CN104229777B - A kind of green reducing preparation method of self-supporting oxidation graphene film - Google Patents
A kind of green reducing preparation method of self-supporting oxidation graphene film Download PDFInfo
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- CN104229777B CN104229777B CN201410241862.3A CN201410241862A CN104229777B CN 104229777 B CN104229777 B CN 104229777B CN 201410241862 A CN201410241862 A CN 201410241862A CN 104229777 B CN104229777 B CN 104229777B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 75
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 230000003647 oxidation Effects 0.000 title claims description 23
- 238000007254 oxidation reaction Methods 0.000 title claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 239000012043 crude product Substances 0.000 claims description 18
- 239000012528 membrane Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- 229950000845 politef Drugs 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 238000003828 vacuum filtration Methods 0.000 claims description 5
- XOGTZOOQQBDUSI-UHFFFAOYSA-M Mesna Chemical compound [Na+].[O-]S(=O)(=O)CCS XOGTZOOQQBDUSI-UHFFFAOYSA-M 0.000 claims description 4
- 235000010323 ascorbic acid Nutrition 0.000 claims description 4
- 239000011668 ascorbic acid Substances 0.000 claims description 4
- 229960005070 ascorbic acid Drugs 0.000 claims description 4
- 229960004635 mesna Drugs 0.000 claims description 4
- PPASLZSBLFJQEF-RXSVEWSESA-M sodium-L-ascorbate Chemical compound [Na+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RXSVEWSESA-M 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 235000010378 sodium ascorbate Nutrition 0.000 claims description 3
- 229960005055 sodium ascorbate Drugs 0.000 claims description 3
- PPASLZSBLFJQEF-RKJRWTFHSA-M sodium ascorbate Substances [Na+].OC[C@@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RKJRWTFHSA-M 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 7
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 230000015556 catabolic process Effects 0.000 abstract description 2
- 238000006731 degradation reaction Methods 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 238000001338 self-assembly Methods 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 42
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 3
- 238000000137 annealing Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000003303 reheating Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005291 magnetic effect Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Abstract
The invention discloses the green reducing preparation method of a kind of self-supporting graphene film. The method includes graphene oxide water solution elder generation and reducing agent pre-reaction at normal temperatures, adopts sucking filtration self-assembly method to prepare prereduction graphene oxide film, then reacts prepared self-supporting graphene film with reducing agent under hydrothermal conditions. The reducing agent that the method adopts is nontoxic, and environment-friendly, it is possible to natural degradation, non-environmental-pollution, preparation process is simple and easy to control.
Description
Technical field
Present invention relates particularly to a kind of self-supporting oxidation graphene film preparation method, belong to technical field of nano material.
Background technology
Graphene is a kind of by the bi-dimensional cellular shape lattice structure carbonaceous material of the tightly packed one-tenth of monolayer carbon atom. Owing to it has the performance of special nanostructured and excellence, the material based on Graphene shows huge application potential at numerous areas such as electronics, optics, magnetics, biomedicine, catalysis, sensor, energy storage.
Graphene film is one of focus of Graphene research, and graphene film is typically based on graphene oxide film and prepares. Owing to graphene oxide film oxy radical number is many and conducts electricity hardly, limit its application in electronic device, its electric conductivity will be recovered and graphene oxide film must be reduced.
Graphene film is prepared in graphene oxide film reduction generally can adopt two kinds of methods: (1) hydrazine steam reduction graphene oxide membrane, reheating annealing reduction; (2) there iing dispersant to deposit electronation graphene oxide solution in case, preparing graphene film by the graphene oxide solution of reduction, reheating annealing reduction. In the method for hydrazine steam reduction graphene oxide membrane, owing to the vapour permeability of grapheme material is poor, steam reduction can only be worked in uppermost surface, causes that film resistor increases up to saturated along with the thickness of thin film. Another kind of method electronation graphene oxide in the solution, it usually needs use hydrazine or sodium borohydride etc. poisonous or expensive reagent, and cause environmental pollution.
Summary of the invention
A kind of method that it is an object of the invention to adopt green reduction, first by graphene oxide water solution and reducing agent pre-reaction at normal temperatures, sucking filtration self assembly prepares prereduction graphene oxide film, then prereduction graphene oxide film and reducing agent is reacted prepared self-supporting graphene film under hydrothermal conditions.
The green reducing preparation method of a kind of self-supporting oxidation graphene film, comprises the steps:
(1) weigh reducing agent and join in the graphene oxide water solution that mass concentration is 2～5mg/mL, under room temperature, stirring carries out prereduction reaction 16～24 hours, preparing prereduction graphene oxide mixed solution, the mass ratio of wherein said reducing agent and graphene oxide is 0.5: 1～2: 1;
(2) the prereduction graphene oxide mixed solution that step (1) the is prepared politef microporous filter membrane vacuum filtration by 0.22 micron of aperture, peel off and remove politef microporous filter membrane, prepare prereduction graphene oxide film crude product, it is placed in 80～150 DEG C of vacuum drying ovens dry 16～24 hours, prepares prereduction graphene oxide film;
(3) described prereduction graphene oxide film is placed in water heating kettle, adding mass concentration is 2.5～20mg/mL reducing agent aqueous solution, water heating kettle carries out hydro-thermal reaction 16～24 hours under 90～150 DEG C of conditions, preparing oxidation graphene film crude product, the mass ratio of wherein said reducing agent and prereduction graphene oxide is 0.5: 1～4: 1;
(4) take out described oxidation graphene film crude product, by rinsed with deionized water, after drying, obtain self-supporting oxidation graphene film;
Wherein said reducing agent refers to the one in mesna, ascorbic acid or sodium ascorbate.
The preparation method of the present invention, the reducing agent of employing is nontoxic, it is possible to natural degradation, environment-friendly, non-environmental-pollution, and preparation process is simple and easy to control.
Accompanying drawing explanation
Fig. 1 is the optical photograph of the self-supporting oxidation graphene film of preparation in embodiment 1. Wherein a figure is self-supporting oxidation graphene film face-up optical photo; B figure is self-supporting oxidation graphene film curved optical photo.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described, but protection scope of the present invention is not limited to this.
Embodiment 1
Weigh reducing agent mesna 0.1g, join in the graphene oxide water solution that 25mL concentration is 4mg/mL, under room temperature, stirring carries out prereduction reaction 24h, gained mixed solution is carried out vacuum filtration by aperture 0.22um politef microporous filter membrane, peel off and remove politef microporous filter membrane, prepare prereduction graphene oxide film crude product. After prereduction graphene oxide film crude product is placed in 80 DEG C of vacuum drying ovens dry 24h, take out, prepare prereduction graphene oxide film. It is placed in water heating kettle, adds the mesna aqueous solution 20mL that mass concentration is 5mg/mL, in water heating kettle, carry out hydro-thermal reaction 24h under 120 DEG C of conditions, prepare oxidation graphene film crude product. Take out described oxidation graphene film crude product, by rinsed with deionized water, after drying, obtain self-supporting oxidation graphene film, as shown in Figure 1.
Embodiment 2
Weigh reducing agent ascorbic acid 0.2g, join in the graphene oxide water solution that 25mL concentration is 4mg/mL, under room temperature, stirring carries out prereduction reaction 16h, gained mixed solution is carried out vacuum filtration by aperture 0.22um politef microporous filter membrane, peel off and remove politef microporous filter membrane, prepare prereduction graphene oxide film crude product. After prereduction graphene oxide film crude product is placed in 150 DEG C of vacuum drying ovens dry 16h, take out, prepare prereduction graphene oxide film. It is placed in water heating kettle, adds the aqueous ascorbic acid 20mL that mass concentration is 20mg/mL, in water heating kettle, carry out hydro-thermal reaction 24h under 90 DEG C of conditions, prepare oxidation graphene film crude product. Take out described oxidation graphene film crude product, by rinsed with deionized water, after drying, obtain self-supporting oxidation graphene film
Embodiment 3
Weigh reducing agent sodium ascorbate O.05g, join in the graphene oxide water solution that 25mL concentration is 4mg/mL, under room temperature, stirring carries out prereduction reaction l6h, gained mixed solution is carried out vacuum filtration by aperture 0.22um politef microporous filter membrane, peel off and remove politef microporous filter membrane, prepare prereduction graphene oxide film crude product. After prereduction graphene oxide film crude product is placed in 80 DEG C of vacuum drying ovens dry 16h, take out, prepare prereduction graphene oxide film.It is placed in water heating kettle, adds the ascorbic acid sodium water solution 20mL that mass concentration is 2.5mg/mL, in water heating kettle, carry out hydro-thermal reaction 16h under 150 DEG C of conditions, prepare oxidation graphene film crude product. Take out described oxidation graphene film crude product, by rinsed with deionized water, after drying, obtain self-supporting oxidation graphene film.
Claims (1)
1. the green reducing preparation method of a self-supporting oxidation graphene film, it is characterised in that comprise the steps:
(1) weigh reducing agent and join in the graphene oxide water solution that mass concentration is 2～5mg/mL, under room temperature, stirring carries out prereduction reaction 16～24 hours, preparing prereduction graphene oxide mixed solution, the mass ratio of wherein said reducing agent and graphene oxide is 0.5: 1～2: 1;
(2) the prereduction graphene oxide mixed solution that step (1) the is prepared politef microporous filter membrane vacuum filtration by 0.22 micron of aperture, peel off and remove politef microporous filter membrane, prepare prereduction graphene oxide film crude product, it is placed in 80～150 DEG C of vacuum drying ovens dry 16～24 hours, prepares prereduction graphene oxide film;
(3) described prereduction graphene oxide film is placed in water heating kettle, adding mass concentration is 2.5～20mg/mL reducing agent aqueous solution, water heating kettle carries out hydro-thermal reaction 16～24 hours under 90～150 DEG C of conditions, preparing oxidation graphene film crude product, the mass ratio of wherein said reducing agent and prereduction graphene oxide is 0.5: 1～4: 1:
(4) take out described oxidation graphene film crude product, by rinsed with deionized water, after drying, obtain self-supporting oxidation graphene film;
Wherein said reducing agent refers to the one in mesna, ascorbic acid or sodium ascorbate.
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| CN110980797A (en) * | 2019-12-16 | 2020-04-10 | 岭南师范学院 | Preparation method of graphene/porous zinc oxide composite film |
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| MX2016016239A (en) | 2014-06-16 | 2017-04-06 | Univ California | Hybrid electrochemical cell. |
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| US11097951B2 (en) * | 2016-06-24 | 2021-08-24 | The Regents Of The University Of California | Production of carbon-based oxide and reduced carbon-based oxide on a large scale |
| WO2018044786A1 (en) | 2016-08-31 | 2018-03-08 | The Regents Of The University Of California | Devices comprising carbon-based material and fabrication thereof |
| CN106698402A (en) * | 2017-01-05 | 2017-05-24 | 东南大学 | Production method of metal nano-particle doped flexible self-supporting graphene film |
| CN110117003A (en) * | 2018-02-05 | 2019-08-13 | 庄鹏宇 | A kind of preparation method of redox graphene film |
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| CN101800310B (en) * | 2010-04-02 | 2013-02-13 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for preparing graphene-doped anode material for lithium-ion batteries |
| WO2014020003A1 (en) * | 2012-08-03 | 2014-02-06 | Asml Netherlands B.V. | Lithographic apparatus and method of manufacturing a device |
| CN103021574B (en) * | 2012-12-27 | 2016-01-13 | 上海交通大学 | A kind of Graphene/inorganic semiconductor composite film and preparation method thereof |
| CN103449504B (en) * | 2013-06-26 | 2015-06-10 | 中山大学 | Zinc oxide nanodisk/graphene composite material and preparation method thereof |
| CN103726133B (en) * | 2014-01-02 | 2016-04-06 | 东华大学 | High strength, compact neat porous graphene fiber and continuous production method thereof |
| CN103787319B (en) * | 2014-01-17 | 2015-10-14 | 深圳粤网节能技术服务有限公司 | Large-scale preparation method of graphene quantum dots |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110980797A (en) * | 2019-12-16 | 2020-04-10 | 岭南师范学院 | Preparation method of graphene/porous zinc oxide composite film |
| CN110980797B (en) * | 2019-12-16 | 2022-04-05 | 岭南师范学院 | Preparation method of graphene/porous zinc oxide composite film |
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