CN104828810B - Preparation method of graphene aerogel with ultrahigh specific surface area - Google Patents
Preparation method of graphene aerogel with ultrahigh specific surface area Download PDFInfo
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Abstract
The invention discloses a preparation method of graphene aerogel with an ultrahigh specific surface area, and aims to enlarge the specific surface area of graphene aerogel without affecting the chemical structure of graphene. The preparation method comprises the following steps: taking graphite powder and siloxane as the main raw materials, preparing oxidized graphene, preparing a dispersion liquid of oxidized graphene, preparing silicon oxide hybridized graphene gel, drying the gel, and finally carrying out high-temperature decomposition to obtain the graphene aerogel with an ultrahigh specific surface area. The raw materials are mixed in liquid, after reactions, silicon oxide nano particles with an extremely small particle size can be evenly dispersed, thus the graphene is dispersed, and the agglomeration is prohibited. Furthermore, high-temperature decomposition is performed to remove the silicon oxide, at the same time the high-temperature decomposition has a certain activating effect, thus the prepared graphene aerogel has an ultrahigh specific surface area, which can reach 2491 m<2>/g, and at the same time the chemical structure is barely influenced.
Description
Technical field
The present invention relates to a kind of preparation method of graphene aerogel, more particularly, to a kind of superhigh specific surface area Graphene gas
The preparation method of gel.
Technical background
Graphene aerogel is the three-dimensional porous structure material mutually being overlapped by Graphene, and this material has super
Gently, high-elastic, specific surface area is big, a series of high features of conductive and heat-conductive rate, in catalysis, electrochemistry, the energy, sensor, super electricity
The many such as appearance, absorption, thermal control fields have huge application potential.Redox graphene dispersion liquid or aeroge are mesh
A kind of front the most commonly used method preparing graphene aerogel, this method has that method is simple, low cost, performance are more excellent
Different the features such as.But in reduction process, (oxidation) Graphene is easy to reunite, the ratio of the graphene aerogel therefore prepared
Surface area is much smaller than the specific surface area (2600m of Graphene2/ g), this is very significant considering that for the performance of Graphene, seriously
Have impact on the application in many fields for the graphene aerogel.Therefore, the specific surface area improving graphene aerogel just becomes very
Important.
At present, improving a kind of maximally effective method of graphene aerogel is activation method, prepares Graphene airsetting first
Glue, then recycles vapor, co2, koh etc. activates to graphene aerogel.Document [zhu-yin sui, qing-han
meng,ji-tao li,jian-hua zhu,yi cui,bao-hang han.high surface area porous
carbons produced by steam activation of graphene aerogels.j.mater.chem.a
2014] (high specific surface area porous carbon is prepared by steam activation graphene aerogel) by steam activation method be prepared for greatly than
The graphene aerogel of surface area, specific surface area maximum is up to 1230m2/ g, but this value is still had with the specific surface area of Graphene
Larger gap.
Document [shuwen wang, ferdinando tristan, daiki minami, toshihiko fujimori,
rodolfo cruz-silva,mauricio terrones,kenji takeuchi,katsuya teshima,francisco
rodri′guez-reinoso,morinobu endo,katsumi kaneko.activation routes for high
surface area graphene monoliths from graphene oxide colloids.carbon,76(2014)
220 231] pass through co (from graphene oxide colloid to the activation method of graphene with high specific surface block)2Activation and chemistry are lived
Change (zncl2、h3po4, koh) be prepared for the graphene aerogel of bigger serface, find to carry out activating the graphite of preparation with koh
Alkene aeroge specific surface area is maximum, and its maximum is up to 2150m2/ g, this value still has larger difference with the specific surface area of Graphene
Away from.Activation process itself can produce certain impact to the chemical constitution of Graphene so that producing more on Graphene simultaneously
Defect and room, thus have adverse effect on to some performances of Graphene (aeroge).
Additionally, the method increasing graphene aerogel specific surface area also includes template (i.e. with other bigger serface materials
Expect to prepare graphene aerogel for template) and introduce polymerization inhibitor (stoping the reunion of oxidation (Graphene) with some compounds) etc.
Method, but these methods for graphene aerogel specific surface area increase effect all not as good as activation method, the Graphene of preparation
The specific surface area of aeroge is usually no more than 1200m2/g.
How both to improve the specific surface area of graphene aerogel, and the chemical constitution of Graphene has not been produced to significantly affect and be
The technical problem of those skilled in the art's extremely concern.
Content of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of superhigh specific surface area graphene aerogel,
The specific surface area improving graphene aerogel simultaneously and does not produce to the chemical constitution of Graphene and significantly affects.
A kind of preparation method of superhigh specific surface area graphene aerogel is it is characterised in that include the system of graphene oxide
Standby, the preparation of graphene oxide dispersion, the preparation of oxidation silicon hybridization Graphene gel, it is dried, Pintsch process five step.Concrete step
Suddenly as follows:
The first step, the preparation of graphene oxide: graphite powder is mixed homogeneously according to portion rate 1:3～10 with potassium permanganate and obtains
To graphite powder/potassium permanganate mixture, by strong phosphoric acid (concentration > 85%) and concentrated sulphuric acid (concentration > 95%) according to portion rate 1:5～
15 mix homogeneously obtain nitration mixture, 10～40 parts of nitration mixture are added under conditions of ice bath and stirring 1 part of graphite powder/Gao Meng
In sour potassium mixture, it is warming up to 40～90 DEG C, reacts 5～24h under conditions of stirring, the mixture that reaction is obtained adds 10
In～50 portions of frozen water containing 0.1～3 part of 30% hydrogen peroxide, 1h is centrifuged with the rotating speed of 1000～15000r/min, is separated out
Thing, is dissolved in separating out thing 10～100 parts of deionized water and is centrifuged 1h with the rotating speed of 1000～15000r/min, then will separate out thing
It is dissolved in the 10%～35% of 10～100 parts hydrochloric acid and 1h is centrifuged with the rotating speed of 1000～15000r/min, finally will separate out thing
Be dissolved in 10～100 parts of ethanol (technical pure) and 1h (repeating 3～10 times) be centrifuged with the rotating speed of 1000～15000r/min, take from
Go out thing and be dried to obtain graphene oxide.
Described part is milliliter for liquid, for solid be gram, similarly hereinafter.
Described alr mode is mechanical agitation or magnetic agitation.
Described mixing speed is 100～1000r/min.
Described drying mode is vacuum drying or constant pressure and dry.
Described baking temperature is 0～50 DEG C.
Second step, the preparation of graphene oxide dispersion: the graphene oxide that 1 part of first step is obtained is added to 30～
In 1000 parts of deionized waters, stir 20～150min, then 20～600min is processed with the frequency ultrasound of 10～100khz, then with
Centrifugation 10～the 120min of 1000～15000r/min, takes supernatant to obtain graphene oxide dispersion.
Described alr mode is mechanical agitation or magnetic agitation, and mixing speed is 100～1000r/min.
3rd step, the preparation of oxidation silicon hybridization Graphene gel: the graphene oxide dispersion that 1 part of second step is obtained with
0.001～0.1 part of siloxanes mix homogeneously, mixture is warming up to 60～180 DEG C of insulation 1～48h, obtains aoxidizing silicon hybridization stone
Black alkene gel.
Described siloxanes is tetraethyl orthosilicate, methyl silicate, MTMS, triethoxysilane, first
Base trimethoxy silane or one kind of trimethoxy silane.
4th step, is dried: drying can adopt lyophilization or co2Supercritical drying, when intentionally get have simultaneously micro-
Lyophilization is adopted, when intentionally getting aperture collection during the silica with great specific surface area hydridization graphene aerogel of hole and macroporous structure
In adopt co in the silica with great specific surface area hydridization graphene aerogel of 1～500nm2Supercritical drying.
Described lyophilization is the oxidation silicon hybridization Graphene gel liquid nitrogen freezing obtaining the 3rd step, is then placed in
In freeze drier, at a temperature of 0～-50 DEG C, 12～240h is dried, takes out and can get silica with great specific surface area hydridization
Graphene aerogel.
Described co2Supercritical drying be 3～50 times of volumes of hydridization Graphene gel that the 3rd step is obtained go from
Sub- water is replaced 3～15 times, then the ethanol replacement 3～15 times with 3～50 times of volumes, and each time swap is 3～12h, obtains molten
Oxidation silicon hybridization Graphene gel after agent displacement, then the oxidation silicon hybridization Graphene gel after solvent is replaced puts into co2Super
In the drying kettle of critical drying device, then pass to the co of supercriticality2, replace 2～20 hours, finally with 100kpa/min
Speed release pressure, furnace cooling, take out can get silica with great specific surface area hydridization graphene aerogel.
5th step, Pintsch process: the oxidation silicon hybridization graphene aerogel that the 4th step is obtained is put in pyrolysis furnace, with 20
The flow velocity of～600ml/min is passed through noble gases, then with the ramp of 0.5 DEG C/min～50 DEG C/min to 1000～2000
DEG C, it is incubated 0.5～10h, furnace cooling can get superhigh specific surface area graphene aerogel.
Described noble gases are the mixture of one or more of nitrogen, argon, helium, neon, Krypton.
Following technique effect can be reached using the present invention:
The present invention is realized raw material by way of being mixed with liquid and fully and uniformly mixes, reacted generation particle diameter pole
Little, finely dispersed silica nano particle, thus graphene dispersion is come, stops it from reuniting；The present invention further through
Pintsch process removes silicon oxide, simultaneously works as the effect of similar activation, so that the superhigh specific surface area Graphene gas obtaining
Gel specific surface area superelevation and high temperature stability performance is excellent, catalysis, electrochemistry, the energy, sensor, super capacitor, absorption,
The fields such as thermal control have a good application prospect.
(1) present invention the 3rd step passes through siloxanes and graphene oxide dispersion liquid-phase mixing it is ensured that silicon oxide
Grain is uniform in whole reaction system to be generated and is distributed so that the silicon oxide particle particle diameter obtaining is less, is uniformly dispersed, thus
Sufficiently Graphene is separated, the superhigh specific surface area graphene aerogel specific surface area therefore obtaining is high.
(2) siloxanes that the present invention the 3rd step introduces and the silicon oxide of siloxane reactions generation contain silicone hydroxyl or alkoxyl
Can react with the oxy radical of surface of graphene oxide, thus ensureing that the silicon oxide particle introducing can sufficiently play
Compartmentation.
(3) present invention the 5th step can remove the internal Graphene table of oxidation silicon hybridization graphene aerogel by Pintsch process
So that the specific surface area of graphene aerogel gets a promotion, this process can play and activate the silicon oxide particle in face simultaneously
The effect that process is similar to, so that its specific surface area improves further, the superhigh specific surface area Graphene airsetting that therefore obtains
Glue specific surface area superelevation, up to 2491m2/g.
(4) present invention the 5th step can make silicon oxide and Graphene react and effusion of gasifying by Pintsch process, because
The superhigh specific surface area graphene aerogel silicone content that this obtains is low.
(5) present invention the 5th step be can be by Pintsch process makes the group of the internal graphenic surface of graphene aerogel take off
Remove, therefore structure is more stable, can apply at high temperature and the change of volume and structure etc. does not occur.
Therefore, preparation method process is simple of the present invention, low cost, the product preparing catalysis, electrochemistry, the energy,
The fields such as sensor, super capacitor, absorption, thermal control have a good application prospect.
Brief description
Fig. 1 is the overview flow chart of the inventive method.
Fig. 2 is superhigh specific surface area graphene aerogel sem (field emission scanning electron microscope) photo that embodiment 1 obtains.
Fig. 3 is the N2 adsorption curve of the superhigh specific surface area graphene aerogel that embodiment 1 obtains.
Specific embodiment
The invention will be further described below to use embodiment, but these embodiments are not produced to protection scope of the present invention
Raw any restriction.
Embodiment 1
(1) 3g graphite powder is mixed homogeneously with 15g potassium permanganate, 40ml strong phosphoric acid is mixed homogeneously with 360ml concentrated sulphuric acid
Obtain nitration mixture, gained nitration mixture is added under the mechanical agitation of ice bath and 300r/min gained graphite powder/potassium permanganate
In mixture, it is warming up to 50 DEG C, reacts 12h under the mechanical agitation of 300r/min, the mixture that reaction is obtained adds
Contain in the frozen water of 10ml30% hydrogen peroxide to 400ml, with the rotating speed centrifugation of 2000r/min, obtain separating out thing, thing will be separated out molten
Deionized water in 200ml and the rotating speed with 2000r/min centrifugation 1h, then by separate out thing be dissolved in 200ml 30% hydrochloric acid simultaneously
1h is centrifuged with the rotating speed of 2000r/min, is finally dissolved in separating out thing the ethanol of 200ml and 1h is centrifuged with the rotating speed of 2000r/min
(3 times), take and separate out 50 DEG C of vacuum drying of thing and obtain graphene oxide.
(2) graphene oxide obtaining 1g step (1) is added in 100ml deionized water, in the magnetic force of 300r/min
Stir 60min under stirring condition, then 60min is processed with the frequency ultrasound of 50khz, then the centrifugation with 8000r/min
120min, takes supernatant to obtain graphene oxide dispersion.
(3) graphene oxide dispersion obtaining 5ml step (2) is mixed homogeneously with 0.05ml tetraethyl orthosilicate, will mix
Compound is warming up to 110 DEG C of insulation 24h, obtains aoxidizing silicon hybridization Graphene gel.
(4) the oxidation silicon hybridization Graphene gel liquid nitrogen freezing obtaining step (3), is then placed in freeze drier
In, 48h is dried at a temperature of -50 DEG C, takes out and obtain aoxidizing silicon hybridization graphene aerogel.
(5) the oxidation silicon hybridization graphene aerogel that step (4) obtains is put in pyrolysis furnace, with the stream of 100ml/min
Speed is passed through argon, then with the ramp of 2 DEG C/min to 1000 DEG C, is incubated 1h, furnace cooling can get superelevation specific surface
Long-pending graphene aerogel.
Adopt the quality of the extremely-low density hydridization graphene aerogel heat-barrier material that weighs with scale, surpassed using vernier caliper measurement
The overall dimensions of low-density hydridization graphene aerogel heat-barrier material, with quality divided by its volume, calculate embodiment 1 and obtain
Superhigh specific surface area graphene aerogel density be 0.0060g/cm3.
Extremely-low density hydridization graphene aerogel heat-barrier material is tested using hitachi s4800 field emission scanning electron microscope
Microstructure, the sem photo of the silica with great specific surface area hydridization graphene aerogel that embodiment 1 obtains is as shown in Fig. 2 wherein
A () figure amplification is 3000 times, the deeper part of color is hole, and the shallower part of color is that the stone of silicon oxide particle is distributed with
Black alkene, (b) figure amplification is 30000 times, and granular substance is silicon oxide particle, and the paper-like thing full of fold is Graphene, from
In figure can be seen that the hole that there are a large amount of apertures inside aeroge in several microns to some tens of pm, and graphene aerogel surface
The silicon oxide particle of the overwhelming majority removes during Pintsch process, the only remaining few silicon oxide particle in surface.Using
The light of the superhigh specific surface area graphene aerogel that escalab 250xi type x-ray photoelectron spectrograph testing example 1 obtains
Electronic energy spectrum, through analyzing its silicone content only 1.74%.
The superelevation ratio being obtained using the autosorb-1 type Full-automatic physical adsorption instrument testing example 1 of Kang Ta company of the U.S.
The N2 adsorption curve (as shown in Figure 3) of surface area graphene aerogel, wherein abscissa are relative pressure, and vertical coordinate is absorption
Amount, calculates its specific surface area using bet (brunauer emmett teller) method, the superelevation specific surface that embodiment 1 obtains
The specific surface area of long-pending graphene aerogel is 2332m2/g.
First step graphite powder and potassium permanganate portion rate, strong phosphoric acid and concentrated sulphuric acid portion rate, nitration mixture and graphite powder/permanganic acid
Potassium mixture portion rate, reaction temperature and time, the number of frozen water and hydrogen peroxide mainly affects to obtain the oxidation of graphene oxide
Degree and lamellar spacing, when parameters value is all in given range, the graphene oxide degree of oxidation obtaining and piece thickness
Degree is impacted less, all more suitable, and therefore these parameters affect on the specific surface area of superhigh specific surface area graphene aerogel
Less；First step alr mode, mixing speed, drying mode and temperature do not affect on course of reaction, only needed for influence process
Time, impact will not be produced on the graphene oxide degree of oxidation obtaining and lamellar spacing, therefore to superhigh specific surface area stone
The specific surface area impact of black alkene aeroge is less；The consumption of first step deionized water, the concentration of hydrochloric acid and consumption, the use of ethanol
Amount, the rotating speed of centrifugation and time, is dissolved in ethanol and the number of times that is centrifuged is to the graphene oxide degree of oxidation obtaining and lamellar spacing
No affect, only a little impact is produced on the purity of the graphene oxide obtaining, therefore these parameters are to superhigh specific surface area graphite
The specific surface area impact of alkene aeroge is less.
Second step alr mode, mixing speed, mixing time, supersonic frequency, ultrasonic time, centrifugal rotational speed, centrifugation time
The main impact scattered uniformity coefficient of graphene oxide dispersion, when parameters are in the range of being given, to graphite oxide
The impact of alkene dispersion liquid scattered uniformity coefficient less, all can obtain uniform graphene oxide dispersion, therefore these parameters
The specific surface area of superhigh specific surface area graphene aerogel is affected less.
3rd step holding temperature and time mainly affect the abundant degree that siloxanes is reacted with graphene oxide dispersion, are
React fully and carry out, the temperature range being given and time have exceeded siloxanes and fully reacted institute with graphene oxide dispersion
The temperature and time needing, therefore holding temperature and time affect not on the specific surface area of superhigh specific surface area graphene aerogel
Greatly.
4th step lyophilization temperature and time mainly affects the speed of drying and abundant degree, to superhigh specific surface area stone
Black alkene aeroge structure will not produce impact, therefore lyophilization temperature and time is to superhigh specific surface area Graphene airsetting
The specific surface area impact of glue is less.
Embodiment 2～162
As shown in table 1, its technical process is same as Example 1, difference for the technological parameter that embodiment 2～162 is adopted
Place is siloxanes species, deionized water and graphene oxide portion rate, siloxanes and graphene oxide dispersion portion rate, splits
4 parameters such as solution temperature, in addition to technological parameter write in table, remaining technological parameter is same as Example 1.
Table 1 embodiment 2～162 prepares preparation technology parameter and the performance of superhigh specific surface area graphene aerogel
Embodiment 163
Embodiment 163 is the 4th step with the difference of embodiment 1, and remaining technological parameter is same as Example 1.Implement
Example 163 the 4th step is: by step (3), the hydridization Graphene gel deionized water of 10 times of volumes obtaining, ethanol are replaced respectively
10 times, each time swap is 6h, obtains the oxidation silicon hybridization Graphene gel after solvent displacement, then the oxygen after solvent is replaced
SiClx hydridization Graphene gel puts into co2In the drying kettle of supercritical drying device, then pass to the co of supercriticality2, displacement
5 hours, finally pressure is discharged with the speed of 100kpa/min, furnace cooling can get superhigh specific surface area Graphene airsetting
Glue.
The performance of the superhigh specific surface area graphene aerogel that embodiment 163 obtains is shown in Table 3.
The volume of the 4th step deionized water and ethanol and displacement number of times and time mainly affect the removal of impurity in gel
The degree that in thorough degree and gel, solvent is replaced by alcohol, no affects on the structure and property of gel, when parameters are being given
In the range of when, all can thoroughly remove the impurity in gel and the solvent in gel can also thoroughly be replaced by alcohol,
Therefore these parameters affect less on the specific surface area of superhigh specific surface area graphene aerogel.Supercriticality co2During displacement
Between alcohol is displaced in main impact gel thorough degree, when in the range of being given, alcohol is thoroughly replaced, therefore super faces
Boundary's state co2Time swap affects less on the specific surface area of superhigh specific surface area graphene aerogel.
Embodiment 164～324
As shown in table 2, its technical process is identical with embodiment 163, no for the technological parameter that embodiment 164～324 is adopted
It is siloxanes species, deionized water and graphene oxide portion rate, siloxanes and graphene oxide dispersion number with part
Than 4 parameters larger to superhigh specific surface area graphene aerogel performance impact such as, cracking temperatures, except technique write in table
Outside parameter, remaining technological parameter is identical with embodiment 163.
Table 2 embodiment 163～324 prepares preparation technology parameter and the performance of superhigh specific surface area graphene aerogel
Claims (10)
1. a kind of preparation method of superhigh specific surface area graphene aerogel is it is characterised in that comprise the steps:
The first step, the preparation of graphene oxide: graphite powder is mixed homogeneously according to portion rate 1:3～10 with potassium permanganate and obtains stone
Powdered ink/potassium permanganate mixture, strong phosphoric acid is mixed homogeneously according to portion rate 1:5～15 with concentrated sulphuric acid and obtains nitration mixture, by 10～
40 parts of nitration mixture is added in 1 part of graphite powder/potassium permanganate mixture under conditions of ice bath and stirring, is warming up to 40～90
DEG C, react 5～24h under conditions of stirring, the mixture that reaction is obtained adds 10～50 parts to contain 0.1～3 part 30% pair
In the frozen water of oxygen water, it is centrifuged 1h, obtains separating out thing, be dissolved in separating out thing 10～100 parts of deionized water and be centrifuged 1h, then will be from
Go out thing to be dissolved in 10～100 parts of 10%～35% hydrochloric acid and be centrifuged 1h, finally will separate out the ethanol that thing is dissolved in 10～100 parts simultaneously
Centrifugation 1h, repeats 3～10 times, takes and separates out thing and be dried to obtain graphene oxide；
Second step, the preparation of graphene oxide dispersion: the graphene oxide that 1 part of first step is obtained is added to 30～1000 parts
In deionized water, stir 20～150min, then 20～600min is processed with the frequency ultrasound of 10～100khz, then it is centrifuged 10～
120min, takes supernatant to obtain graphene oxide dispersion；
3rd step, the preparation of oxidation silicon hybridization Graphene gel: the graphene oxide dispersion that 1 part of second step is obtained with
0.001～0.1 part of siloxanes mix homogeneously, mixture is warming up to 60～180 DEG C of insulation 1～48h, obtains aoxidizing silicon hybridization stone
Black alkene gel；
4th step, is dried: the oxidation silicon hybridization Graphene gel that the 3rd step obtains is dried, obtains high-specific surface area oxidation
Silicon hybridization graphene aerogel；
5th step, Pintsch process: the oxidation silicon hybridization graphene aerogel that the 4th step is obtained is put in pyrolysis furnace, is passed through inertia
Gas, then heats to 1000～2000 DEG C, is incubated 0.5～10h, and furnace cooling obtains superhigh specific surface area Graphene airsetting
Glue；
Described part is milliliter for liquid, for solid be gram.
2. superhigh specific surface area graphene aerogel as claimed in claim 1 preparation method it is characterised in that the first step,
Alr mode described in two steps is mechanical agitation or magnetic agitation；Mixing speed during stirring is 100～1000r/min.
3. superhigh specific surface area graphene aerogel as claimed in claim 1 preparation method it is characterised in that the first step from
Going out mode when thing is dried is vacuum drying or constant pressure and dry；Baking temperature is 0～50 DEG C.
4. the preparation method of superhigh specific surface area graphene aerogel as claimed in claim 1 is it is characterised in that first step institute
The strong phosphoric acid concentration stated > 85%, concentrated sulphuric acid concentration > 95%, ethanol is technical pure.
5. the preparation method of superhigh specific surface area graphene aerogel as claimed in claim 1 is it is characterised in that the 3rd step institute
The siloxanes stated is tetraethyl orthosilicate, methyl silicate, MTMS, triethoxysilane, methyl trimethoxy epoxide
Silane or one kind of trimethoxy silane.
6. the preparation method of superhigh specific surface area graphene aerogel as claimed in claim 1 is it is characterised in that the 4th step is adopted
With lyophilization, will the oxidation silicon hybridization Graphene gel liquid nitrogen freezing that obtains of the 3rd step, be then placed in freeze drier
In, 12～240h is dried at a temperature of 0～50 DEG C, takes out the high-specific surface area with micropore and macroporous structure
Oxidation silicon hybridization graphene aerogel.
7. the preparation method of superhigh specific surface area graphene aerogel as claimed in claim 1 is it is characterised in that the 4th step is adopted
Use co2Supercritical drying, will the hydridization Graphene gel that obtains of the 3rd step deionized water of 3～50 times of volumes replace 3～
15 times, then the ethanol replacement 3～15 times with 3～50 times of volumes, each time swap is 3～12h, obtains the oxygen after solvent displacement
SiClx hydridization Graphene gel, then the oxidation silicon hybridization Graphene gel after solvent is replaced puts into co2Supercritical drying device
Drying kettle in, then pass to the co of supercriticality2, replace 2～20 hours, finally with the speed release pressure of 100kpa/min
Power, furnace cooling, takes out and can get the silica with great specific surface area hydridization graphene aerogel that aperture concentrates on 1～500nm.
8. the preparation method of superhigh specific surface area graphene aerogel as claimed in claim 1 is it is characterised in that the 5th step institute
The noble gases stated are the mixture of one or more of nitrogen, argon, helium, neon, Krypton.
9. the preparation method of superhigh specific surface area graphene aerogel as claimed in claim 1 is it is characterised in that described centrifugation
Rotating speed be 1000～15000r/min.
10. the preparation method of superhigh specific surface area graphene aerogel as claimed in claim 1 is it is characterised in that the 5th step is led to
The flow velocity entering noble gases is 20～600ml/min, and the speed of intensification is 0.5 DEG C/min～50 DEG C/min.
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| GB201204169D0 (en) * | 2012-03-09 | 2012-04-25 | Bio Nano Consulting | Graphene and graphene oxide aerogels/xerogels for co2 capture |
| CN103537236B (en) * | 2013-10-22 | 2015-12-02 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of graphene aerogel |
| CN104098089B (en) * | 2014-07-25 | 2015-11-11 | 西南民族大学 | A kind of preparation method of doped graphene foam |
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