CN108069419A - A kind of macroscopic view graphene aerogel and preparation method thereof - Google Patents
A kind of macroscopic view graphene aerogel and preparation method thereof Download PDFInfo
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- CN108069419A CN108069419A CN201711391881.4A CN201711391881A CN108069419A CN 108069419 A CN108069419 A CN 108069419A CN 201711391881 A CN201711391881 A CN 201711391881A CN 108069419 A CN108069419 A CN 108069419A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 141
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 84
- 239000004964 aerogel Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 52
- 239000010439 graphite Substances 0.000 claims abstract description 52
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 150000002978 peroxides Chemical class 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 239000011229 interlayer Substances 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 5
- 238000002791 soaking Methods 0.000 claims abstract description 3
- 239000002253 acid Substances 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 4
- -1 Delanium Chemical compound 0.000 claims description 3
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 3
- 235000019394 potassium persulphate Nutrition 0.000 claims description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 2
- 239000002041 carbon nanotube Substances 0.000 claims description 2
- JRKICGRDRMAZLK-UHFFFAOYSA-N peroxydisulfuric acid Chemical compound OS(=O)(=O)OOS(O)(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-N 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 150000001336 alkenes Chemical class 0.000 claims 1
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium peroxydisulfate Substances [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims 1
- VAZSKTXWXKYQJF-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)OOS([O-])=O VAZSKTXWXKYQJF-UHFFFAOYSA-N 0.000 claims 1
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims 1
- 239000004575 stone Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 13
- 238000004132 cross linking Methods 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 13
- 238000001035 drying Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 238000009834 vaporization Methods 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000003490 calendering Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000007210 heterogeneous catalysis Methods 0.000 description 1
- 239000000138 intercalating agent Substances 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/24—Thermal properties
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
Abstract
A kind of preparation method of macroscopic view graphene aerogel, which is characterized in that comprise the following steps：Raw graphite is added in the sulfuric acid solution of peroxide, after standing reaction, then open placement, obtain primary graphite three-dimensional structure；Obtained primary graphite three-dimensional structure is subjected to soaking and water washing and is dried, obtains the expansible graphite aeroge of interlayer residual sulfuric acid；Obtained expansible graphite aeroge is subjected to high-temperature heat expansion, temperature is 400 ~ 1000 DEG C, obtains macroscopical graphene aerogel.The present invention method it is easy to operate, low energy consumption, efficient, be it is a kind of can prepare with scale graphene aerogel method.The graphene film of gained macroscopic view graphene aerogel remains the hexagonal crystal structures of height, farthest inherits the intrinsic property of graphene；Gained macroscopic view graphene aerogel includes abundant and firm crosslinking points, has the performances such as excellent structural stability and electronics conduction.
Description
Technical field
The invention belongs to nano-carbon material preparation fields, and in particular to a kind of macroscopic view graphene aerogel and its preparation side
Method.
Background technology
Graphene aerogel is a kind of to carry out the porous carbon materials that are formed of overlap joint in three dimensions by graphene film.It has light
The features such as matter, high temperature resistant, corrosion-resistant, high-specific surface area, highly conductive, high heat conduction, high porosity, can be widely applied to pollutant suction
Attached, heat management, conduction, electromagnetic shielding and inhale the fields such as ripple, pressure sensing, electrode material of lithium battery and heterogeneous catalysis.
The typical method for preparing graphene aerogel at present mainly has two kinds of chemical vapour deposition technique and sol-gal process.Before
Graphene defect is few in aeroge prepared by person, but cost is high, it is difficult to large-scale production.The latter is to have certain solution point
The graphene of property is dissipated as raw material, and the liquid phase under stablizing including graphene oxide and surfactant removes graphene.And function
Group and the presence of surfactant weaken conductive or heat conduction network continuity in aeroge significantly, limit it and actual answer
With.
Therefore, develop it is a kind of low cost, can prepare with scale High-performance graphene aeroge method, will greatly promote
Development and practical application of the graphene aerogel in fields such as electrode material, conductive and heat-conductive composite material and electromagnetic shielding materials.
The content of the invention
In view of the foregoing deficiencies of prior art, it is an object of the invention to provide a kind of macroscopical graphene aerogel and
Its preparation method, at the same solve to be difficult to scale in prepared by graphene aerogel, graphene defect is more and specific surface area is low
These three problems.
In order to achieve the above object, the technical solution adopted by the present invention is：A kind of preparation side of macroscopic view graphene aerogel
Method comprises the following steps：
Step（1）Raw graphite is added in the sulfuric acid solution of peroxide, after standing reaction, then open placement, graphene
Further overlap joint occurs between piece, obtains primary graphite three-dimensional structure；
Step（2）By the step（1）Obtained primary graphite three-dimensional structure carries out soaking and water washing and dries, and it is residual to obtain interlayer
Stay the expansible graphite aeroge of sulfuric acid；
Step（3）By the step（2）Obtained expansible graphite aeroge carries out high-temperature heat expansion, and temperature is 400 ~ 1000
DEG C, obtain macroscopical graphene aerogel.
Related content in above-mentioned preparation method technical solution is explained as follows：
1st, in said program, the step（1）Raw graphite be selected from thermal expansion graphite, crystalline flake graphite, Delanium（It is such as high
Anneal crack solution graphite）, graphene powder, conductive black, one or more of activated carbon and carbon nanotubes.It is more than one when selecting
During kind raw material, graphene-based composite aerogel finally can obtain.
2nd, in said program, the step（1）Peroxide be selected from permonosulphuric acid, peroxy-disulfuric acid, hydrogen peroxide, over cure
One or more of sour ammonium, potassium peroxydisulfate and sodium peroxydisulfate.
3rd, in said program, the weight of the sulfuric acid solution of the peroxide is 10 ~ 500 times of the weight of raw graphite；
The mass ratio of the sulfuric acid and peroxide is 1 ~ 100：1.
4th, in said program, in the step（1）In, opening place time for 1 minute to 24 it is small when.What opening was placed
Purpose is：A. further overlap joint occurs in the water absorption course placed in opening, between graphene film；B. open place can make graphite
The moisture in sulfuric acid slow-absorbing air inside worm is a kind of method of slow diluting concentrated sulfuric acid, can avoid step（2）
In plus very exothermic vaporization occurs during water, trigger the disintegration and failure of primary graphite three-dimensional structure.
5th, in said program, in the step（1）In, it is 0 ~ 130 DEG C to stand reaction temperature, and time of repose is small for 0.1 ~ 1
When.
6th, in said program, in the step（3）In, the processing time of high-temperature heat expansion is 1 ~ 300 second.
7th, in said program, the macroscopic view graphene aerogel has multilevel hierarchy, and the form of the multilevel hierarchy is graphite
Alkene piece is vermicular texture in three dimensions inside lap, and is occurred securely by the overlap joint of graphene film between vermicular texture
Adhesion.The specific surface area of macroscopical graphene aerogel is 200 ~ 800 m2/ g has micropore, mesoporous and macroporous structure.Macroscopic view
Graphene is averaged the number of plies as 1 ~ 7 layer in graphene aerogel.
The present invention can be used above-mentioned preparation method and macroscopical graphene aerogel be prepared.
The present invention, by chemically expansible, makes graphite expand and piece splitting, formation vermiform using graphite as raw material
Graphite, while quasiflake graphite is spontaneous is arranged, and form the close adhesion between graphite worm；It is dry using appropriateness washing
It is dry, the expansible graphite three-dimensional structure of the intercalator containing residual is obtained, through high-temperature heat expansion, obtains that there is the grand of high-specific surface area
See graphene aerogel.
By using above-mentioned technology, compared with prior art, favourable advantage of the invention is：
1st, the present invention is using cheap graphite as raw material, by chemically expansible, while completes the stripping of graphene and preliminary liquid phase
Assembling.Arrangement and close adhesion are formed between graphene worm, constructs the graphene network of highly conductive high heat conduction.And previous public
In the chemically expansible technology opened, they should be noted only that it removes effect to the expansion of graphite, ignore special in chemically expansible
Arrangement and sticking effect between some worms.It is to be particularly noted that the open placement operation of the present invention, there are two important spies for tool
Sign：（1）During opening is placed, the sulfuric acid inside graphite worm slowly absorbs water, so as to which generation between graphene film be made further to overlap,
The slight shrinkage phenomenon of the volume of graphite three-dimensional structure can be observed in appearance；（2）It avoids in water washing operations, sulfuric acid is quick
The very exothermic vaporization that dilution triggers causes the destruction of node in gel.Water absorption course during opening is placed has graphene film
Effect overlap joint is of great significance, and close and abundant node significantly improves graphene aerogel and led in the conduction of macro-scale
Hot property.
2nd, the chemically expansible graphite after the present invention innovatively washes appropriateness, as a kind of expansible graphite, adopts it
Take high-temperature heat expansion, i.e. interlayer sulfuric acid discharges rapidly, and realizes the further stripping of graphene film, prepares high-specific surface area
Macroscopical graphene aerogel, the macro property of graphene aerogel is improved, for example, capability of electromagnetic shielding.
3rd, it is not related to the irreversible oxidation to graphene in the present invention, maintains the complete hexagonal structure of graphene, therefore
Farthest retain the attributes such as graphene itself excellent conduction, heat conduction, mechanics.
4th, reaction process to container and equipment without particular/special requirement, the release of no toxic and harmful gas, greatly solve with
High energy consumption and the problems such as being difficult to scale into technology.
5th, the pore wall thickness in macroscopical graphene aerogel in the present invention is 1 ~ 7 layer, and rigidity can bear constant pressure and dry
The capillary force of process.Macroscopical graphene aerogel after constant pressure and dry is carried out, without apparent shrink by volume.It is open compared to previous
Graphene aerogel prepare involved in Vacuum Freezing ＆ Drying Technology, the present invention have apparent cost advantage, cost of use
The drying to macroscopical graphene aerogel can be realized in cheap constant pressure and dry method.
In short, the method for the present invention is easy to operate, low energy consumption, efficient, is that one kind can prepare with scale graphene airsetting
The method of glue.Gained macroscopic view graphene aerogel has two big advantages：（1）Graphene film remains the hexagonal structure knot of height
Structure farthest inherits the intrinsic property of graphene；（2）Comprising abundant and firm crosslinking points, effectively reduce between piece
The resistance and thermal resistance of node assign three dimensions continuity, excellent structural stability and the electron/phonon conduction of its height
Etc. performances.Therefore, it can be widely applied to high-performance conductive and Heat Conduction Material, polymer composites, pollutant absorption, energy storage
The fields such as device, sensor material.
Description of the drawings
Attached drawing 1 is the photomacrograph of graphene aerogel, it is seen that has apparent arrangement architecture between graphene worm.
Attached drawing 2 is the electron scanning micrograph of graphene aerogel microstructure, and stabilization is formed between graphene film
Crosslinking points, including between worm inside and worm；（a）With（b）Represent aeroge surface；（c）With（d）It represents inside aeroge.
Scale is 200 microns in figure.Attached drawing 3 is the relation of graphene aerogel vertical direction conductivity and density in compression process
Curve, 18 mg/cm3The conductivity of aeroge is up to 12 S/cm.
Attached drawing 4 is the capability of electromagnetic shielding of graphene aerogel.Test sample surface density is 3.3 mg/cm2, thickness is
The graphene aerogel of 1.1 mm.In X-band, shield effectiveness reaches 120 ~ 130 dB.
Specific embodiment
The invention will be further described with reference to the accompanying drawings and embodiments：
Embodiment 1：A kind of macroscopic view graphene aerogel and preparation method thereof
Step（1）, 10 grams of ammonium persulfates are dissolved in 90 grams of concentrated sulfuric acids.
Step（2）, 1 gram of crystalline flake graphite is added to step（1）In solution in.When 60 DEG C of standing reactions 2 are small.Finally
Obtain about 400 cubic centimetres of the primary graphite three-dimensional structure for absorbing acid solution.
Step（3）, by step（2）Middle primary graphite three-dimensional structure is open place 6 it is small when, added in dropper along wall of cup
500 milliliters of water impregnate, and after impregnating two hours, incline supernatant liquid, places into 70 DEG C of oven for drying, obtain interlayer residual sulfuric acid
Expansible graphite aeroge.
Step（4）, above-mentioned expansible graphite aeroge be placed in 800 DEG C of Muffle furnaces further expand, processing time
For 60 seconds, macroscopical graphene aerogel is obtained.The test of nitrogen De contamination shows referring to attached drawing 1 that attached drawing 4 specific surface area is
800 m2/g.The thermal conductivity of gained graphene paper reaches 840 W/ (Km after calendering densification）, conductivity is 2800 S/cm.
Embodiment 2：A kind of macroscopic view graphene aerogel and preparation method thereof
Step（1）, by 10 grams of permonosulphuric acid solutions in 90 grams of concentrated sulfuric acids.
Step（2）, 1 gram of thermal expansion graphite is added to step（1）In solution in.When 60 DEG C of standing reactions 2 are small.Most
About 400 cubic centimetres of the primary graphite three-dimensional structure for absorbing acid solution is obtained afterwards.
Step（3）, by step（2）In preliminary three-dimensional structure it is open place 6 it is small when, add in 500 along wall of cup with dropper
Milliliter water impregnate, impregnate two hours after, incline supernatant liquid, places into 70 DEG C of oven for drying, obtain interlayer residual sulfuric acid can
Expanded graphite aeroge.
Step（4）, above-mentioned expansible graphite aeroge be placed in 500 DEG C of Muffle furnaces further expand, processing time
For 60 seconds, macroscopical graphene aerogel is obtained.The test of nitrogen De contamination shows that its specific surface area is 300 m2/g。
Embodiment 3：A kind of macroscopic view graphene aerogel and preparation method thereof
Step（1）, 10 grams of potassium peroxydisulfates are dissolved in 90 grams of concentrated sulfuric acids.
Step（2）, 1 gram of crystalline flake graphite and 0.5g conductive blacks be added to step（1）In solution in.In 60 DEG C of standings
React 2 it is small when.Finally obtain about 400 cubic centimetres of the primary graphite three-dimensional structure for absorbing acid solution.
Step（3）, by step（2）In preliminary three-dimensional structure it is open place 15 minutes, add in 500 along wall of cup with dropper
Milliliter water impregnate, impregnate two hours after, incline supernatant liquid, places into 70 DEG C of oven for drying, obtain interlayer residual sulfuric acid can
Expanded graphite aeroge.
Step（4）, above-mentioned expansible graphite aeroge be placed in 800 DEG C of Muffle furnaces further expand, processing time
For 60 seconds, macroscopical graphene aerogel is obtained.Density is 4.5 mg/cm3When, conductivity is 1.2 S/cm.After rolling densification
The thermal conductivity of gained graphene paper reaches 500 W/ (Km）, conductivity is 2000 S/cm.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar can understand present disclosure and implement according to this, and it is not intended to limit the scope of the present invention.It is all according to the present invention
The equivalent change or modification that Spirit Essence is made, should be covered by the protection scope of the present invention.
Claims (8)
1. a kind of preparation method of macroscopic view graphene aerogel, which is characterized in that comprise the following steps：
Step（1）Raw graphite is added in the sulfuric acid solution of peroxide, after standing reaction, then open placement, graphene
Further overlap joint occurs between piece, obtains primary graphite three-dimensional structure；
Step（2）By the step（1）Obtained primary graphite three-dimensional structure carries out soaking and water washing and dries, and it is residual to obtain interlayer
Stay the expansible graphite aeroge of sulfuric acid；
Step（3）By the step（2）Obtained expansible graphite aeroge carries out high-temperature heat expansion, and temperature is 400 ~ 1000
DEG C, obtain macroscopical graphene aerogel.
2. a kind of preparation method of macroscopical graphene aerogel according to claim 1, it is characterised in that：The step
（1）Raw graphite be selected from thermal expansion graphite, crystalline flake graphite, Delanium, graphene powder, conductive black, activated carbon and
One or more of carbon nanotubes.
3. a kind of preparation method of macroscopical graphene aerogel according to claim 1, it is characterised in that：The step
（1）Peroxide in permonosulphuric acid, peroxy-disulfuric acid, hydrogen peroxide, ammonium persulfate, potassium peroxydisulfate and sodium peroxydisulfate
It is one or more of.
4. a kind of preparation method of macroscopical graphene aerogel according to claim 1, it is characterised in that：The peroxidating
The weight of the sulfuric acid solution of object is 10 ~ 500 times of the weight of raw graphite；The mass ratio of the sulfuric acid and peroxide for 1 ~
100：1.
5. a kind of preparation method of macroscopical graphene aerogel according to claim 1, it is characterised in that：In the step
（1）In, opening place time for 1 minute to 24 it is small when.
6. a kind of preparation method of macroscopical graphene aerogel according to claim 1, it is characterised in that：In the step
（3）In, the processing time of high-temperature heat expansion is 1 ~ 300 second.
7. a kind of preparation method of macroscopical graphene aerogel according to claim 1, it is characterised in that：The macroscopic view stone
Black alkene aeroge has a multilevel hierarchy, and the form of the multilevel hierarchy is that graphene film in three dimensions inside lap is vermiform knot
Structure, and firm adhesion is occurred by the overlap joint of graphene film between vermicular texture, in the macroscopic view graphene aerogel
Contain micropore, mesoporous and macropore.
8. macroscopical graphene aerogel that the preparation method according to any one of claim 1 ~ 7 is prepared.
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| CN110775966A (en) * | 2019-11-21 | 2020-02-11 | 秦皇岛中科瀚祺科技有限公司 | Flexible graphene film and application thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1096767A (en) * | 1993-06-19 | 1994-12-28 | 李儒臣 | A kind of method of making low-sulfur expansible black lead with chemical method |
| CN1102398A (en) * | 1993-11-05 | 1995-05-10 | 宋克敏 | Manufacturing method of low-sulfur expansible black lead |
| CN1453209A (en) * | 2003-04-30 | 2003-11-05 | 中国科学院山西煤炭化学研究所 | Prepn of sulfur-free low-ash high-purity expanded graphite |
| CN1623895A (en) * | 2004-11-16 | 2005-06-08 | 清华大学 | Method for mfg. low sulfur expansive graphite by oxydol sulfate |
| CN101456553A (en) * | 2007-12-11 | 2009-06-17 | 晟茂（青岛）先进材料有限公司 | Chemical processing method for preparing high quality inflatable graphite |
| US20120034442A1 (en) * | 2010-08-06 | 2012-02-09 | Lawrence Livermore National Security, Llc | Graphene aerogels |
| CN104591141A (en) * | 2013-10-30 | 2015-05-06 | 青岛泰浩达碳材料有限公司 | Method for preparing low-sulfur high-multiple expanded graphite |
| CN105502372A (en) * | 2016-01-11 | 2016-04-20 | 赵社涛 | Expanded graphite low-cost production method |
-
2017
- 2017-12-21 CN CN201711391881.4A patent/CN108069419B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1096767A (en) * | 1993-06-19 | 1994-12-28 | 李儒臣 | A kind of method of making low-sulfur expansible black lead with chemical method |
| CN1102398A (en) * | 1993-11-05 | 1995-05-10 | 宋克敏 | Manufacturing method of low-sulfur expansible black lead |
| CN1453209A (en) * | 2003-04-30 | 2003-11-05 | 中国科学院山西煤炭化学研究所 | Prepn of sulfur-free low-ash high-purity expanded graphite |
| CN1623895A (en) * | 2004-11-16 | 2005-06-08 | 清华大学 | Method for mfg. low sulfur expansive graphite by oxydol sulfate |
| CN101456553A (en) * | 2007-12-11 | 2009-06-17 | 晟茂（青岛）先进材料有限公司 | Chemical processing method for preparing high quality inflatable graphite |
| US20120034442A1 (en) * | 2010-08-06 | 2012-02-09 | Lawrence Livermore National Security, Llc | Graphene aerogels |
| CN104591141A (en) * | 2013-10-30 | 2015-05-06 | 青岛泰浩达碳材料有限公司 | Method for preparing low-sulfur high-multiple expanded graphite |
| CN105502372A (en) * | 2016-01-11 | 2016-04-20 | 赵社涛 | Expanded graphite low-cost production method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110775966A (en) * | 2019-11-21 | 2020-02-11 | 秦皇岛中科瀚祺科技有限公司 | Flexible graphene film and application thereof |
| CN110775966B (en) * | 2019-11-21 | 2021-07-27 | 秦皇岛中科瀚祺科技有限公司 | Flexible graphene film and application thereof |
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