxide liquid crystal drop obtained, room temperature 25 DEG C of seasoninies, obtain the graphene oxide film with birefringent phenomenon.
Claims (2)
1. a preparation method for different sheet number of plies graphene oxide sheet/liquid crystal/film, is characterized in that step is as follows:
(1), graphite oxide is scattered in solvent, be made into the suspension of mass concentration 0.05-0.5%, supersound process 20-60min, then it is carried out centrifugation under 8000-20000r/min, extract a subnatant at interval of 0.5-3h and be labeled as one group of sample, till upper liquid water white transparency, namely the solvent in removing sample obtains graphene oxide sheet, and the graphene oxide sheet obtained is with the increase of extraction time, the sheet number of plies reduces gradually;
(2) the further centrifugal concentrating of graphene oxide sheet, step (1) obtained, this time centrifugal centrifugation rate is identical with the centrifugation rate of step (1), centrifugation time is identical with the interval time of step (1), gets subnatant removing solvent wherein and namely obtains graphene oxide liquid crystal;
(3), be coated in substrate by the graphene oxide liquid crystal drop that step (2) obtains, 15-35 DEG C of drying, obtains graphene oxide film.
2. the preparation method of different sheet number of plies graphene oxide sheet/liquid crystal/film as claimed in claim 1, it is characterized in that: described solvent is one or more the combination in water, DMF, N-Methyl pyrrolidone, ethanol, Virahol, propyl carbinol and ethylene glycol.
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| CN201510369445.1A CN105174248B (en) | 2015-06-30 | 2015-06-30 | A kind of preparation method of different piece number of plies graphene oxide sheet/liquid crystal/films |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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| 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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2015
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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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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