CN104401987B - A kind of preparation method of porous graphene elastic foam - Google Patents
A kind of preparation method of porous graphene elastic foam Download PDFInfo
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- CN104401987B CN104401987B CN201410705370.5A CN201410705370A CN104401987B CN 104401987 B CN104401987 B CN 104401987B CN 201410705370 A CN201410705370 A CN 201410705370A CN 104401987 B CN104401987 B CN 104401987B
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- graphene
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Abstract
The present invention relates to the preparation method of a kind of porous graphene elastic foam, the graphite oxide Hummers method of improvement prepared adds in distilled water, obtains graphite oxide dispersion, ultrasonic disperse, obtaining graphene oxide solution, vacuum filters, and obtains graphene oxide film；By above-mentioned graphene oxide film hydroiodic acid solution reduction, washing, it is dried, obtains graphene film；Above-mentioned graphene film iraser is irradiated, to obtain final product.The preparation method of the present invention is simple, the mechanical property that obtained porous graphene elastic foam has continuous print three-dimensional cavernous structure, density is relatively low, excellent.
Description
Technical field
The invention belongs to the preparation field of grapheme foam, particularly to the preparation method of a kind of porous graphene elastic foam.
Background technology
Since English physicist in 2004 successfully prepares Graphene, its special two-dimensional structure and excellent performance attract
The concern of numerous scientific research personnel.Research shows, Graphene is with SP by carbon atom2The regular hexagon cycle honeycomb of hydridization composition
The new material of the monolayer laminated structure that lattice structure is constituted, the Graphene thickness of the two-dimension single layer of only one of which carbon atom thickness is about
0.35nm, the Graphene of monolayer has the characteristics such as high transparency and thermal conductivity, hard, electrical conductivity is high.The Graphene of two dimension can
To form three-dimensional graphite, one-dimensional CNT, the fullerene etc. of zero dimension by stacking, winding, warpage etc..Graphene
Excellent properties is widely used at nanometer electronic device, transistor, sensing and aeronautical material.
Grapheme foam is to have high specific surface area and low-density porous nanometer material.Grapheme foam has substantial amounts of duct
Structure and higher porosity, have the absorption property of excellence.Grapheme foam material has its character particularity, and porous graphene steeps
The application of foam is studied widely.There is the grapheme foam of electric conductivity as framework material, fill in loose structure
There is the polymethyl methacrylate materials of self-healing properties, the Graphene artificial skin with self-reparing capability can be prepared
(Hou C,et al.Scientific reports,2013,3.).By the graphene film prepared carried out special place's science and engineering
Sequence, makes graphene film have certain thermoelectricity capability, can be used for preparing wearable device and carrys out the vital sign of the monitoring record mankind
(Hou C,et al.Adv.Mater.DOI:10.1002/adma.201401367).Additionally, the relevant hole utilizing grapheme foam
Hole structure and big specific surface area and good electric conductivity, prepare Graphene ultracapacitor (Deng W, et al.Applied
Surface Science, 2014,305:433-438.) etc..
At present, the preparation of grapheme foam generally uses steam reduction method, is steamed by heating hydrazine hydrate at closed reactor
Vapour, steam enters in graphene film lamella, can obtain many empty grapheme foams (Niu Z, et al.Adv.Mater., 2012,
24:4144–4150.).But, these methods obtain the condition harshness that grapheme foam needs, and preparation flow is complicated, and cost is high.
Summary of the invention
The technical problem to be solved is to provide the preparation method of a kind of porous graphene elastic foam, the method operation letter
Single, preparation method is quick；Prepared porous graphene elastic foam has the mechanical property of excellence, it is possible to many second compression energy
Well keeping its elastic modelling quantity, the graphene film after hydroiodic acid reduces has oleophilic drainage performance, can be used to remove
Oily matter in water.
A kind of preparation method of the porous graphene elastic foam of the present invention, including:
(1) graphite oxide prepared by the Hummers method improved: aoxidize the graphite powder of 500 mesh with potassium permanganate and concentrated sulphuric acid, take out
The filter cake that filter obtains is placed in 60 DEG C of oven drying 24h, grinds and obtains graphite oxide powder.The Hummers side that will improve
Graphite oxide prepared by method adds in distilled water, obtains graphite oxide dispersion, ultrasonic disperse, obtains graphene oxide
Solution, vacuum filters, obtains graphene oxide film；
(2) by above-mentioned graphene oxide film hydroiodic acid solution reduction, washing, it is dried, obtains graphene film；
(3) above-mentioned graphene film iraser is irradiated, obtain porous graphene elastic foam.
In described step (1), the concentration of graphite oxide dispersion is 1-10mg/mL.
In described step (1), the ultrasonic disperse time is 1-5h.
In described step (1), vacuum filters particularly as follows: graphene oxide solution adds in core filter funnel, uses cellulose mixture filter
Film vacuum filters 48-72h.
The aperture of described cellulose mixture filter membrane is 0.22 μm.
In described step (2), the concentration expressed in percentage by volume of hydroiodic acid solution is 40-60%；Recovery time is 1-4h.
In described step (2), washing is deionized water wash 2-5 time；It is dried as natural drying at room temperature.
The power density of described step (3) mid-infrared laser is 8～16w/cm2, irradiation time is 5-60s.
The present invention prepares the porous graphene elastic foam of different-thickness, regulation hydrogen by regulation graphite oxide concentration and volume
The time of iodic acid reduction and concentration and the time with laser irradiation control the pattern of porous graphene elastic foam pore space structure.
Graphite oxide dispersion is obtained graphene oxide solution through ultrasonic stripping by the inventive method, by molten to graphene oxide
Liquid vacuum filtration, during moisture detaches, is self-assembly of graphene oxide film between graphene oxide.Then hydrogen is used
Iodic acid reduction obtains graphene film, then obtains porous graphene elastic foam by laser reduction.
The preparation method of the present invention is simple, and obtained porous graphene elastic foam has continuous print three-dimensional cavernous structure, density
Relatively low, excellent mechanical property.Additionally, this porous graphene elastic foam has the performance of lipophilicity substance.Therefore, prepare
Porous graphene elastic foam have the biggest application prospect in absorption, oil-water separation etc..
Beneficial effect
(1) operational approach of the present invention is simple, preparation process fast and easy；
(2) the porous graphene elastic foam prepared by the present invention has the mechanical property of excellence, it is possible to many second compression also can well be protected
Holding its elastic modelling quantity, the graphene film after hydroiodic acid reduces has oleophilic drainage performance, can be used to the oil removing in water
Property material；
(3) the porous graphene elastic foam prepared by the present invention has bigger specific surface area, and inner void structure is similar to rhombus, has
Stable elasticity, flexibility and electric conductivity, can the electronic component of deformation and the absorption aspect such as pollutant have broad application prospects.
Accompanying drawing explanation
Fig. 1 embodiment 1 prepares the XRD figure spectrum of porous graphene elastic foam；
Fig. 2 embodiment 1 prepares the Raman spectrogram of porous graphene elastic foam；
Fig. 3 embodiment 1 prepares nitrogen adsorption desorption figure and the specific surface area of porous graphene elastic foam；
Fig. 4 embodiment 1 prepare porous graphene elastic foam strain-time m-stress curve；
Fig. 5 embodiment 2 prepares the SEM figure of porous graphene elastic foam；
Fig. 6 embodiment 3 prepares the SEM figure of porous graphene elastic foam.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.Should be understood that these embodiments be merely to illustrate the present invention and not
For limiting the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, those skilled in the art can
To make various changes or modifications the present invention, these equivalent form of values fall within the application appended claims limited range equally.
Embodiment 1
At room temperature, weigh the graphite oxide 160mg prepared by the Hummers method improved, be placed in the beaker of 100mL,
Then deionized water 40mL is made into the dispersion liquid that concentration is 4mg/mL, is then put into by beaker and processes 2h in ultrasonic pond by oxygen
It is graphene oxide that graphite is peeled off, and obtains homodisperse graphene oxide solution 40mL；Dress is filtered with the core of 250mL
Putting vacuum to filter, under room temperature, adding one layer of aperture on the core of sand core funnel is 0.22 μm cellulose mixture filter membrane, fixing
Good device also connects vacuum pump, scattered graphene oxide solution is poured into, and vacuum filtration 48h obtains graphene oxide film；
The above-mentioned graphene oxide film being attached together and cellulose mixture filter membrane are taken off in the culture dish putting into a diameter of 90mm,
Adding the hydroiodic acid reductase 12 h that volume fraction is 50%, clean 3-5 time with deionized water, at room temperature natural drying i.e. obtains
Graphene film；It is 8W/cm by power density2Iraser irradiate graphene film 10s, i.e. can get elastic graphite alkene
Foam.Fig. 1 is the XRD figure spectrum of elastic graphite alkene foam prepared by the present embodiment, it will thus be seen that peak value 2 θ of graphene film=
10.8 °, correspond to (002) face, and peak value 2 θ=24.5 ° of grapheme foam, the carbon atom obtaining grapheme foam is spaced about
0.46nm.Fig. 2 is the Raman spectrogram of grapheme foam prepared by the present embodiment, it will thus be seen that the most bimodal (D in figure
Peak and G peak) all change after hydroiodic acid reduction and laser pre-irradiation, the ratio I of peak valueD/IGBy 1.08 increases before reducing
For 1.43 after reduction, then become 1.45 after being irradiated from laser, show that hydroiodic acid reduction makes graphenic surface structure change,
Reduction degree is very big, and laser irradiates while obtaining loose structure reduction.Fig. 3 is grapheme foam prepared by the present embodiment
Adsorption/desorption curve to nitrogen, obtains specific surface area S of grapheme foamBET=68.9m3g-1.Fig. 4 is thickness prepared by this example
Degree for 1.26mm elastic graphite alkene foam strain-time m-stress curve, can be seen that from figure, elasticity aeroge every
Original volume can be returned to during second compression 60%, and repeatedly this phenomenon rear can keep, it can be seen that during every second compression
The maximum stress of elastic gel keeps stable value, shows that this elastic gel can keep stablizing of its mechanical property after repeatedly deformation.
Embodiment 2
At room temperature, weigh the graphite oxide 120mg prepared by the Hummers method improved, be placed in the beaker of 100mL,
Then deionized water 40mL is made into the dispersion liquid that concentration is 3mg/mL, is then put into by beaker and processes 1h in ultrasonic pond by oxygen
It is graphene oxide that graphite is peeled off, and obtains homodisperse graphene oxide solution 40mL；Dress is filtered with the core of 250mL
Putting vacuum to filter, under room temperature, adding one layer of aperture on the core of sand core funnel is 0.22 μm cellulose mixture filter membrane, fixing
Good device also connects vacuum pump, scattered graphene oxide solution is poured into, and vacuum filtration 48h obtains graphene oxide film；
The above-mentioned graphene oxide film being attached together and cellulose mixture filter membrane are lifted down the culture dish putting into a diameter of 90mm
In, add the hydroiodic acid reductase 12 h that volume fraction is 50%, clean 3-5 time with deionized water, at room temperature natural drying is i.e.
Obtain graphene film；It is 8W/cm by power density2Iraser irradiate graphene film 10s, i.e. available elastic stone
Ink alkene foam.The elastic gel obtained is tested, finds that its thickness is thin relative to the sample in example 1, surveys its Raman spectrum,
According to ID/IGRatio is it is observed that reducing degree keeps consistent with the sample in example 1 substantially.
Embodiment 3
At room temperature, weigh the graphite oxide 160mg prepared by the Hummers method improved, be placed in the beaker of 100mL,
Then deionized water 40mL is made into the dispersion liquid that concentration is 4mg/mL, is then put into by beaker and processes 2h in ultrasonic pond by oxygen
It is graphene oxide that graphite is peeled off, and obtains homodisperse graphene oxide solution 40mL；Dress is filtered with the core of 250mL
Putting vacuum to filter, under room temperature, adding one layer of aperture on the core of sand core funnel is 0.22 μm cellulose mixture filter membrane, fixing
Good device also connects vacuum pump, scattered graphene oxide solution is poured into, and vacuum filtration 48h obtains graphene oxide film；
The above-mentioned graphene oxide film being attached together and cellulose mixture filter membrane are lifted down the culture dish putting into a diameter of 90mm
In, add the hydroiodic acid reductase 12 h that volume fraction is 50%, clean 3-5 time with deionized water, at room temperature natural drying is i.e.
Obtain graphene film；It is 16W/cm by power density2Iraser irradiate graphene film 10s, i.e. available elastic stone
Ink alkene foam.The twice that power density is example 1 of the laser used when being prepared sample by example 3, the size obtaining sample is thick
Degree has increased；Survey its Raman spectrum, can be from ID/IGFind out, the reducing degree of sample and the sample in example 1 in example 3
Reducing degree is basically identical.
Claims (8)
1. a preparation method for porous graphene elastic foam, including:
(1) graphite oxide the Hummers method of improvement prepared adds in distilled water, obtains graphite oxide dispersion, ultrasonic point
Dissipating, obtain graphene oxide solution, vacuum filters, and obtains graphene oxide film；
(2) by above-mentioned graphene oxide film hydroiodic acid solution reduction, washing, it is dried, obtains graphene film；
(3) above-mentioned graphene film iraser is irradiated, obtain porous graphene elastic foam.
The preparation method of a kind of porous graphene elastic foam the most according to claim 1, it is characterised in that: described step (1)
The concentration of middle graphite oxide dispersion is 1-10mg/mL.
The preparation method of a kind of porous graphene elastic foam the most according to claim 1, it is characterised in that: described step (1)
The middle ultrasonic disperse time is 1-5h.
The preparation method of a kind of porous graphene elastic foam the most according to claim 1, it is characterised in that: described step (1)
Middle vacuum filters particularly as follows: graphene oxide solution adds in core filter funnel, uses cellulose mixture filter membrane vacuum to filter
48-72h。
The preparation method of a kind of porous graphene elastic foam the most according to claim 4, it is characterised in that: described composite fibre
The aperture of element filter membrane is 0.22 μm.
The preparation method of a kind of porous graphene elastic foam the most according to claim 1, it is characterised in that: described step (2)
The concentration expressed in percentage by volume of middle hydroiodic acid solution is 40-60%；Recovery time is 1-4h.
The preparation method of a kind of porous graphene elastic foam the most according to claim 1, it is characterised in that: described step (2)
Middle washing is deionized water wash 2-5 time；It is dried as natural drying at room temperature.
The preparation method of a kind of porous graphene elastic foam the most according to claim 1, it is characterised in that: described step (3)
The power density of mid-infrared laser is 8～16w/cm2, irradiation time is 5-60s.
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| CN104807861B (en) * | 2015-04-09 | 2017-05-24 | 山东师范大学 | Preparation method of spongy graphene-based stretchable gas sensor |
| CN106773143B (en) * | 2016-12-06 | 2020-01-17 | 东华大学 | Near-infrared photoinduced deformation graphene/NIPAAm composite film and preparation and application thereof |
| CN106672944B (en) * | 2016-12-15 | 2018-08-14 | 东华大学 | A kind of grapheme foam film and its preparation and application |
| CN106732738B (en) * | 2017-02-15 | 2019-08-06 | 东华大学 | A kind of graphene/g-C3N4Three-dimensional network laminated film and its preparation and application |
| RU2753510C1 (en) * | 2017-10-13 | 2021-08-17 | Чжэцзян Юниверсити | Independent freely located graphene film and method for production thereof |
| CN108002366B (en) * | 2017-11-10 | 2020-10-27 | 清华大学 | Graphene solar water cleaning foam and preparation method and application thereof |
| CN108467026B (en) * | 2018-01-16 | 2020-03-27 | 中国科学院上海应用物理研究所 | Porous graphene material and preparation method and application thereof |
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