CN108530073A - A kind of preparation method of the three-dimensional porous graphene film of flexible self-supporting - Google Patents
A kind of preparation method of the three-dimensional porous graphene film of flexible self-supporting Download PDFInfo
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- CN108530073A CN108530073A CN201710926647.0A CN201710926647A CN108530073A CN 108530073 A CN108530073 A CN 108530073A CN 201710926647 A CN201710926647 A CN 201710926647A CN 108530073 A CN108530073 A CN 108530073A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62218—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining ceramic films, e.g. by using temporary supports
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
- C04B38/0635—Compounding ingredients
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Abstract
The present invention provides a kind of preparation method of the three-dimensional porous graphene film of flexible self-supporting, the high molecular polymer for choosing thermal stability difference is template, is blended with graphene oxide, filters film forming, then high-temperature heat treatment under inert gas protection.In high-temperature heat treatment process, graphene oxide is reduced to graphene, and the high molecular polymer of thermal stability difference decomposes leave flourishing hole completely, to obtain the three-dimensional porous graphene film of flexible self-supporting, the thickness of film is can be controlled within the scope of 5 100 um, for pore size in 5 100nm ranges, specific surface area is 300 1600 m2/g.Hole shape, size and the porosity of the three-dimensional porous graphene film of prepared flexible self-supporting can pass through the pattern of high score polymer template（Such as linear, spherical and column）, molecular weight and dosage easily regulate and control.The material can be applied in flexible super capacitor, flexible battery, microelectronics, the fields such as ionic adsorption and UF membrane.
Description
Technical field
The present invention relates to a kind of preparation methods of the three-dimensional porous graphene film of flexible self-supporting.
Background technology
Graphene is a kind of New Two Dimensional carbon nano-material, has high specific surface area, conductivity and intensity.Graphene is received
Rice piece can form Flexible graphene film under the action of Van der Waals force with self assembly.This flexible membrane has very strong mechanicalness
Can, this special structure and unique property make it have in fields such as material science, flexible energy storage, microelectronics, UF membranes
Wide application prospect.Currently, the method that laboratory prepares graphene film mainly prepares graphite oxide by vacuum filtration method
Then alkene film uses electronation or thermal reduction to obtain graphene film.The stacking of graphene sheet layer leads to the practical ratio of graphene
Surface is far below theoretical value, to affect its application in electrochemical energy storage, ionic adsorption etc..Porous structure can carry
High material specific surface shortens Ion transfer path, helps to improve performance of the graphene in electrochemical energy storage and ionic adsorption.
The preparation method of porous graphene has multiple applications report at present, such as hydro-thermal self-assembly method and using foam metal as template
Chemical meteorology deposition method（CVD）Three-dimensional structure graphene can be prepared, using highly basic KOH activation, phosphoric acid activation and titanium dioxide
Carbon activation method etc. etches the powdered graphite alkene that graphene nanometer sheet can get porous structure.But flexible, porous graphene film
Research there is presently no ripe method, Flexible graphene film generally relies on the Close stack film forming of two-dimensional nano lamella, such as
Where keep introducing porous structure under the premise of flexibility and intensity in the structure of Flexible graphene being a challenge.
Invention content
The object of the present invention is to provide a kind of preparation methods of the three-dimensional porous graphene film of flexible self-supporting.What is obtained is porous
Graphene flexible membrane has good flexible and intensity, controllable hole pattern, high specific surface and high conductivity, has both two dimension
The advantage of both nano material and porous material, the application for graphene film in materials science field have a very big significance.
The present invention provides a kind of preparation method of the three-dimensional porous graphene film of flexible self-supporting, it is characterised in that：With hot steady
The high molecular polymer of qualitative difference is template, it is evenly dispersed with graphene oxide solution, then vacuum filtration film forming exists
The three-dimensional porous graphene film of flexible self-supporting is prepared in high temperature pyrolysis under inert atmosphere protection；The high molecular polymer is poly-
Vinyl alcohol (PVA), polyethylene glycol (PEG), polymethyl methacrylate (PMMA), polystyrene (PS), polyvinylpyrrolidone
One or more of (PVP)；Molecular weight is in 5000 to 100000 ranges；It the described method comprises the following steps
（1）Graphene oxide is configured to the aqueous solution of a concentration of 0.5-10 mg/mL；
（2）In deionized water by high molecular polymer dispersion, a concentration of 5-50 mg/mL；
（3）By solution（2）With（1）It mixes according to a certain percentage, stirring, ultrasound make two kinds of solution be uniformly dispersed；
（4）By mixed solution（3）Vacuum filtration film forming, it is dry, obtain graphene oxide and high molecular polymer composite membrane；
（5）Graphene oxide and high molecular polymer composite membrane are warming up to 400-1000 °C under inert gas protection, constant temperature
2-8 h are heat-treated, the three-dimensional porous graphene film of flexible self-supporting is obtained.
The present invention also provides the three-dimensional porous graphene films of flexible self-supporting, it is characterised in that the graphene film has cellular three
Tie up network porous structure and good flexibility, the thickness of film can be controlled in 5-100 um ranges, pore size in 2-100 nm, than
Surface area is 300-1600 m2/g。
Wherein（3）The mass ratio of the step high molecular polymer and graphene oxide is（0.1-10）:1.
Described（5）Inert gas in step is nitrogen, argon gas, helium, any one or a few the mixing in neon.
The present invention is prepared using one step of carbonizatin method is blended, and the principle of the method is, in high-temperature heat treatment process, graphite oxide
The thermal reduction of alkene and the thermal degradation of polymer are carried out at the same time, and graphene oxide is reduced to graphene, and the high score of thermal stability difference
Sub- polymer decomposes leave flourishing hole completely, to obtain the three-dimensional porous graphene film of flexible self-supporting, compared to first adopting
With chemical method redox graphene, then the operation of polymer template is washed away with organic solvent or other processing, work can be shortened
Skill flow.In addition, the present invention is not limited to organic polymer, the inorganic polymer and inorganic nanoparticles for indissoluble are equally suitable
With high-temperature process under inert gas shielding removes template and can be obtained porous graphene film.
Compared with the latest prior art, technical solution provided by the invention has following remarkable advantage：
1 present invention is for the first time that template prepares porous graphene film, specific surface using the high molecular polymer of thermal stability difference
Height, pore structure are flourishing.Pore structure uniform, controllable, by select the polymer controls hole of linear or spherical different structure pattern and
Size can regulate and control porosity by adjusting the ratio of polymer and graphene oxide；
In 2 present invention thermal reduction of graphene oxide and the pyrolysis of polymer template it is synchronous carry out, directly obtained after heat treatment more
Hole graphene first prepares graphene relative to traditional, then builds the operation of porous structure, and the program has preparation process letter
It is single, the advantage that low energy consumption；
The thickness of porous graphene film in 3 present invention can be regulated and controled by the way that the amount of graphene oxide and polymer is added, and be had
Loose structure and excellent ionic conductivity can be applied to electrochemical energy storage, absorption, in catalyst and catalyst carrier.
Description of the drawings：
Fig. 1 is the SEM of the graphene oxide and spherical shape PS composite membranes in embodiment 2, it can be seen that film thickness about 50um；
Fig. 2 is the SEM of the graphene oxide and the partial enlargement of spherical shape PS composite membranes in embodiment 2, stannic oxide/graphene nano piece
Uniformly it is wrapped in the surfaces PS；
Fig. 3 is the SEM of porous graphene film after the heat treatment in embodiment 2, it can be seen that film still has good integrality, heat
In processing procedure, the structure that the two is built is not caved in, film thickness about 50um；
Fig. 4 is the SEM of the partial enlargement of porous graphene film after the heat treatment in embodiment 2, and PS is decomposed, and graphene sheet layer builds
Porous pattern keep good.
Specific implementation mode：
Further clear complete explanation, but it are done to technical solution provided by the invention below by the mode of specific embodiment
Be not construed as limiting the invention.
Embodiment 1
（1）Graphene oxide is configured to the graphene oxide water solution of 0.5 mg/mL；
（2）The linear PVA that molecular weight is 5000 is add to deionized water, the stirring and dissolving at temperature T=60 DEG C, is made dense
Degree is the PVA solution of 5 mg/mL；
（3）100 mL graphene oxide water solutions are taken to be mixed with 1mL PVA solutions, stirring, ultrasound keep two kinds of solution dispersions equal
It is even；
（4）Mixed solution is filtered by vacuum and is formed a film, it is dry, obtain graphene oxide and PVP composite membranes；
（5）Graphene oxide and PVP composite membranes are warming up to 400 °C under nitrogen gas protection, constant temperature is heat-treated 8 h, obtains
The three-dimensional porous graphene film of flexible self-supporting.
Embodiment 2
（1）Graphene oxide is configured to the graphene oxide water solution of 1 mg/mL；
（2）The spherical PS that molecular weight is 10000 is add to deionized water, ultrasonic disperse, is made a concentration of 50 mg/mL's
PS solution；
（3）100 mL graphene oxide water solutions are taken to be mixed with 2 mL PS solution, stirring, ultrasound keep two kinds of solution dispersions equal
It is even；
（4）Mixed solution is filtered by vacuum and is formed a film, it is dry, obtain graphene oxide and PS composite membranes（Such as Fig. 1, stone is aoxidized shown in 2
The SEM of black alkene and PS composite membranes, Fig. 1 are macro morphology figure, and Fig. 2 is partial enlarged view）；
（5）Graphene oxide and PS composite membranes are warming up to 800 °C under argon gas protection, constant temperature is heat-treated 2 h, obtains
The three-dimensional porous graphene film of flexible self-supporting（If Fig. 3, the SEM of porous graphene film shown in 4, Fig. 3 are macro morphology figure, Fig. 4
For partial enlarged view）.
Embodiment 3
（1）Graphene oxide is configured to the graphene oxide water solution of 10 mg/mL；
（2）The spherical PMMA that molecular weight is 100000 is add to deionized water, ultrasonic disperse, a concentration of 10 mg/mL is made
PMMA solution；
（3）1 mL graphene oxide water solutions are taken to be mixed with 10 mL PMMA solution, stirring, ultrasound keep two kinds of solution dispersions equal
It is even；
（4）Mixed solution is filtered by vacuum and is formed a film, it is dry, obtain graphene oxide and PMMA composite membranes；
（5）Graphene oxide and PMMA composite membranes are warming up to 500 °C under helium atmosphere protection, constant temperature is heat-treated 6 h, obtains
To the three-dimensional porous graphene film of flexible self-supporting.
Embodiment 4
（1）Graphene oxide is configured to the graphene oxide water solution of 5 mg/mL；
（2）The linear PEG that molecular weight is 80000 is add to deionized water, ultrasonic disperse, is made a concentration of 5 mg/mL's
PEG solution；
（3）20 mL graphene oxide water solutions are taken to be mixed with 10 mL PEG solution, stirring, ultrasound keep two kinds of solution dispersions equal
It is even；
（4）Mixed solution is filtered by vacuum and is formed a film, it is dry, obtain graphene oxide and PEG composite membranes；
（5）Graphene oxide and PEG composite membranes are warming up to 700 °C under neon gas shield, constant temperature is heat-treated 6 h, obtains
The three-dimensional porous graphene film of flexible self-supporting.
Claims (4)
1. a kind of preparation method of the three-dimensional porous graphene film of flexible self-supporting, it is characterised in that：Using high molecular polymer as mould
Plate agent, by it, ultrasonic disperse is uniform in a solvent with graphene oxide, vacuum filtration film forming, then high under inert atmosphere protection
The three-dimensional porous graphene film of flexible self-supporting is prepared in warm processing；The high molecular polymer is polyvinyl alcohol (PVA),
Polyethylene glycol (PEG), polymethyl methacrylate (PMMA), polystyrene (PS), one kind in polyvinylpyrrolidone (PVP)
Or it is several；The molecular weight of the high molecular polymer is in 5000 to 100000 ranges；It the described method comprises the following steps：
（1）Graphene oxide is configured to the aqueous solution of a concentration of 0.5-10 mg/mL；
（2）In deionized water by high molecular polymer dispersion, a concentration of 5-50 mg/mL；
（3）By solution（2）With（1）It mixes according to a certain percentage, stirring, ultrasound make high molecular polymer and graphene oxide point
It dissipates uniform；
（4）By mixed solution（3）Vacuum filtration film forming, it is dry, obtain graphene oxide and high molecular polymer composite membrane；
（5）Graphene oxide and high molecular polymer composite membrane are warming up to 400-1000 °C under inert gas protection, constant temperature
2-8 h are heat-treated, the three-dimensional porous graphene film of flexible self-supporting is obtained.
2. a kind of three-dimensional porous graphene film of flexible self-supporting, it is characterised in that the graphene film has cellular three-dimensional network
The thickness of porous structure and good flexibility, film can be controlled in 5-100 um ranges, and pore size is in 2-100 nm, specific surface area
For 300-1600 m2/g。
3. according to a kind of preparation method of the three-dimensional porous graphene film of flexible self-supporting described in claim 1, it is characterised in that
Step（3）The mass ratio of the high molecular polymer and graphene oxide is（0.1-10）:1.
4. according to a kind of preparation method of the three-dimensional porous graphene film of flexible self-supporting described in claim 1, it is characterised in that
Step（5）In inert gas be nitrogen, argon gas, helium, any one or a few the mixing in neon.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109244484A (en) * | 2018-10-15 | 2019-01-18 | 山东大学 | A kind of preparation method of porous graphene/carbon nano tube flexible self-supported membrane material |
| CN110965067A (en) * | 2019-11-29 | 2020-04-07 | 哈尔滨工程大学 | Preparation method of graphene grid reinforced titanium-based metal oxide anode |
| CN111484002A (en) * | 2020-04-17 | 2020-08-04 | 南京动量材料科技有限公司 | Preparation method and application of porous graphene membrane |
| CN111547707A (en) * | 2020-04-24 | 2020-08-18 | 中国科学院山西煤炭化学研究所 | Graphene bubble film and preparation method and application thereof |
| CN112117436A (en) * | 2020-09-24 | 2020-12-22 | 北京化工大学 | Novel two-dimensional carbon composite flexible electrode of sodium ion battery and preparation method thereof |
| CN112978719A (en) * | 2021-04-29 | 2021-06-18 | 杭州高烯科技有限公司 | Thickness-controllable high-performance graphene film and preparation method thereof |
| CN114180558A (en) * | 2021-12-27 | 2022-03-15 | 广东墨睿科技有限公司 | Preparation method of graphene micro-nano cavity superconducting film, related product and application |
| CN114293218A (en) * | 2021-12-08 | 2022-04-08 | 国网辽宁省电力有限公司经济技术研究院 | Water electrolysis hydrogen production electrode based on graphene aerogel and synthesis method thereof |
| CN114585588A (en) * | 2020-01-10 | 2022-06-03 | 株式会社Lg新能源 | Porous reduced graphene oxide, method for producing same, sulfur-carbon composite material containing same, and lithium secondary battery |
| CN114906843A (en) * | 2021-02-03 | 2022-08-16 | 南通第六元素材料科技有限公司 | Preparation method of graphene oxide film |
| CN115057436A (en) * | 2022-06-24 | 2022-09-16 | 中山烯利来设备科技有限公司 | Preparation method and application of foam graphene |
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| CN109244484A (en) * | 2018-10-15 | 2019-01-18 | 山东大学 | A kind of preparation method of porous graphene/carbon nano tube flexible self-supported membrane material |
| CN110965067A (en) * | 2019-11-29 | 2020-04-07 | 哈尔滨工程大学 | Preparation method of graphene grid reinforced titanium-based metal oxide anode |
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| CN114585588A (en) * | 2020-01-10 | 2022-06-03 | 株式会社Lg新能源 | Porous reduced graphene oxide, method for producing same, sulfur-carbon composite material containing same, and lithium secondary battery |
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| CN111547707A (en) * | 2020-04-24 | 2020-08-18 | 中国科学院山西煤炭化学研究所 | Graphene bubble film and preparation method and application thereof |
| CN112117436B (en) * | 2020-09-24 | 2021-08-20 | 北京化工大学 | Novel two-dimensional carbon composite flexible electrode of sodium ion battery and preparation method thereof |
| CN112117436A (en) * | 2020-09-24 | 2020-12-22 | 北京化工大学 | Novel two-dimensional carbon composite flexible electrode of sodium ion battery and preparation method thereof |
| CN114906843A (en) * | 2021-02-03 | 2022-08-16 | 南通第六元素材料科技有限公司 | Preparation method of graphene oxide film |
| CN112978719A (en) * | 2021-04-29 | 2021-06-18 | 杭州高烯科技有限公司 | Thickness-controllable high-performance graphene film and preparation method thereof |
| CN112978719B (en) * | 2021-04-29 | 2022-05-06 | 杭州高烯科技有限公司 | Thickness-controllable high-performance graphene film and preparation method thereof |
| CN114293218A (en) * | 2021-12-08 | 2022-04-08 | 国网辽宁省电力有限公司经济技术研究院 | Water electrolysis hydrogen production electrode based on graphene aerogel and synthesis method thereof |
| CN114180558A (en) * | 2021-12-27 | 2022-03-15 | 广东墨睿科技有限公司 | Preparation method of graphene micro-nano cavity superconducting film, related product and application |
| CN114180558B (en) * | 2021-12-27 | 2023-09-08 | 广东墨睿科技有限公司 | Preparation method of graphene micro-nano cavity superconducting film, related product and application |
| CN115057436A (en) * | 2022-06-24 | 2022-09-16 | 中山烯利来设备科技有限公司 | Preparation method and application of foam graphene |
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