CN104229777A - Green reduction preparation method of self-supporting reduced graphene oxide thin film - Google Patents
Green reduction preparation method of self-supporting reduced graphene oxide thin film Download PDFInfo
- Publication number
- CN104229777A CN104229777A CN201410241862.3A CN201410241862A CN104229777A CN 104229777 A CN104229777 A CN 104229777A CN 201410241862 A CN201410241862 A CN 201410241862A CN 104229777 A CN104229777 A CN 104229777A
- Authority
- CN
- China
- Prior art keywords
- graphene oxide
- prereduction
- self
- film
- reductive agent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 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
- 230000002829 reductive effect Effects 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000010409 thin film Substances 0.000 title abstract 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000001914 filtration Methods 0.000 claims abstract description 11
- 230000003647 oxidation Effects 0.000 claims description 22
- 238000007254 oxidation reaction Methods 0.000 claims description 22
- 239000012043 crude product Substances 0.000 claims description 18
- 239000003795 chemical substances by application Substances 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 10
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 7
- 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 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 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
- 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
- 229960004635 mesna Drugs 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
- 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 3
- 238000000034 method Methods 0.000 abstract description 7
- 239000003638 chemical reducing agent Substances 0.000 abstract description 5
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 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
- 238000006722 reduction reaction Methods 0.000 description 10
- 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
- 239000012528 membrane Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000003303 reheating Methods 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000015556 catabolic process Effects 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
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000006185 dispersion 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
- 230000035699 permeability Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
Abstract
The invention discloses a green reduction preparation method of a self-supporting reduced graphene oxide thin film. The method comprises the following steps: pre-reacting a graphene oxide water solution with a reducing agent at normal temperature, and preparing a pre-reduced graphene oxide thin film through a suction filtering self-assembly method; and reacting the pre-reduced thin film with the reducing agent under a hydrothermal condition to obtain the self-supporting graphene oxide thin film. The reducing agent adopted by the method is non-toxic, environmentally friendly, naturally degradable and free from environmental pollution, and the preparation process is simple and easy to control.
Description
Technical field
The present invention is specifically related to a kind of self-supporting oxidation graphene film preparation method, belongs to technical field of nano material.
Background technology
Graphene is a kind of bi-dimensional cellular shape crystalline network carbonaceous material by the tightly packed one-tenth of monolayer carbon atom.Because it has special nanostructure and the performance of 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 obtains based on graphene oxide film usually.Because graphene oxide film oxy radical number is many and conduct electricity hardly, limit its application in electron device, recover its electroconductibility must reduce to graphene oxide film.
Graphene oxide film reduction is prepared graphene film and generally can be adopted two kinds of methods: (1) hydrazine steam reduction graphene oxide membrane, reheating annealing reduction; (2) there iing dispersion agent to deposit chemical reduction graphene oxide solution in case, obtaining graphene film by the graphene oxide solution of reduction, reheating annealing reduction.In the method for hydrazine steam reduction graphene oxide membrane, because the vapour permeability of grapheme material is poor, steam reduction can only be worked in uppermost surface, causes sheet resistance to reach capacity along with the thickness increase of film.Another kind method is chemical reduction graphene oxide in the solution, usually needs to use the poisonous or expensive reagent such as hydrazine or sodium borohydride, and causes environmental pollution.
Summary of the invention
The object of the invention is a kind of method adopting green reduction, first by graphene oxide water solution and reductive agent pre-reaction at normal temperatures, suction filtration self-assembly obtains prereduction graphene oxide film, then prereduction graphene oxide film and reductive agent is reacted obtained self-supporting graphene film under hydrothermal conditions.
A green reducing preparation method for self-supporting oxidation graphene film, comprises the steps:
(1) taking reductive agent, to join mass concentration be in the graphene oxide water solution of 2 ~ 5mg/mL, stirred at ambient temperature carries out prereduction reaction 16 ~ 24 hours, obtained prereduction graphene oxide mixing solutions, the mass ratio of wherein said reductive agent and graphene oxide is 0.5: 1 ~ 2: 1;
(2) by the tetrafluoroethylene millipore filtration vacuum filtration of prereduction graphene oxide mixing solutions obtained for step (1) by 0.22 micron, aperture, peel off and remove tetrafluoroethylene millipore filtration, obtained prereduction graphene oxide film crude product, to be placed in 80 ~ 150 DEG C of vacuum drying ovens dry 16 ~ 24 hours, obtained prereduction graphene oxide film;
(3) described prereduction graphene oxide film is placed in water heating kettle, adding mass concentration is 2.5 ~ 20mg/mL reductive agent aqueous solution, hydro-thermal reaction is carried out 16 ~ 24 hours under 90 ~ 150 DEG C of conditions in water heating kettle, obtained oxidation graphene film crude product, the mass ratio of wherein said reductive agent and prereduction graphene oxide is 0.5: 1 ~ 4: 1;
(4) take out described oxidation graphene film crude product, after rinsed with deionized water, drying, obtain self-supporting oxidation graphene film;
Wherein said reductive agent refers to the one in mesna, xitix or sodium ascorbate.
Preparation method of the present invention, the reductive agent of employing is nontoxic, can natural degradation, and environment-friendly, non-environmental-pollution, 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.
Embodiment
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
Take reductive agent mesna 0.1g, joining 25mL concentration is in the graphene oxide water solution of 4mg/mL, stirred at ambient temperature carries out prereduction reaction 24h, gained mixing solutions is carried out vacuum filtration by aperture 0.22um tetrafluoroethylene millipore filtration, peel off and remove tetrafluoroethylene millipore filtration, obtained prereduction graphene oxide film crude product.After prereduction graphene oxide film crude product being placed in 80 DEG C of dry 24h of vacuum drying oven, take out, obtained prereduction graphene oxide film.Be placed in water heating kettle, add 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, obtained oxidation graphene film crude product.Take out described oxidation graphene film crude product, after rinsed with deionized water, drying, obtain self-supporting oxidation graphene film, as shown in Figure 1.
Embodiment 2
Take reductive agent xitix 0.2g, joining 25mL concentration is in the graphene oxide water solution of 4mg/mL, stirred at ambient temperature carries out prereduction reaction 16h, gained mixing solutions is carried out vacuum filtration by aperture 0.22um tetrafluoroethylene millipore filtration, peel off and remove tetrafluoroethylene millipore filtration, obtained prereduction graphene oxide film crude product.After prereduction graphene oxide film crude product being placed in 150 DEG C of dry 16h of vacuum drying oven, take out, obtained prereduction graphene oxide film.Be placed in water heating kettle, add 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, obtained oxidation graphene film crude product.Take out described oxidation graphene film crude product, after rinsed with deionized water, drying, obtain self-supporting oxidation graphene film
Embodiment 3
Take reductive agent sodium ascorbate O.05g, joining 25mL concentration is in the graphene oxide water solution of 4mg/mL, stirred at ambient temperature carries out prereduction reaction l6h, gained mixing solutions is carried out vacuum filtration by aperture 0.22um tetrafluoroethylene millipore filtration, peel off and remove tetrafluoroethylene millipore filtration, obtained prereduction graphene oxide film crude product.After prereduction graphene oxide film crude product being placed in 80 DEG C of dry 16h of vacuum drying oven, take out, obtained prereduction graphene oxide film.Be placed in water heating kettle, add the xitix 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, obtained oxidation graphene film crude product.Take out described oxidation graphene film crude product, after rinsed with deionized water, drying, obtain self-supporting oxidation graphene film.
Claims (1)
1. a green reducing preparation method for self-supporting oxidation graphene film, is characterized in that comprising the steps:
(1) taking reductive agent, to join mass concentration be in the graphene oxide water solution of 2 ~ 5mg/mL, stirred at ambient temperature carries out prereduction reaction 16 ~ 24 hours, obtained prereduction graphene oxide mixing solutions, the mass ratio of wherein said reductive agent and graphene oxide is 0.5: 1 ~ 2: 1;
(2) by the tetrafluoroethylene millipore filtration vacuum filtration of prereduction graphene oxide mixing solutions obtained for step (1) by 0.22 micron, aperture, peel off and remove tetrafluoroethylene millipore filtration, obtained prereduction graphene oxide film crude product, to be placed in 80 ~ 150 DEG C of vacuum drying ovens dry 16 ~ 24 hours, obtained prereduction graphene oxide film;
(3) described prereduction graphene oxide film is placed in water heating kettle, adding mass concentration is 2.5 ~ 20mg/mL reductive agent aqueous solution, hydro-thermal reaction is carried out 16 ~ 24 hours under 90 ~ 150 DEG C of conditions in water heating kettle, obtained oxidation graphene film crude product, the mass ratio of wherein said reductive agent and prereduction graphene oxide is 0.5: 1 ~ 4: 1:
(4) take out described oxidation graphene film crude product, after rinsed with deionized water, drying, obtain self-supporting oxidation graphene film;
Wherein said reductive agent refers to the one in mesna, xitix or sodium ascorbate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410241862.3A CN104229777B (en) | 2014-05-28 | 2014-05-28 | A kind of green reducing preparation method of self-supporting oxidation graphene film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410241862.3A CN104229777B (en) | 2014-05-28 | 2014-05-28 | A kind of green reducing preparation method of self-supporting oxidation graphene film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104229777A true CN104229777A (en) | 2014-12-24 |
| CN104229777B CN104229777B (en) | 2016-06-15 |
Family
ID=52218801
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410241862.3A Active CN104229777B (en) | 2014-05-28 | 2014-05-28 | A kind of green reducing preparation method of self-supporting oxidation graphene film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104229777B (en) |
Cited By (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105385417A (en) * | 2015-10-23 | 2016-03-09 | 同济大学 | Preparation method for three-dimensional graphene/phase change heat conduction composite material |
| CN105964151A (en) * | 2016-05-05 | 2016-09-28 | 浙江工业大学 | Preparation method and use of graphene composite film with interlayer MOFs |
| CN106698402A (en) * | 2017-01-05 | 2017-05-24 | 东南大学 | Production method of metal nano-particle doped flexible self-supporting graphene film |
| CN109476487A (en) * | 2016-06-24 | 2019-03-15 | 加利福尼亚大学董事会 | Carbon-based oxides and the large-scale production for restoring carbon-based oxides |
| WO2019149018A1 (en) * | 2018-02-05 | 2019-08-08 | 庄鹏宇 | Preparation method of reduced graphene oxide film |
| CN110127671A (en) * | 2019-06-10 | 2019-08-16 | 中国烟草总公司郑州烟草研究院 | A kind of general preparative methods of redox graphene group compound film |
| CN110127672A (en) * | 2019-06-10 | 2019-08-16 | 中国烟草总公司郑州烟草研究院 | A kind of preparation method of redox graphene film |
| CN110420567A (en) * | 2019-07-12 | 2019-11-08 | 中国工程物理研究院材料研究所 | A kind of preparation method of graphene hydrophobic membrane and the application method of membrane distillation |
| CN111977639A (en) * | 2019-05-22 | 2020-11-24 | 常州第六元素材料科技股份有限公司 | Pre-reduced graphene oxide film and preparation method thereof, graphene heat conduction film and preparation method thereof |
| CN112062121A (en) * | 2020-08-26 | 2020-12-11 | 广西大学 | Method for preparing thermal reduction graphene oxide film by blending sodium lignosulfonate and graphene oxide |
| CN113200534A (en) * | 2021-05-19 | 2021-08-03 | 重庆交通大学 | Preparation method of graphene oxide reduction self-assembly film based on planar base film |
| US11397173B2 (en) | 2011-12-21 | 2022-07-26 | The Regents Of The University Of California | Interconnected corrugated carbon-based network |
| CN115246949A (en) * | 2021-04-27 | 2022-10-28 | 天津工业大学 | Reduced graphene oxide flexible conductive film and three-step moderate reduction preparation process thereof |
| US11569538B2 (en) | 2014-06-16 | 2023-01-31 | The Regents Of The University Of California | Hybrid electrochemical cell |
| CN115784706A (en) * | 2022-11-21 | 2023-03-14 | 中国电子科技集团公司第十八研究所 | Self-supporting reduced graphene oxide film, lithium-free negative current collector and application thereof |
| US11791453B2 (en) | 2016-08-31 | 2023-10-17 | The Regents Of The University Of California | Devices comprising carbon-based material and fabrication thereof |
| US11810716B2 (en) | 2014-11-18 | 2023-11-07 | The Regents Of The University Of California | Porous interconnected corrugated carbon-based network (ICCN) composite |
| US11842850B2 (en) | 2016-01-22 | 2023-12-12 | The Regents Of The University Of California | High-voltage devices |
| US11891539B2 (en) | 2015-12-22 | 2024-02-06 | The Regents Of The University Of California | Cellular graphene films |
| US11915870B2 (en) | 2012-03-05 | 2024-02-27 | The Regents Of The University Of California | Capacitor with electrodes made of an interconnected corrugated carbon-based network |
| US11961667B2 (en) | 2016-03-23 | 2024-04-16 | The Regents Of The University Of California | Devices and methods for high voltage and solar applications |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110980797B (en) * | 2019-12-16 | 2022-04-05 | 岭南师范学院 | Preparation method of graphene/porous zinc oxide composite film |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101800310A (en) * | 2010-04-02 | 2010-08-11 | 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 |
| CN103021574A (en) * | 2012-12-27 | 2013-04-03 | 上海交通大学 | Graphene/inorganic semiconductor composite film and preparation method thereof |
| CN103449504A (en) * | 2013-06-26 | 2013-12-18 | 中山大学 | Zinc oxide nanodisk/graphene composite material and preparation method thereof |
| WO2014020003A1 (en) * | 2012-08-03 | 2014-02-06 | Asml Netherlands B.V. | Lithographic apparatus and method of manufacturing a device |
| CN103726133A (en) * | 2014-01-02 | 2014-04-16 | 东华大学 | High-strength, compact and ordered porous graphene fiber and continuous preparation method thereof |
| CN103787319A (en) * | 2014-01-17 | 2014-05-14 | 深圳粤网节能技术服务有限公司 | Large-scale preparation method of graphene quantum dots |
-
2014
- 2014-05-28 CN CN201410241862.3A patent/CN104229777B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101800310A (en) * | 2010-04-02 | 2010-08-11 | 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 |
| CN103021574A (en) * | 2012-12-27 | 2013-04-03 | 上海交通大学 | Graphene/inorganic semiconductor composite film and preparation method thereof |
| CN103449504A (en) * | 2013-06-26 | 2013-12-18 | 中山大学 | Zinc oxide nanodisk/graphene composite material and preparation method thereof |
| CN103726133A (en) * | 2014-01-02 | 2014-04-16 | 东华大学 | High-strength, compact and ordered porous graphene fiber and continuous preparation method thereof |
| CN103787319A (en) * | 2014-01-17 | 2014-05-14 | 深圳粤网节能技术服务有限公司 | Large-scale preparation method of graphene quantum dots |
Cited By (24)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11397173B2 (en) | 2011-12-21 | 2022-07-26 | The Regents Of The University Of California | Interconnected corrugated carbon-based network |
| US11915870B2 (en) | 2012-03-05 | 2024-02-27 | The Regents Of The University Of California | Capacitor with electrodes made of an interconnected corrugated carbon-based network |
| US11569538B2 (en) | 2014-06-16 | 2023-01-31 | The Regents Of The University Of California | Hybrid electrochemical cell |
| US11810716B2 (en) | 2014-11-18 | 2023-11-07 | The Regents Of The University Of California | Porous interconnected corrugated carbon-based network (ICCN) composite |
| CN105385417B (en) * | 2015-10-23 | 2019-01-25 | 同济大学 | A kind of preparation method of three-dimensional grapheme/heat conduction with phase change composite material |
| CN105385417A (en) * | 2015-10-23 | 2016-03-09 | 同济大学 | Preparation method for three-dimensional graphene/phase change heat conduction composite material |
| US11891539B2 (en) | 2015-12-22 | 2024-02-06 | The Regents Of The University Of California | Cellular graphene films |
| US11842850B2 (en) | 2016-01-22 | 2023-12-12 | The Regents Of The University Of California | High-voltage devices |
| US11961667B2 (en) | 2016-03-23 | 2024-04-16 | The Regents Of The University Of California | Devices and methods for high voltage and solar applications |
| CN105964151A (en) * | 2016-05-05 | 2016-09-28 | 浙江工业大学 | Preparation method and use of graphene composite film with interlayer MOFs |
| CN109476487A (en) * | 2016-06-24 | 2019-03-15 | 加利福尼亚大学董事会 | Carbon-based oxides and the large-scale production for restoring carbon-based oxides |
| US11791453B2 (en) | 2016-08-31 | 2023-10-17 | 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 |
| WO2019149018A1 (en) * | 2018-02-05 | 2019-08-08 | 庄鹏宇 | Preparation method of reduced graphene oxide film |
| CN110117003A (en) * | 2018-02-05 | 2019-08-13 | 庄鹏宇 | A kind of preparation method of redox graphene film |
| CN111977639A (en) * | 2019-05-22 | 2020-11-24 | 常州第六元素材料科技股份有限公司 | Pre-reduced graphene oxide film and preparation method thereof, graphene heat conduction film and preparation method thereof |
| CN110127672A (en) * | 2019-06-10 | 2019-08-16 | 中国烟草总公司郑州烟草研究院 | A kind of preparation method of redox graphene film |
| CN110127671A (en) * | 2019-06-10 | 2019-08-16 | 中国烟草总公司郑州烟草研究院 | A kind of general preparative methods of redox graphene group compound film |
| CN110420567A (en) * | 2019-07-12 | 2019-11-08 | 中国工程物理研究院材料研究所 | A kind of preparation method of graphene hydrophobic membrane and the application method of membrane distillation |
| CN112062121A (en) * | 2020-08-26 | 2020-12-11 | 广西大学 | Method for preparing thermal reduction graphene oxide film by blending sodium lignosulfonate and graphene oxide |
| CN115246949B (en) * | 2021-04-27 | 2023-11-03 | 天津工业大学 | Reduced graphene oxide flexible conductive film and three-step moderate reduction preparation process thereof |
| CN115246949A (en) * | 2021-04-27 | 2022-10-28 | 天津工业大学 | Reduced graphene oxide flexible conductive film and three-step moderate reduction preparation process thereof |
| CN113200534A (en) * | 2021-05-19 | 2021-08-03 | 重庆交通大学 | Preparation method of graphene oxide reduction self-assembly film based on planar base film |
| CN115784706A (en) * | 2022-11-21 | 2023-03-14 | 中国电子科技集团公司第十八研究所 | Self-supporting reduced graphene oxide film, lithium-free negative current collector and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104229777B (en) | 2016-06-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104229777A (en) | Green reduction preparation method of self-supporting reduced graphene oxide thin film | |
| CN103599769B (en) | ZnSn (OH)6 nanometer cubic particle/graphene sandwich structure compound light catalyst | |
| CN103011152B (en) | Graphene material with porous structure and preparation method of graphene material | |
| CN103803537A (en) | Preparation method of graphene | |
| CN104209514A (en) | Method for preparing Ni@C or Co@C core-shell nanoparticles | |
| CN103708450B (en) | A kind of preparation method of graphene nanobelt paper | |
| CN103736993B (en) | The preparation method of graphene/copper composite material | |
| CN107629215B (en) | Method for preparing various metal organic frameworks by using aqueous solvent system | |
| CN112531119B (en) | Flexible transparent electrode and battery suitable for flexible photoelectric device and preparation method | |
| CN105565305A (en) | Method for preparing graphene by using green reducing agent | |
| CN104399998A (en) | Preparation method of graphene/nano-silver composite material | |
| CN108483502A (en) | A kind of preparation method and application of rhenium disulfide nanometer sheet | |
| CN103818898A (en) | Graphene hybrid material with controllable appearance and preparation and appearance control method thereof | |
| CN109569670A (en) | A kind of preparation method of BiOBr/ black phosphorus alkene hetero-junctions nanocomposite | |
| CN106186040A (en) | A kind of hydro-thermal method prepares the method for transient metal doped ZnO nano-wire | |
| CN103665358B (en) | Phosphorus nitrogen copolyester material containing ring three phosphazenium groups and preparation method thereof | |
| CN109513442B (en) | NaBH4Hydrogen production catalyst Co-CoOx@ C-rGO and preparation method thereof | |
| CN111747401A (en) | Preparation method of fluorinated graphene material | |
| CN103395773B (en) | Nano carbon hollow sphere and preparation method thereof | |
| CN109326790A (en) | A kind of 1-dimention nano threadiness sodium titanate and its preparation method and application | |
| CN104261393B (en) | A kind of be reducing agent with guanidine hydrochloride graphene preparation method | |
| CN105016333B (en) | A kind of method that D-glucosamine derivant prepares Graphene | |
| CN103738949A (en) | Preparation method for single-layer graphene isopropanol solution | |
| CN107899378B (en) | Application of metal organic complex membrane as gas separation membrane | |
| CN103738947A (en) | Preparation method for single-layer graphene ethylene glycol solution |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20180529 Address after: 222300 Donghai County Development Zone, Lianyungang, Jiangsu, north of Weihe Road, west of Mount Huangshan road. Patentee after: LIANYUNGANG BOWEI METALLURGICAL MATERIALS Co.,Ltd. Address before: 222005 No. 59 Cangwu Road, Huaihai Institute of Techology, Lianyungang, Jiangsu. Patentee before: Huaihai Institute of Technology |
|
| TR01 | Transfer of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: A green reduction method for preparation of self supported reduced graphene oxide films Effective date of registration: 20201118 Granted publication date: 20160615 Pledgee: Jiangsu Credit Financing Guarantee Co.,Ltd. Pledgor: LIANYUNGANG BOWEI METALLURGICAL MATERIALS Co.,Ltd. Registration number: Y2020980008201 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20211210 Granted publication date: 20160615 Pledgee: Jiangsu Credit Financing Guarantee Co.,Ltd. Pledgor: LIANYUNGANG BOWEI METALLURGICAL MATERIALS Co.,Ltd. Registration number: Y2020980008201 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: A kind of green reduction preparation method of self-supporting reduced graphene oxide film Effective date of registration: 20220902 Granted publication date: 20160615 Pledgee: Lianyungang financial holding Financing Guarantee Co.,Ltd. Pledgor: LIANYUNGANG BOWEI METALLURGICAL MATERIALS Co.,Ltd. Registration number: Y2022980014400 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20230923 Granted publication date: 20160615 Pledgee: Lianyungang financial holding Financing Guarantee Co.,Ltd. Pledgor: LIANYUNGANG BOWEI METALLURGICAL MATERIALS Co.,Ltd. Registration number: Y2022980014400 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right |